PARAMETRIC STUDY ON THE NAOH PRE-TREATMENT

OF NON-METALLIC FRACTION OF WASTE PRINTED

CIRCUIT BOARDS FOR HYDROGEN BROMIDE
EMISSION REDUCTION DURING
PYROLYSIS

NIKA BARRAMEDA
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1. INTRODUCTION

1.1. Background of the Study

In this modern age, electronic gadgets have become a necessity. It is integrated in our social

and economic lifestyles, much so that its development is still growing rapidly. Due to this rapid

growth, electronic products are designed to last much shorter in order to make way for the new

and upcoming products. This means that there is a huge stream of electronic wastes (e-waste) along

the development of the electrical and electronics industry. According to Ilankoon, Ghorbani, Nan,

Herath, & Moyo (2018) e-waste generated annually in the world is estimated to have an increasing

rate of 3-5%.

An electrical and electronic equipment, or an EEE, contains a printed circuit board that

holds and connects the necessary electronic components needed for an EEE to function and serve

its purpose. Once it no longer functions or is replaced, the PCB becomes the primary e-waste of

concern. This is because it is made up of metals, plastics and organic compounds which are proven

to be toxic and hazardous environmental pollutant, if not disposed of properly.

The non-metallic fraction is commonly dumped to landfills or sent to incinerators.

However, dumping and incinerating of these fraction can cause pollution because it will produce

leachate and toxic fumes – primarily dioxins and furans. According to Sohaili, Muniyandi, &

Mohamad (2012), these types of wastes need to be recycled to recover the reusable resources and

lessen waste disposal that could harm the people and the environment.

They also reviewed the different researches that reuse the non-metallic fractions. The

studies listed takes advantages on the physical properties of the wastes and is therefore used as

fillers for construction materials, composite boards and others alike. On another study, Guanghan,
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Zhu, Wenyi, Chenglong, & Wen (2016) noted some of the chemical process’s useful derivatives

of the wastes. They cited researchers that employ pyrolysis to produce oils and gases that can be

used as fuel and reinforcement for materials. However, its most significant disadvantage is the

formation of harmful dioxins, furans and other harmful gases. In a study by Shen, Chen, Ge, &

Chen (2018), they identified the composition of the char from the pyrolysis of non-metallic waste

PCBs and from there, determined the appropriate pre-treatment process that will lower harmful

pollutant emission upon pyrolysis. In this study, the alkali pre-treatment process parameters using

NaOH will be investigated.

1.2. Significance of the Study

In printed circuit board manufacturing, both metal and non-metal substances are used. This

therefore create a heterogeneous waste that has high economic value and high pollution potential.

Studies on the recycling of these wastes are conducted in order to reduce toxic waste disposal,

recover the aforementioned resources, and increase possible profits for the company. The recycling

of the non-metallic fraction of waste PCBs are now taken into consideration to prevent resource

wasting and possible pollution. One of the promising researches are on the pyrolysis of NMF-

WPCBs, however this process generate hazardous fumes of HBr. The pursuit of this study can help

in the reduction of HBr emission by fixation of Br to the char. It can help in the development of a

large-scale plant that recovers all the resources from printed circuit board without the problem of

releasing harmful fumes and pollutants. It can also encourage electronics manufacturing

companies to uphold the extended producer responsibility due to its economic benefits.
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1.3. Objectives of the Study

The study generally aims to reduce HBr gas emission during pyrolysis of NMF-WPCBs

during pyrolysis by pre-treatment using NaOH for the fixation of bromine to char. For the

achievement of the general objective, the study aims to:

1. Separate the metallic and non-metallic fraction by physical processes;

2. Investigate the effect of soaking time, temperature, and weight loading of non-

metallic WPCBs and NaOH on the fixation of bromine to char;

3. Determine the composition of pyrolysis by-products through char characterization by

thermogravimetric method, and gas analysis by gas chromatography; and

4. Describe the relationship of the NaBr formation with respect to NaOH treatment

parameters during pyrolysis of NMF-WPCBs.

1.4.Scope and Limitations of the Study

Printed circuit boards collected from junkshops will be used. A fabricated pyrolyzer with

gas collection system will be utilized because of the unavailability of the equipment. Only NaBr

formation will be considered during the pyrolysis of NMF-WPCBs. The composition of oil will

not be characterized because it is assumed that there are no Br contamination in the oils.
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1.5.Time and Place of the Study

The experiment will be conducted from August to October 2019 at the Department of

Chemical Engineering and Agro-Industrial Technology, University of the Philippines, Los Baños,

Laguna.
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2. Review of Related Literature

2.1.Electrical and Electronic Equipment in the Philippines

Electrical and electronic equipment (EEE) is identified to be any device that requires a

battery or a power supply to function, operates at 1000V (AC) or 1500V (DC) and is under any

legal exemptions. It is also categorized to six types: (1) temperature exchange equipment, (2)

screens, monitors, and equipment containing screens with surface greater than 100 cm2, (3) Lamps,

(4) Large equipment which are greater than 50cm, (5) small equipment, and (6) small IT and

telecommunications equipment with no external dimensions greater than 50cm (Balde, Forti, Gray,

Kuehr, & Stegmann, 2017).

One of the most commonly observed electronic gadget used by the Filipinos are cellphones

which falls under the sixth category. Last 2015, it is estimated that around 65.3% of the Filipino

population has owned a mobile device and by 2022 it will increase to 69.2% of the population

(Statista, 2014). The 2015 census showed that there are 101, 716, 359 Filipinos and by 2025 the

number will reach to about 117, 664, 680. This data alone can be used to predict the amount of

electrical waste from one of the EEE category alone. It is also important to note that in today’s

society it is common for people to have more than one of these devices.

The increase in use of EEE could be attributed to the increase in the cost of living of the

world to catch-up on the pace of development and the lowering of the standards of some producers

and markets that allows consumers to purchase products at an affordable price with the sacrifice of

quality. The sacrifice of quality can be observed by the low life expectancy of the gadget wherein

in just a course of few months, the product becomes unusable. Since it is cheaper and there are
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more new features developed in the market, consumers will tend to purchase again and dispose of

the old ones.

An integral part of the EEE is the printed circuit board (PCB) which comprises of about

5% of the total volume of the equipment. The percentage is quite small, but the most important

function of the whole EEE could be traced back to this core. It also contains valuable substances

that have high economic values. Further discussion regarding waste generation will be made to

provide the context of the amount of PCB discarded around the world.

2.2. Waste Generation and Recycling of Printed Circuit Boards

Over the past two decades, the technological development in the world had grown

exponentially giving rise to complex and reliable gadgets and equipment used today. This

increased the demand for an easily accessible and affordable product because world has leaned

towards the reliability for communication, comfort in living and productive capacity of individuals

in all aspects of life. The consequences, however, is that technological advancements also mean

that there are by-product of wastes that are harmful for both the environment and the people.

The figure below shows that there is an increasing rate of e-waste generated annually in

the world. It is even estimated that by 2021 there will be 52.2 megatons of e-waste with every

person generating e-waste at a rate of 6.8 kg/ inhabitant. Their gathered data also shown that Asia

alone contributed to about 40.7% of the world’s e-waste amounting to about 18.2 megatons. The

problem with these wastes is that it contains large amounts of hazardous substances not properly

collected and disposed and that amount of high value products are wasted.
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Figure 2-1. Annual world trend of e-waste generation

by the world and per individual
Source: Baldé, Forti, Gray, Kuehr, & Stegmann (2017).

Around 2.7 megatons of e-waste in Asia have proper documentation of collection and

recycling. Compared to the predicted actual e-waste generated, it is only a small fraction (Baldé et

al., 2017). The rest could be stocked in houses until final disposal, brought to informal recycling

facilities, or chucked to the nearest trash can for disposal in landfills or incinerators. Informal

recycling facilities takes on these wastes because of the precious metals of copper, gold and the

like which can be sold at higher prices.

Recycling of printed circuit boards can be divided into two categories – the physical

processes and the chemical processes. The physical process does not alter or change the chemical

composition of the substance as opposed to the chemical processes. It mostly deals with the size

reduction and separation of the components of the printed circuit board – metal and non-metal.

This type of process is commonly done by self-established recycling facilities. On the other hand,

chemical processes use substances that could leach out precious metals from the printed circuit

board or use heat to decompose the organic material present in the substance. Both of this could

also be used hand-in-hand to effectively separate and recycle the high value product recovered.
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2.3.Recovery of Resources from Waste Printed Circuit Boards

The accumulation of e-waste containing, collectively, high economic value resource

becomes a subject for research. In earlier studies, metals recovery was focused on because of its

higher resource value compared to the recycling of the non-metallic fraction which are often

disposed of in landfills or incinerated. The problem with these disposal methods is that it is a

potential avenue for the release of harmful chemical substances that can cause health hazards and

environmental pollution. In order to address this problem, there are studies conducted that recycle

these wastes without harmful environmental pollution.

Before any recycling is done, the PCBs are subjected to size reduction. It is the preliminary

step for the preparation of PCBs. Size reduction can be done by shredding, grinding or crusher.

These equipment have sieves that allows passage of the desired particle size for treatment. Some

of the equipment are hammer mills, rotary crushers, ball mills and shredders (Kaya, 2016). These

are often used to produce particle sizes of 0.023 to 0.003 inches (Perry, Green, & Maloney, 1997).

After size reduction the ground PCB will be subjected to either physical or chemical treatment to

separate the metallic and non-metallic portions.

The easiest and low cost of recycling of the non-metallic part is through the physical

processes of separation. This method include sieving, corona electrostatic separation, drum

separators and sink-float separation among others (Kanchanapiya, Metal, & Kwonpongsagoon,

2015; Sohaili et al., 2012).

Once the metal and non-metallic fractions are separated, the NMF can be used as fillers for

concrete and other composite products that requires great mechanical strength. It can also improve

the flexural strength of composite boards allowing it to hold greater bending stresses. Another
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component of printed circuit board is the epoxy resin which has great compatibility to resin

adhesives that improves binding and molding capabilities (Sohaili et al., 2012).

As for the chemical processes of recycling, pyrolysis and gasification were researched by

some of the scientists. Due to the chemical characteristics of most part of the PCB, it can easily be

degraded by the pyrolysis process. Pyrolysis products include oil, char and gasses. The oil can be

used as fuel source once refined (Kaya, 2016; Sohaili et al., 2012; Shen et al., 2018). According to

the study, the oil contains components of phenol, isopropyl phenol and bisphenol A. These oils

can be used to recover the resin used and the char can be used as raw material for carbon nanotubes

and other adsorbents and also, the char containing glass fibers, metal and resin can also be used as

fillers similar to those obtained from the physical separation (Guanghan et al., 2016).

2.4.The Non-Metallic Fraction of Waste Printed Circuit Boards (NMF-WPCBs)

The substrate of the PCB is made-up of an epoxy resin. This epoxy resin is made by

reacting tetrabromobisphenol-A with epoxy. The bromine in bisphenol acts as the flame retardant

in case the electrical equipment experience short circuits or other fire hazards. If an electrical

equipment is on fire, the chemicals incorporated in the substrate of the printed circuit boards are

released. Based on the structure, the hydrogen in bisphenol-A is replaced by four bromines in

tetrabromo-bisphenol A. In the case of PCB without the fire retardant, the burning board will

release H2 gases, which are also flammable. It adds more fuel to the fire. However, in the case of

the tetrabromo-bisphenol, the burning forms radical bromine. This bromine will then compete with

any chemical formation that will sustain the flame. The fire-retardant is classified as halogenated

fire-retardant (IPCS INCHEM, n.d.).

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(a)

(b)

Figure 2-2. Structure of (a) tetrabromobisphenol-A

and (b) bisphenol-A
Source: Pecht and Deng, 2006 and Hoban and
Soucheray, 2012

The pyrolysis of this substrate will release the harmful HBr gas, as concluded by different

studies which pyrolyze PCBs. This lead to research on the inhibition of HBr gas. One study focused

on the addition of alkali substances such as NaOH, KOH, K2CO3, and Na2CO3. The results showed

that the NaOH has the highest brome fixation efficiency of about 53.6% (Ghosh, Ghosh, Parhi,

Mukherjee, & Mishra, 2015; Shen et al., 2018). Using this as reference, the study will be improving

on the bromine fixation of NaOH by exploring the different parameters.

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3. MATERIALS AND METHODS

3.1. General Process Flow Chart

The general methods for the experiment are divided into 4 parts: (1) Sample Preparation,

(2) NaOH Treatment, (3) Pyrolysis and (4) Analysis. Consider figure 1. The different colored

shapes represent the different parts of the experiment; wherein green is for sample preparation,

blue for the NaOH treatment, orange for the pyrolysis and yellow for the analysis.

Figure 3-1. Overall process flowchart

3.2. Experimental Design

The study aims to reduce HBr gas emission during pyrolysis of NMF-WPCBs during

pyrolysis by pre-treatment using NaOH for the fixation of bromine to char. Three parameters were

chosen, specifically, temperature of NaOH solution, weight loading by % weight per weight of
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NMF-WPCBs to NaOH pellet, and soaking time of NMF-WPCBs in NaOH solution to investigate

effectiveness of bromine fixation. Consider table 1 for the experimental parameters to be explored

wherein the values for reference are based on Shen et. al (2018).

Table 3-1. Experimental parameters

PARAMETER REFERENCE A B
Temperature, C 20 30 40
Weight loading, %w/w 5:1 5:1.5 5:2
Time, hrs. 2 4 6

Two trials will be performed for the study for each of the combinations. By 2-K factorial,

the runs will be generated from Design Expert.

3.3. Preparation of Non-Metallic Fraction of WPCBs

First part of the experiment is the preparation of the samples. The main material that will

be used for the experiment is the NMF-WPCBs therefore metallic and non-metallic portions of the

collected WPCBs must be separated. In this study, the physical separation process will only be

done and will be based on the conclusion by Warapon as cited and conducted by Kanchanapiya,

Metal, & Kwonpongsagoon (2015) that particle sizes less than 150m was proven to contain

almost 100% non-metallic fraction.

The obtained waste printed circuit board will undergo size reduction first using a rotary

cutter mill. A screen with mesh number 150 and opening size of 0.149mm will be used to make

sure that the portion collected will mostly contain the non-metallic fraction. It is assumed that the

physical processes are enough to separate the metallic and non-metallic portion however if

characterization shows otherwise the experiment can still proceed as planned because it is assumed
 13

that metal contamination will not affect any bromine fixation to char. Kaya (2016) discussed that

a method of recovery for metals is the use of pyrolysis which depolymerizes the substrate and not

affecting the metal. The separation only makes sure that the precious metals will easily be

recovered for other purposes and that the char will be readily used for fillers in composite board;

which is not part of the study. After sample preparation is the experiment proper where the

different parameters that could affect bromine fixation to char will be investigated.

3.4. Experiment Proper

Treatment with NaOH. The NaOH treatment is the main part of the experiment because

the parameters needed during this step will be investigated for the bromine fixation efficiency.

Figure 3-2 shows the experimental set-up for NaOH soaking.

Figure 3-2. NaOH treatment set-up

The experiment will be using a round bottom flask, containing the sample and solution

with a magnetic stirrer, placed on a hot-water bath maintained at the temperature given by the run.

15g of NMF-WPCBs will be mixed with 3g, 4.5g, and 6g of NaOH for the ratios of 1, 1.5

and 2, respectively. It will be placed into the flask and 904ml of distilled water will be added for

each set-up. As the ratio of NaOH increases, the concentration of the solution increases. The
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solution will be stirred for 2hrs, 4hrs, and 6hrs at the given temperatures, both depending on the

conditions.

After that, the mixture will be filtered using a simple filtration set-up using filter paper.

The residue will be collected, and oven dried at 105C for 1hr. The oven-dried, chemically pre-

treated samples will then be used for pyrolysis.

Figure 3-3. Schematic pyrolysis set-up by Shen, Y. et.al (2018)

A fabricated pyrolysis equipment similar to figure 1 will be used. A gas collection system

is installed to collect the gases produced during the experimental proper. This will contain any

unreacted HBr gases and it will be accounted for in the calculation of bromine fixation efficiency.

The collected gas will be analyzed using gas chromatography. Their set-up also contains a liquid

collection system for oil production. However, since this study assumes that no bromine will leach

into the oil, the liquid collection system will not be used.

Pyrolysis. The pyrolysis operation will be based on the study conducted by Shen et. al

(2018), however the liquid collection system will not be followed. First, the sample is placed

inside the oven. Then it is pumped with N2 at 0.5L/min at the pressure of 1.5bar to purge the air

inside the oven. This creates an inert atmosphere. After that, the oven is slowly heated at a rate of
 15

50C/min until it reaches 500C. Finally, it is left for another 1hr and 10min to ensure that the

reaction is complete. As mentioned in the limitations, only NaBr formation will be considered

during the pyrolysis of NMF-WPCBs. The char and gas will be collected for the analysis. Char

will be analyzed for NaBr formation while the gas will be analyzed for HBr formation. The total

Br found will be the total amount of Br in the sample while the Br found in the char will be the

amount fixed into the char. These values will be used to determine the %efficiency of the

experimental set-ups.

3.5. Analysis

The composition of the char will be identified by XRF/XRD Analysis and the amount of

bromine will be determined by thermo-gravimetric method. On the other hand, the bromine gas

will be determined by gas chromatography.

Thermo-gravimetry. The pyrolyzed char will be place in a beaker and will be mixed with

200mL of distilled water. The solution will be stirred using a magnetic stirrer at room temperature

for 3mins to ensure that all of the NaBr salt is dissolved in the water. After that, the mixture will

be decanted and filtered using a simple filtration set-up. The filtrate will be collected for

evaporation to leave the salt behind. The residue after evaporation is the NaBr.

Gas chromatography. The collected gas will be placed in a gas chromatograph that is

already calibrated to determine the amount of HBr gas.

𝑚𝑎𝑠𝑠 𝑜𝑓 𝐵𝑟 𝑖𝑛 𝑐ℎ𝑎𝑟
% 𝑒𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦 = 𝑥 100
𝑚𝑎𝑠𝑠 𝐵𝑟 𝑖𝑛 𝑓𝑒𝑒𝑑

The mass of Br in both cases will be computed using stoichiometry.

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4. EXPECTED RESULTS

It is assumed that temperature, weight loading, and soaking time will affect the bromine

fixation efficiency therefore 3 levels for each parameter was set and analyzed. In order to determine

the effect of each parameter, set-ups and combinations were generated using Design Expert that

will hold two parameters constant. The following are expected to behave for each given parameter:

increasing the temperature of the reaction will give energy to drive the reaction forward, increasing

the weight loading of NaOH at constant NMF-WPCB load will increase the amount of NaOH that

will react with HBr; and increasing the soaking time will also allow the time for reaction to go into

completion.

The conversion of Br can be represented by reaction:

HBr + NaOH → NaBr + H2O

HBr, as an aqueous solution, is an acid and when it reacts with NaOH, a basic solution,

will form a neutral solution composed of water and NaBr salt. The reaction is spontaneous.

However given all those assumptions, there are still factors that must be considered: the

optimal time may not be the longest time used in the experiment; there is just a limit on the

maximum conversion that could occur in a reaction; the optimal temperature may not be the

highest temperature used in the experiment. All these factors affect the economics of the large-

scaling of the process, however the discussion for large-scaling is not covered in the study. This

study can only provide the lab-scale parametric conditions for the highest bromine fixation

efficiency which can be referenced for bench marking.

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5. SUMMARY AND CONCLUSIONS

The prevalent use and disposal of electrical and electronic gadgets brings about the increase

of electrical wastes or e-wastes. These e-wastes contain printed circuit boards (PCBs) that is both

valuable and toxic. Collectively, these wastes can become a highly valuable raw material resource

or a highly hazardous, toxic health and environmental pollutant. The current trend for handling

these wastes, especially in the Philippines, is through landfilling. Recycling in junkshops are also

done to recover precious metals however these practices often do not follow the proper handling

procedures which leads back to hazards and pollution. Recovery methods have been researched in

order to tap into its potential raw material source.

Pyrolysis was deemed to be one of the most effective recovery methods for both metal and

non-metal resource. This is because pyrolysis can produce by-products that can be used for fillers,

fuel source and phenol oils which is different from the traditional precious metals of copper, gold

and other metals. However, the disadvantage of this method is the production of HBr gases which

is toxic and an environmental pollutant. The bromine comes from the fire-retardant tetrabromo-

bisphenol A incorporated in the laminate resin. The pyrolysis process degrades the organic

compound (non-metallic) which bounds this substance, eliminating it as HBr gas. It is important

address this reaction in order to develop an effective large-scale waste printed circuit board

processing plant that will handle such wastes and at the same time recover economical raw

material. This will also encourage electrical and electronic manufacturing plants to gain interest

and responsibility for the end-of-life EEEs.

This study can help in determining the important parameters that affect bromine fixation

into char using NaOH soaking pre-treatment; therefore, making pyrolysis an effective, sustainable,
 18

and environmentally-friendly waste handling method for treating waste PCBs. The circuit boards

were size reduced to a diameter of about 150m and passed through mesh 100. The undersize

contains approximately 100% NMF and it was used for the experiment. The parameters explored

for the NaOH pre-treatment are temperature, %w/w loading, and soaking time. A fabricated

pyrolysis equipment was made due to lack of equipment. The pyrolyzed NMF-WPCBs was

analyzed by XRF/XRD to determine the char’s composition, thermo-gravimetry to determine the

amount of fixed Br, and lastly, gas chromatography to determine the unreacted HBr gases. It is

expected that increasing temperature, %w/w loading and soaking time will increase the %fixation

efficiency of bromine in char. In conclusion, the parameters are directly proportional to the

bromine fixation efficiency.

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