Deep-Processing Engineering of AVH 150

Thousand tons/year Coal Tar

Operation Procedures of Tar Distillation

(Trial)
目录
1 Scope............................................................................................................................................ 1
2 Main Professional Documents for This Position.......................................................................... 1
3 Special Qualification Requirements............................................................................................. 1
4 Responsibilities and Authority......................................................................................................2
4.1 Responsibilities...................................................................................................................2
4.2 Authority............................................................................................................................. 2
5 Relations of Posts......................................................................................................................... 3
6 Operating Conditions....................................................................................................................4
6.1 Human resources................................................................................................................ 4
6.2 Natural resources................................................................................................................ 4
6.3 Equipment and tools........................................................................................................... 4
6.4 Safety protection................................................................................................................. 5
6.5 Environmental State........................................................................................................... 6
6.6 Site Set Management.......................................................................................................... 6
7 Technological Description............................................................................................................ 6
7.1 Technological process.........................................................................................................6
7.2 Introduction to technology..................................................................................................7
8 Quality of Raw Materials and Products........................................................................................8
8.1 Quality of raw materials..................................................................................................... 8
8.2 Specification of products.................................................................................................... 9
9 Main Operating Parameters........................................................................................................ 12
9.1 Temperature of oil products.............................................................................................. 12
9.2 Temperature of materials through tube heating furnace................................................... 12
9.3 Parameters of each tower..................................................................................................13
9.4 Operation parameters for tube heating furnace................................................................ 13
9.5 Oil temperature at the outlet of each con-cooler:............................................................. 13
9.6 Level at the bottom of each tower.................................................................................... 13
10 Basic Requirements for Working Process................................................................................ 14
10.1 Preparation...................................................................................................................... 14
10.2 Pre-production meeting.................................................................................................. 14
10.3 Inspection for taking over shift.......................................................................................14
10.4 Evaluation of operating conditions................................................................................. 14
10.5 Operating process........................................................................................................... 14
10.6 Summary of operating status.......................................................................................... 22
10.7 Shift exchange................................................................................................................ 22
10.8 After-production activities.............................................................................................. 23
11 Standard revision history (refer to Appendix A).......................................................................23
1 Scope

This document specifies the main professional documents, special requirements of job
quality, responsibilities and authority, post interface relation, and working conditions for the post
of tar distillation of Indian AVH Company.
This standard applies to the post of tar distillation of Indian AVH Company.

2 Main Professional Documents for This Position

GB 12710-2008 Safety Code for the Coking Plant

3 Special Qualification Requirements

3.1 Know well about the production technology of this process, be familiar with the production
technology of prior and next processes, and learn about the production technology and related
knowledge of other processes. Be able to independently deal with general production operation
accidents.
3.2 Know well about the performance of the devices involved in this post, and be able to analyze
and determine the reasons that cause the changes of operating parameters.
3.3 Be able to maintain the devices involved in this post, and have necessary basic knowledge,
expertise and certain theoretical level related to this post.
3.4 Be equipped with Junior Middle school graduate degree and above or meet the requirements
of skills for the intermediate workers.
3.5 Know well about the production control methods related to the quality of products, and
general trouble-shooting methods of pipes and valves.
3.6 Know well about basic principles and knowledge about distillation, and the physicochemical
properties and safety protection knowledge related to tar, pitches, anthracene oil, light oil,
three-mixing distillate, and such materials and fuel oil, steam, nitrogen, and compressed air.
3.7 Possess skilled fire-fighting skills and other knowledge about hazards, environmental factors,
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and hazardous chemicals as well as other emergency response skills.

4 Responsibilities and Authority

4.1 Responsibilities

4.1.1 Under the leadership of the team leader, complete the work related to production, quality,
equipment, safety, environmental protection, and fixed location management.
4.1.2 Participate in weekly security meeting, pre-production meeting and other activities to learn
about safety knowledge.
4.1.3 Be responsible for using, daily maintenance and check related to equipment, facilities, tools
and pipe network of power technology, assist the servicing and participate in overhaul KYT
(Kiken Yochi Training) activity, and supervise and manage various types of constructions within
the monitored area.
4.1.4 Learn about all information before and after the shift and that related to production, quality,
equipment, safety and environmental protection, to control well the handover and production
process. Timely report all issues involved in production to the team leader with respect to
production, quality, equipment, safety and environmental protection.
4.1.5 Follow the instructions of the team leader, and be responsible for starting, stopping and
adjusting the tar distillation system. Notify the personnel of the related posts before and after
starting and stopping the system, and report the team leader.
4.1.6 Be responsible for controlling the output and quality, and for taking and sending samples.
4.1.7 Timely and accurately handle the requests about production from the involved posts, and
keep in touch with the involved posts.
4.1.8 Patrol and inspect on time and fill in related records, and timely report the related
information to the team leader.
4.1.9 Actively look for various hazards and timely handle and report.
4.1.10 Be responsible for keeping the area of responsibility clean and patrolling and examining
the green fields.
4.1.11 Finish other tasks assigned by the leaders.

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4.2 Authority

4.2.1 In case of emergency, have the right to take emergency measures to deal with the
conditions related to major security, environmental protection, equipment, measuring, production
operation or quality accidents, and report to the team leader afterwards.
4.2.2 Keep in touch with the team leader and with the proceeding and subsequent personnel in
charge at any time, learn about related information and put forward to needed assistance.
4.2.3 Stop all kinds of violation actions, and avoid command against rules and reckless
adventures.
4.2.4 Put forward valuable suggestions or improvement measures with respect to various issues
arising during the production process.
4.2.5 Have the right to reject unqualified raw materials.

5 Relations of Posts

The following diagram shows the relations between posts.

Team leader
instruction
Give
situation
Reflect the

Unwashed
three-mixing
distillate
an

Reflux
flow Washing
Tar pump Tar distillation
Modified pitches
worker
Treatment Mid-temperature
capacity pitch
Pouring Report Take
samples samples

Oil depot worker Laboratory

5.1 With tar pump worker: Contact the worker to know about the treatment capacity of the tar.
Ensure that the reflux of the dewatering tower, pitch tower and distillate tower is in good
condition.

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5.2 With the post of modified pitch: Describe the quality and flow of the pitches to the staff of
modified pitches, and regulate the quality and production of the pitches based on the
requirements of the modified pitch production.
5.3 With the post of washing: Supply the unwashed three-mixing distillate.
5.4 With the worker of oil depot: Describe the production conditions related to pitches,
anthracene oil, phenol oil and light oil and assist the operation.
5.5 Relation with the laboratory: Timely take samples and adjust production operations
according to the test results.

6 Operating Conditions

6.1 Human resources

6.1.1 The staff for this post must meet the requirements of physical fitness, and have necessary
basic knowledge, expertise and certain theoretical level related to this post.
6.1.2 The staff for this post shall accept the training about safety and technology and they should
not take the jobs until they pass the training examination.
6.2 Natural resources

Operation process for this post must require (anti-fire) water, steam, electricity and other
power substances.
6.3 Equipment and tools

6.3.1 Main production equipments:

Specifications and
No. Name Quantity Weight (kg)
Performance
1 Dewatering tower K-7101 DN1200/1800 H=24312 1
2 Pitch tower K-7102 DN2300 H=28429 1
3 Distillation tower K-7103 DN2100 H=45780 1
Effective thermal load of tar tube
4 385×104 kCal/hr 1
furnace F-7101
6.3.2 Tools
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 No. Name Type Quantity
1 Pipe wrench 450—60 2
10# 1
300—40 1
2 Adjustable wrench 300×36 2
200×24 1
3 Scraper 1

4 Hacksaw 1
5 Snip 1
6 Screw driver 1
7 Pincer 1
8 Iron hammer 1
9 Oil resistant high 6
temperature
resistant rubber
hose
10 Ring spanner 6
6.3.3 Necessary equipment and apparatus for emergency
Type Quantity
Dry power extinguisher
Fire hydrant
6.4 Safety protection

6.4.1 Identification of hazardous sources and environmental factors for this post: ① Light oil and
such chemical medium could easily lead to air pollution, fire, explosion and other accidents.
Precautions: regular inspection and careful operation; ② tube furnace, distillation tower and such
equipment with high temperature could lead to burns damage. Precautions: carefully operate
with thermal insulation layers for technological pipelines; ③ the leakage of fuel oil may cause
fire, explosion, poisoning and other accidents. Precautions: ventilate the area, and take
immediate measures if any odor arises; ④ narrow and complicated working area is easy to slip.
Precautions: Keep a good mental state. Carefully walk to avoid slipping.
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6.4.2 Protective Equipment
6.4.2.1 General protective equipment: helmets, masks, cotton labor protective clothing, gloves,
work shoes, and flashlight.
6.4.2.2 Special protective equipment: safety belts, oxygen respirator.
6.5 Environmental State

6.5.1 This post requires maintaining lighting, good ventilation, unimpeded channels without
obstacles.
6.5.2 The safe marks on site are complete and their contents comply with the environmental
requirements.
6.6 Site Set Management
6.6.1 Make sure there is no skin of fruit, paper, plastic bags or such sundries inside and outside
door, to keep clean and tidy, beautiful, no dust, cobwebs, cigarette butts, and no oil pollution on
the ground.
6.6.2 Keep the instruments and operating cabinet clean, no oil pollution, dust, and maintain the
integrity of the recording paper.
6.6.3 Keep record books clean and record content complete, and in correct place.

6.6.4 Keep tables clean, place all kinds of tools in the toolboxes or the specified location and
keep tidy, and clear the groceries that have nothing to do with the production operations and are
inconsistent with the environment.
6.6.5 All kinds of signs on the production field shall be complete, clear and standard.
6.6.6 Fire-fighting and flood control facilities shall be placed in specified location and not be
used for other purposes.
6.6.7 All kinds of signs on the production field shall be clear and standard.

7 Technological Description

7.1 Technological process

After dewatering through static storage dehydration and centrifuge, removing water and
oil by flashing through dewatering tower, and removing the pitches and II-anthracene oil by
negative pressure distillation through the pitch tower, the tar flows into the distillation tower and
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generates the washed three-mixing distillate including I-anthracene oil, phenol oil and
phenol-naphthalene oil through the way of negative pressure distillation. The washed
three-mixing distillate mixes with industrial naphthalene and they are distilled to generate phenol
oil, wash oil and industrial naphthalene. The phenols that are removed by washing will be made
to neutral sodium phenolate for sales. I-anthracene oil generates crude anthracene after the
centrifugal crystallization. Industrial naphthalene is crystallized into refined naphthalene. The
residual oil after crystallizing the industrial naphthalene is treated into water reducer.
7.2 Introduction to technology

After treated by the tar preheater (E-7104), the dehydrated tars will be heat-exchanged
(E-7103) with mid-temperature pitch (or modified pitch) from the bottom of pitch tower (K-7102)
by the heat exchanger. Then the tars will enter the dewatering tower (K-7101). The water at the
top of dewatering tower and the steam of light oil are congealed by a condenser (E-7102) and
then sent to the oil-water separator (S-7101) (the temperature at the top of dewatering tower is
limited at 88-95℃). The separated water flows automatically into the phenol water tank (T-7108)
of reservoir area; and the separated light oil enters the light oil reflux tank (T-7101), where some
of them are pumped back to the dewatering tower (K-7101) by a light oil reflux pump
(P-7101AB), some of them will mix with crude tars and enter the dewatering tower for
azeotropic distillation, and some of them will be taken as products and delivered to the light oil
storage tank (T-7104). Parts of anhydrous tars (water content limited less than 0.2%) from the
bottom of tower (K-7101) will be sent to the convection section of tube furnace (F-7101) via tar
circulating pump (P-7102AB), which will come back to the dewatering tower (K-7101) after
being heated; the other parts will be sent to the radiation section of tube furnace (F-7101) via the
extraction pump (P-7104AB) of dewatering tower and then enter the pitch tower (K-7102) after
being heated to 330-350℃.
The pitch tower (K-7102) is under negative pressure operation. During production, the
mid-temperature pitch is extracted from the bottom of pitch tower (K-7102). After heated with
anhydrous tars (E-7105) and crude tar (E-7103), the mid-temperature pitch will enter the pitch
head tank for producing solid mid-temperature pitch. During production of modified pitch, the
mid-temperature pitch extracted from the bottom of pitch tower (K-7102) will enter the modified
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pitch unit directly, and the modified pitch coming out of pitch system will be heat-exchanged
with anhydrous tars (E-7105) and crude tar (E-7103) one more time. During preparation of
carbon black oil, the maltha instead of Ⅱ-anthracene oil will be extracted. Gaseous phase
(phenol oil, naphthalene oil, wash oil, anthracene oil and the like distilled steam) of the top
(K-7102) enter the lower-bottom part of distillation tower (K-7103) via communicating pipe. At
the top of pitch tower (K-7102) there is a reflux unit of I-anthracene oil, and Ⅱ-anthracene oil
will be extracted from the side. After cooled at the Ⅱ-anthracene oil cooler (E-7108), the oil will
enter the Ⅱ-anthracene oil storage tank (T-7103).
The distillation tower (K-7103) uses negative pressure operation. After cooled at the
condenser (E-7101), the gaseous phase distilled from phenol oil that is leaked from the top
(K-7103) will enter the oil-water separator (S-7102) of phenol oil for oil-water separation.
Separated water flows into the phenol water tank (T-7108), and phenol oil will be distilled into
the phenol oil reflux tank (T-7102), among which some phenol oil fraction will be sent back to
the top of distillation tower via the reflux pump (P-7107AB), regarded as the reflux of the
distillation tower, and the remaining phenol oil will be taken as products and be delivered to the
phenol oil tank (T-7109). Non-condensable gas at the con-cooler is connected to the vacuum
system (vacuum pump (Z-7101AB), a ring-oiled vacuum pump). Phenol oil, naphthalene oil and
wash oil are extracted from the side of the distillation tower (due to the diversity of raw material
and instability of constituents, more standby side outlets shall be provided at the distillation
tower), cooled at the three-mix cooler (E-7109) and then sent to the intermediate tank
(T-7105AB) of mixed constituents. The I-anthracene oil extracted from the bottom will be sent to
the cooler (E-7107) via I-anthracene oil extraction pump (P-7109AB), cooled and put into the
I-anthracene oil tank (T-7106), among which parts of them are sent to the pitch tower for reflux
(K-7102) via the I-anthracene oil reflux pump (P-7106AB).

8 Quality of Raw Materials and Products

8.1 Quality of raw materials

8.1.1 Tar YB/T5075—93

8
 Item Index
1# 2#
Density (ρ20) g/ml 1.15 ~ 1.21 1.13 ~ 1.22
Toluene insoluble 3.5 ~ 7.0 ≯9
(moisture-free basis) %
Ash content (weight) % ≯ 0.13 ≯ 0.13

Moisture (weight) % ≯ 4.0 ≯ 4.0

Viscosity (E80) ≯ 4.0 ≯ 4.2
Naphthalene content ≮ 7.0 ≮ 7.0
(moisture-free basis)%

8.1.2 Sodium hydroxide GB209—84

Item Index
Diaphragm Diaphragm solid alkali
liquid alkali First Second
Content of sodium ≥42.0 ≥96.0 ≥95.0
hydroxide ％

Content of sodium ≤0.80 ≤1.4 ≤1.8

carbonate ％
Content of sodium ≤2.0 ≤2.8 ≤3.3
chloride ％
Content of iron ≤0.01 ≤0.01 ≤0.02
sesquioxide ％

8.1.3 Dilute sodium hydroxide solution (self-made)

Item Index
Concentration % 8 ~ 12
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 8.2 Specification of products

8.2.1 Light QB001—2007

Item Index
Appearance Yellow transparent liquid
Density (20℃) g/ml 0.88 ~ 0.946
Phenol content (volume)% ≯ 2.5
Naphthalene content (weight)% ≯ 5
Moisture % ≯ 2
Distillation test
Initial boiling point ℃ ≮ 90
Distillation production before 180℃ ml ≮ 90

8.2.2 I-anthracene oil QB002—2007

Item Index
Density (20℃) g/ml 1.11 ~ 1.14
Phenol content % ≯ 0.4
Naphthalene content % ≯ 3
Distillation test
Initial boiling point ＞ 270℃
Distillation production before 300℃ ≯ 10
(weight) %
Distillation production before 360℃ 65 ~ 85
(weight) %
Moisture content (weight) % ≯ 5

8.2.3 Ⅱ-anthracene oil QB003—2007

Item Index

10
 Density (20℃) g/ml 1.15 ~ 1.19
Phenol content % ≯ 0.2
Naphthalene content % ≯ 1
Distillation test
Initial boiling point ℃ ≥ 300℃
Distillation production before 360℃ ≤ 15
(weight) %

Moisture content (weight) % ≯ 5

8.2.4 Pitch GB/T2290—94

Item Index
Low-temperature pitch Mid-temperature pitch High-temperature
pitch
1# 2# 1# 2#
Softening point 35 ~ 45 46 ~ 75 80 ~ 90 75 ~ 95 95 ~ 120
(ring and ball
method) ℃
Content of toluene 15 ~ 25 ＜25
insoluble %
Ash content % ≯0.3 ≯0.5
Moisture % ≯5 ≯5 5
Volatile component 58 ~ 68 55 ~ 75
%
Content of ≯10
quinoline insoluble
%

8.2.5 Phenol oil QB004—2007

Item Index
11
 Moisture % ≯2
Naphthalene content (weight) % ≯ 18
Phenol content (volume) % ≯ 0.5
Distillation production before ≯ 45
200℃(weight) %

8.2.6 Unwashed mixed distillate: QB007—2006

Item Index
Density (20℃) g/ml 1.008 ~ 1.032
Naphthalene content (weight) % 45—55
Phenol content (volume) % ＜ 15
Distillation test
Initial boiling point ℃ 195 ~ 205
Dry point ℃ 280±2

9 Main Operating Parameters

9.1 Temperature of oil products

(1) Temperature of tar through tar/pitch heat exchanger: 200℃;

(2) Temperature of tar after being heated by tar pre-heater: 120℃;
(3) Temperature of gas after being treated by the vacuum non-condensable gas cooler: 40℃;
(4) Temperature of light oil within oil-water separator: 35 ~ 50℃;
(5) Temperature after being treated by phenol oil con-cooler: 70℃;
(6) Temperature after being treated by naphthalene oil cooler: 80 ~ 90℃;
(7) Temperature after being treated by anthracene oil cooler: 90 ~ 105℃。
9.2 Temperature of materials through tube heating furnace

(1) Temperature of outlet at convection section of tube furnace: 190 ~ 245℃;

(2) Temperature of outlet at the radiation section of tube furnace: 340 ~ 360℃ (road binder,
mid-temperature pitch);
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 (3) Temperature of outlet at the radiation section of tube furnace: 360 ~ 390℃
(high-temperature pitch);
(4) Temperature of outlet of the superheated steam: 400 ~ 550℃.
9.3 Parameters of each tower

(1) Temperature at top of dewatering tower: 100 ~ 110℃, temperature at bottom of tower:
235 ~ 245℃;
(2) Temperature at top of pitch tower 315±5℃, temperature at bottom of tower 340 ~ 365℃;
(3) Temperature at top of distillation tower 170±5℃；
(4) Pressure at top of dewatering tower: 15 ~ 35KPa, pressure at bottom: 45 ~ 65 KPa；
(5) Pressure at bottom of pitch tower: -40 ~ -70 KPa；
(6) Working pressure at distillation tower: -50 ~ -80 KPa；
(7) Temperature of mixed distillate in the distillation tower at the time of extraction 185 ~
205℃, temperature of anthracene at the time of extraction: 260 ~ 310℃。
(8) Temperature of oil and gas temperature at top of distillation tower: 170 ~ 190℃.
9.4 Operation parameters for tube heating furnace

(1) Temperature of hearth of tube furnace ≯800℃.

(2) Temperature at convection section of tube furnace: ≯600℃
(3) Pressure of general pipe of fuel >0.6MPa.
(4) Temperature of wasted gas of fume pipe ≯270℃.
(5) Coefficient of excess of air in the front of nozzle 1.4 ~ 1.5.
(6) Superheated steam flowing into the distillation tower ≯400kg/hr.
9.5 Oil temperature at the outlet of each con-cooler:

Light oil 35±5℃ Ⅰ, Ⅱ anthracene oil: 80 ~ 120℃

Mixture: 80 ~ 100℃ High temperature pitch: 230 ~ 300℃
Water temperature at the outlet of each
cooler <45℃

9.6 Level at the bottom of each tower

The level meter shall be kept at 40% ~ 70%.

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10 Basic Requirements for Working Process

10.1 Preparation

Wear protective supplies accordingly, and keep a good mental state.

10.2 Pre-production meeting

Learn about the considerations about production, safety and environmental protection, fire
protection and other information about this work.
10.3 Inspection for taking over shift

Check if safety protective products, fire-fighting, environmental facilities and working tools
are complete and available and can meet the production needs.
10.4 Evaluation of operating conditions

Fill in KYT card according to the actual situation, and look for safety hazards. Check if
human resources, natural resources, equipment and tools, and safety environment meet the
production requirements, if not, timely report to the team leader, and do not carry out the
operation until all issues are solved.
10.5 Operating process

10.5.1 Start-up preparations:

10.5.1.1 For those equipment and pipes that are newly overhauled or newly brought into
production, they should receive single test (the air-tight test should be done for the
depressurizing system after overhaul), and not put into production until they pass the test.
10.5.1.2 Check the storage amount of light oil and phenol oil, the temperature, quality and
storage amount of tar, and check if the flow meter, pressure gauge, thermometer, level gauge and
such measurement equipment and water seal meet the technical requirements.
10.5.1.3 Preheat the jacket of the attached pipes and jacketed pump and valves within this device
before delivering steam. Blow the following pipes with steam:
(1) Inlet for crude tar to dewatering tower → anhydrous tar/soft pitch heat exchanger → tar
preheater → crude tar delivery pump → crude tar tank.
(2) Outlet of anhydrous tar of dewatering tower → circulating pump of anhydrous tar →

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convection section of tube furnace → dewatering tower → condensate cooler of light oil →
oil-water separator → light oil reflux tank → light oil product tank.
Oil-water separator → phenol water tank
(3) Dewatering tower, pitch tower, distillation tower → blowing tank, startup & shutdown
tank.
(4) Dewatering tower → reflux pump of light oil → reflux tank of light oil
(5) Dewatering tower → anhydrous tar pump → radiation section of tube furnace → pitch
tower → distillation tower → phenol oil condensate cooler → the vacuum non-condensable gas
cooler → oil-water separator → reflux tank of phenol oil → product tank of phenol oil.
Oil-water separator → phenol water tank
(6) Pitch tower → tar intermediate tank
(7) Distillation tower → mixture cooler → mixture receiving tank.
(8) Ⅱ-anthracene side→Ⅱ anthracene oil cooler→Ⅱ-anthracene oil storage tank.
(9) Distillation tower→Ⅰ-anthracene oil extraction pump→Ⅰ-anthracene oil
cooler→Ⅰ-anthracene oil storage tank.
(10) Distillation tower → reflux pump of phenol oil → reflux tank of phenol oil
(11) Pitch tower←Ⅰ-anthracene oil reflux pump→Ⅰ-anthracene oil storage tank.
(12) Empty pipes for each tower, blow off pipes for all equipment.
10.5.1.4 Deliver steam to the superheated steam pipe of the tube furnace, whose operation should
strictly comply with the operation procedure for tube furnace.
10.5.1.5 Deliver steam into each steam pipe, and check if the condensate water discharging
system is in good condition and the location of each valve is in correct place.
10.5.1.6 Add water into coolers, inlet steam and preheat to 70~80℃.
10.5.2 Start-up operation
10.5.2.1 Cold circulation operation:
① When everything is ready, notify the oil depot of turning on the crude tar pump, and start
to deliver tars to the dewatering tower.
(2) When the tar level in the dewatering tower is beyond the 50% height, turn on the
circulating pump of the tower, and deliver tars to the tube furnace. After the liquid level is stable,

15
turn on the extraction pump of anhydrous tars to deliver tars to the radiation section of the
extraction pump of anhydrous tars, of which the volume is 0 ~ 1 m³/h less than the primary
section (it turns to 0.5 ~ 1 m³/h after being normal). Adjust extraction volume of crude tars and
anhydrous tars, which enter the startup & shutdown tank.
(3) During cold circulation, check if the pump functions properly, pipelines of tar, flange
and valve are in good condition, and the return bend on the heating pipe of tube furnace has no
leakage. Check if the instrument and meter are correct, and the safety valve is in good condition.
10.5.2.2 Check the discharge pipeline
(1) Check if the level of water in the oil-water separator is over the feeding outlet, and there
is certain water in the receiving tank of phenol oil, and keep the liquid seal.
(2) Confirm that blow off valves for air has been turned on.
10.5.2.3 Thermal circulation operation:
(1) During cold circulation operation, frequently check if equipment, pipelines and metering
devices are in good condition. When no fault has been detected, fill the tar preheater with steam
to heat up. Then fire up the tar tube furnace. (Before ignition, empty the flashing from the steam
pipe, and then blow the steam into the hearth until the steam pours out of the chimney.) Carry out
the ignition operation in strict accordance with the operation steps for heated furnace.
(2) When the temperature at the top of dewatering tank is beyond 80℃, slightly turn on the
cooling water of dewatering tank of light oil tower for condensation and cooling (at the
beginning of start-up, the condenser is filled with steam. Close it after being normal).
(3) When the temperature at the bottom of dewatering tank is beyond 120℃, the preheater
of dewatering tank will be filled with steam for further warming up. When the temperature at the
top of dewatering tank is beyond 95℃, turn on the reflux pump of dewatering tank for reflux.
Use a regulator to make manual adjustment. The temperature at the top of tower is limited at
95—105℃, and then set the regulator to automatic return, and set the temperature regulator to 95
~ 105℃ (the temperature is subject to the quality of products).
10.5.2.4 Reflux of light oil at dewatering tower
(1) Turn on the front and back valves of the flow meter on the reflux pipes and the front and
back valves of the regulation valve of the flow meter.

16
 (2) Control the temperature at the top of tower through little reflux.
10.5.2.5 The temperature at the bottom of dewatering tank shall be kept at 140—150℃.
Continue the thermal circulation for about 1 hour and the tar water content will be removed.
10.5.2.6 During the thermal circulation, ammonia water and light oil are distilled from the top of
the dewatering tower.
10.5.2.7 Observe the level of light oil of the level meter in the oil-water separator and the
condition of the light oil overflowing into the intermediate tank. After overflowing, the light oil
would return to the crude tar pump.
10.5.2.8 Prepare to reduce the pressure of the main tower
(1) Confirm that the exhaust and purification tower has been put into operation.
(2) Before start-up, check and confirm that the vacuum pump could run properly.
(3) Check the injection pipeline of discharge pipeline.
(4) Start the vacuum pump
10.5.2.4 Start to reduce the pressure (after treated by the dewatering tank, the tar water shall be
less than 0.1%).
(1) Turn off the bypass valve and air blow off valve at the suction side, and turn on the
valve leading to exhaust and purification tower.
(2) Slowly turn on the suction valve, and the depressurizing speed at the top of main tower
shall be -665Pa/min.
(3) Keep the negative pressure stable.
10.5.2.5 After the tube furnace starts to heat up, the temperature of the tar outlet at the
convection section shall be increased at a speed of 50 ~ 60℃ per hour, so as to rise up to normal
operation temperature within 4~6 hours.
10.5.2.6 When the tar temperature at the radiation section is up to 150℃, check the running
condition and keep the temperature constantly for 1 hour.
10.5.2.7 During thermal circulation, further check the tar pump, heating furnace pipe, connecting
pipes, flange and bend.
10.5.3 Normal operation
10.5.3.1 Dewatering system

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 (1) The tar filling temperature of dewatering tank shall be limited within 120~165℃.
(2) The internal temperature of light oil separator shall be limited less than 50℃. In case the
temperature is over low, adjust the cooling water flow of light oil condenser.
(3) The temperature at the top of dewatering tank shall be limited around 95-105℃.
(4) Check if the separating layer of each light oil separator stays at 50% of liquid level
meter. Regulate the amount of water release of oil-water separator, and keep this level.
10.5.3.2 Regulation of distillation tower
(1) Regulation of temperature at bottom of the tower (heating).
(2) Regulation of the extraction volume of naphthalene wash oil.
(3) Regulation of the extraction volume of anthracene oil.
(4) Regulation of temperature at top of the tower (reflux).
10.5.3.3 Quick method to determine the naphthalene content of phenol oil: Expose sample of
phenol oil in air, if crystallization of naphthalene separates out, it means the naphthalene content
of phenol oil is high, it should properly reduce the temperature at top of tower.
10.5.3.4 Heating furnace system
(1) Regularly check the combustion state of each burner, and keep it stable. Carefully
regulate the ventilation door and the chimney flap every time.
(2) Regularly visually inspect the appearance of heating tube and be aware of abnormal
state including local color change in early time.
10.5.3.5 Exhaust and purification system
Check the quality and level of the wash oil in the exhaust and purification tower and replace
at regular intervals.
10.5.3.6 During the production of carbon black oil, if the temperature at the radiation section is
up to 250℃, switch to the carbon black oil tank (this operation could be regulated by the
manufacturers according to market demand).
10.5.3.7 To ensure the quality of I-anthracene oil, the temperature at the top of the pitch tower
should be kept at 295±5℃ and use a control valve to automatically adjust. If the automatic
control valve fails, use the bypass pipe of the anthracene oil reflux pump to regulate.
10.5.3.8 The important index for the distillation tower is to guarantee the quality of the phenol

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oil and mixed distillate, therefore, the temperature at the top of the tower is required to keep
between 160 ~ 180℃, and to be regulated through the control valve automatically. If the control
valve fails, use the bypass pipe of the phenol oil reflux pump to regulate.
10.5.3.9 Use a control valve to regulate the superheat steam before flowing into the tower, and
the supply into the tower should be even, avoiding sudden change.
10.5.3.10 Regulation method of the distillate quality
(1) The quality of I-anthracene oil can ensure the temperature at the top of pitch tower, and
the heated steam of distillation tower can also be used for adjustment.
(2) Make use of the amount of the reflux rate of the phenol oil to control the temperature at
the top of the distillation tower, to ensure the quality of the phenol oil.
(3) Mixture can be extracted from different outlets. The quality can be adjusted by the side
opening.
(4) The pitch quality can be controlled by adjusting the outlet temperature at the radiation
section of tube furnace. (During production of carbon black oil, appropriate amount of
anthracene oils can be added).
(5) The distillate extract outlet is not allowed to be altered at will. Any change shall be
approved by the personnel in charge.
10.5.3.11 Operation of con-cooler, cooler and oil-water separator
(1) The volume of cooling water can be used to adjust the temperature of con-cooler, so as
to meet with regulated technical indexes.
(2) The liquid level of oil-water separator shall be kept at 50%.
10.5.3.12 Fill in the operation record form to record the regulation information about the above
systems every hour. Always check the power (fuel, water, electricity, steam) and equipment
functioning.
10.5.4 Stoppage operation
10.5.4.1 Within four hours before shutdown, stop feeding to the tar intermediate tank to reduce
the level.
10.5.4.2 Switch all instruments from automatic mode to manual mode at proper time.
10.5.4.3 Turn off the fuel system of tube furnace, and stop heating.

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10.5.4.4 When the temperature at the radiation section is down to 150℃, turn off the raw
material pump and anhydrous tar pump. Blow the tar from the heating pipe at convection section
to the dewatering tower until the pipes are unblocked. Turn off the vacuum system in real time.
10.5.4.5 After emptying the dewatering tower, turn off the pump at the bottom of tower. Blow the
tar in the heating pipe at the radiation section of tube furnace to the pitch tower until the pipes
are unblocked.
10.5.4.6 When the temperature at the outlet of superheat steam is down to 360 ℃, stop delivering
steam into each tower. After completing stoppage of the tube furnace, turn off the reflux of
I-anthracene oil, and blow the reflux pipe with steam.
10.5.4.7 When the temperature at the top of the distillation tower is down to 100℃, stop the
reflux of the phenol oil, blow the reflux pipe and the outlet pipe of the pump with steam, turn off
the mixture side and I-anthracene oil, and blow the respective pipes with steam.
10.5.4.8 Stop the cooling water to the con-cooler.
10.5.4.9 When the temperature at the bottom of the tower is lower than 150℃, slowly discharge
the oil into the intermediate tank to avoid oil expelling.
10.5.4.10 Stop running all instruments.
10.5.5 Special operations
10.5.5.1 Emergently stop the heating furnace
(1) Turn off the fuel valve, and stop heating.
(2) The hearth is filled with fire extinction steam (nebulization gas can continue).
(3) Turn on the flue flap, and open all observation holes.
(4) Stop pumps at the convection section and radiation section, blow the tar in the heating
pipes at convection section and radiation section into the dewatering tower and pitch tower. If the
steam pressure is insufficient, blow the tar in the pipes of the heating furnace at the radiation
section into the pitch tower, continuously connect the steam into the hearth, until the temperature
is down to 150 ~ 200℃.
(5) If the production could not resume immediately, stop the heating furnace and continue
the next step.
10.5.5.2 If the elbow or furnace tube of tube furnace is damaged, only with a little leakage or

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smoke, stop the heating furnace in general process; if there is much leakage, promptly stop the
heating furnace; if a fire occurs following with oil leakage, with exception to emergency stop of
heating furnace, notify the fire brigade, and report to the dispatch room to organize personnel for
a rescue.
10.5.5.3 If the temperature of the outlet of the tube furnace at the radiation section increases
suddenly and is over the specified number,
(1) Check if the associated anhydrous tar pumps are in good condition, if fail, switch to the
stand-by pump, and promptly stop the heating furnace if switching fails.
(2) Check the bottom of the dewatering tower, if it is empty, it should increase the
knock-out volume for the pumps at the convection section to keep the level stable.
10.5.5.4 Pressure increases via the pump at radiation section
Take samples from the tar at convection section and radiation section for test. If the
moisture is excessive, the operation of dewatering in standing state and dewatering of centrifuge
should be strengthened. If the moisture is not much but the pressure continues to increase, and
the outlet temperature at the radiation section gradually increases, this case may be caused by
coking in the furnace, and the production should be shut down.
10.5.5.5 Pressure increases in distillation tower and the entire system
(1) Check if the condenser-cooler is blocked and that the cooling water is uninterrupted. If it
is blocked, the operator should promptly try to unplug; if the cooling water interrupts, the
operator should report to the dispatch room to shut down.
(2) If the condenser-cooler functions well, the interruption of discharging is due to the
blockage of the tower tray, this case, it should be shut down.
10.5.5.6 The temperature at the top of tower increases suddenly
Check if the flow of reflux pump continues, and find out the reasons. If the reflux pump
fails, switch to the stand-by pump and notify the maintenance personnel to repair the pump; if
the reason is high temperature of oil, regulate the volume of the water supplied to the
condenser-cooler to reduce the temperature of the reflux oil.
10.5.5.7 Blockage of pipes on the condenser-cooler
The production should be stopped if the oil temperature at the outlet of the condenser-cooler

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rises and the water temperature increases, and the pressure of the tower increases.
10.5.5.8 Fuel pressure reduces
If the fuel pressure is too low to meet the requirements of normal production, the soft point
of the pitch should be regulated, and the volume of the feeding could be reduced, and then check
the fuel pump and switch to another pumps; if the fuel pressure continues to decline less than
0.3MPa, the production should be shut down.
10.5.6 Safety precautions
(1) Keep the release pipelines and the inactive pipelines unblocked at any time.
(2) Do not shut off the bypass valve on the fuel control valve.
(3) Empty flashing before blowing.
(4) At the time of startup and shutdown, slowly process every step, and do not pour the oil
with large temperature difference into the storage tank to avoid oil expelling.
(5) Regularly check equipment, pipelines, pressure gauge, thermometer and level meter, and
take prompt measurements if any failure arises.
(6) Always check the fire extinction facilities of the tube furnace to keep them in good
condition.
(7) The overhaul for equipment and pipes should be processed after pressure relief, empty
and clean. A sign should be marked for ignition of pipes and running of equipment.
10.6 Summary of operating status

10.6.1 Implement the operation technology specification as required.

10.6.2 Check and maintain all equipment and facilities to ensure their correct operation.
10.6.3 Analyze, summarize and record all information related to safety and environmental
protection, operation and equipment. Timely handle the abnormal situation in the process of
production to ensure that the equipment and facilities operate in safe and stable condition.
10.7 Shift exchange

10.7.1 Clear various original records.

10.7.2 Describe the situations related to the shift production, safety, environment, and
notifications and orders of superiors.
10.7.3 Hand over the original records and tools and instruments.
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10.7.4 Tell the personnel of the next shift about safety considerations and precautions.
10.8 After-production activities

10.8.1 Participate in the analysis related to production, quality abnormity or accident, analyze
and summarize the production and abnormity conditions on duty to identify issues and to
develop solutions.
10.8.2 Participate in related training as required.

11 Standard revision history (refer to Appendix A)

Appendix A
(Specification appendix)
Document change history

Items to Condition of change Date of change

change (approval)

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