ISSN 1811-2382, Polymer Science, Ser. C, 2007, Vol. 49, No. 1, pp. 6–12. © Pleiades Publishing, Ltd., 2007.

Original Russian Text © G.V. Rybachuk, I.I. Kozlova, V.B. Mozzhukhin, V.V. Guzeev, 2006, published in Klei. Germetiki. Tekhnologii, 2006, No. 1, pp. 30–31; No. 2, pp. 2–6.

PVC Plastisols: Preparation, Properties, and Application

G. V. Rybachuk, I. I. Kozlova, V. B. Mozzhukhin, and V. V. Guzeev
Federal State Unitary Enterprise, Kargin Polymer Chemistry and Technology Research Institute,
Dzerzhinsk, Nizhni Novgorod oblast, 606000 Russia
e-mail: [email protected]

Abstract—The engineering issues of plastisol preparation, composition, properties, and application are con-
sidered. Special attention has been paid to the adhesion characteristics of plastisol coatings.
DOI: 10.1134/S181123820701002X

The processing of poly(vinyl chlorides) (PVCs) To appreciably increase the viscosity of plastisols
through plastisols is one of the most efficient proce- and to render them thixotropic (pseudoelastic) [10–14],
dures. Plastisols are multicomponent heterophase sus- gel-forming agents, such as salts of fatty acids and mul-
pensions of solid ingredients (PVC, fillers, thermosta- tivalent metals (soaps) and various fillers with high oil
bilizers, and pigments) in mixtures of liquid functional absorption, are added. The colloidal silicon dioxide
additives (plasticizers, adhesives, diluents, surfactants). (aerosils) or bentonites are among such fillers [10–14].
Plastisols are prepared via component mixing in a On the contrary, fillers with low oil absorption, for
certain sequence [1] and subsequent degassing of the example, chalk and barium sulfate (up to 20 wt %),
resulting paste. have almost no effect on the viscosity of plastisols [3].
The viscosity of plastisols is frequently decreased with
In the plastisol preparation, paste-forming homo- the use of special suspension PVC extenders as fillers
and copolymers of vinyl chloride with molecular [10, 15–17].
masses from 55000 to 100000 (Fickenscher’s constants
Fillers are incorporated into almost all plastisol for-
are 65–100) are employed. These homo- and copoly-
mulations because, along with modification of proper-
mers are produced by emulsion and microsuspension
ties, they also reduce the cost of the articles.
processes.
The thermal stabilization of plastisols is achieved
The size, structure, and distribution of paste-form- with the same stabilizers as in the case of other PVC-
ing PVC particles, the nature and amount of emulsifiers based materials. Preference is given to liquid stabilizers
and other additives used in the PVC synthesis, and the that, in contrast to powderlike ones, do not raise the vis-
tendency of particles toward agglomeration are factors cosity of plastisols [18].
governing the rheological and processing features of
Pigments, fire retardants, antistatic agents, and other
plastisols [2–6].
additives used for preparation of various PVC-based
The composition of plastisols includes 40–150 phr compositions are also employed in the manufacture of
of primary and secondary plasticizers that are usually plastisols.
used in PVC-based formulations. The plasticizers are Sometimes, substances affecting the processing
esters of o-phthalic, adipic, sebacic, trimellitic, and, behavior of materials are introduced into plastisol for-
rarely, of o-phosphoric acids, polyester compounds, mulations. For example, the addition of a powderlike
and liquid chlorinated paraffins [7–9]. polyethylene (15%) decreases the percolation of a plas-
Diluents or thickeners are used to control the viscos- tisol through a stockinet, whereas calcium or magne-
ity of plastisols. Viscosity is reduced most efficiently sium oxide absorbs moisture [19–21], which worsens
when volatile diluents or polar organic liquids are used. the properties of plastisols and the related products.
In the former compounds, polymers do not swell even Organosilicon liquids reduce the surface tension of
under heating, whereas the latter compounds are capa- plastisols and thus facilitate a more rapid removal of air
ble of polymer solvation. For this purpose, paraffin, ter- bubbles [2, 22]. In order to render plastisols adhesive to
pene, and aromatic hydrocarbons, alcohols, and different materials, unsaturated, epoxy, and nitrogen-
ketones [2, 3] are used and their concentrations may be containing compounds, phenolic resins, and other addi-
as high as 10 wt %. Plastisols with a higher content of tives may be used [23].
volatile diluents are referred to as organosols. Their The character of flow of plastisols may be varied in
preparation and processing into articles are character- a wide range as dependent on the composition, prepa-
ized by certain specific features that are beyond the ration conditions, and shear rate in the course of their
scope of this paper. processing. Hence, the rheological properties of plasti-

6
 PVC PLASTISOLS: PREPARATION, PROPERTIES, AND APPLICATION 7

sols cannot be strictly characterized by viscosity at one size, come into contact with each other, and interfuse to
shear rate (the effective viscosity). Nevertheless, for form a homogeneous body [2, 3].
practical purposes, plastisols may be conditionally As is seen from the foregoing, there are many meth-
classified as low-viscosity (10–50 P), middle-viscosity ods useful for processing of plastisols into articles and
(50–150 P), and high-viscosity (150–10000 P). In this coatings. All of these methods requires that the adhe-
case, viscosity measurements are performed at a low sion phenomena occurring at the plastisol–substrate
shear rate, for instance, at 1 s–1 [3]. interface be taken into consideration. For example, in
Plastisols are processed into final products by dip- the case of cast or rotational molding, the final article
ping, cast molding, rotational molding, extrusion, must be easily taken out of a mold; hence, the adhesive
spraying, spreading, and screen printing. strength of the plastisol–substrate system should be
The dipping technique is employed for the process- minimal. On the contrary, in the sealing of weld seams,
ing of low- or middle-viscosity plastisols that begin to coating of body bottom plates of cars, and manufacture
flow at rather high shear stresses and possess a high pot of metal-based laminates, a high adhesive strength of
life. This technique is used for manufacture of gloves the plastisol coating is required.
(including gloves on the fabric base) [24], pipets, Numerous inventions deal with methods of increas-
bushes, and other articles, deposition of anticorrosive ing the adhesive strength of plastisol coatings. How-
coatings on spare parts of machines and instruments, ever, much less publications are available on the mech-
and application of protective coatings on glass aerosol anism of plastisol coating adhesion. Therefore, interest
flasks. in plastisols capable of adhesion remains rather high.
Cast molding is used in the case of low- or middle Studies in the field of plastisols with high adhesion
viscosity plastisols. These plastisols demonstrate the have long been performed at the Kargin Polymer
pseudoplastic character of flow or character of their Chemistry and Technology Research Institute. As a
flow is nearly the Newtonian one. The method is imple- result, means of controlling the adhesive properties of
mented in two variants: casting into open molds and plastisols through changes in the composition of plasti-
casting with pouring out (the inverse dipping). The sols and in the character of interaction between their
former variant allows one to fabricate monolithic arti- ingredients have been elaborated.
cles, while the latter variant makes it possible to pro- The adhesive strength of the plastisol coating, which
duce various capacities, boots, and other hollow goods. is characterized by the peel work of a film (Ap) depends
Hollow articles are also manufactured by the rotational
molding [3]. on three constituents [27]:
The extrusion technique is mostly applied for fabri- Ap = AA + AD – AS,
cation of wire covering and elastic profiles. In the
course of slow extrusion at a shear rate of 10–100 s–1, where AA is the equilibrium work performed against the
plastisols with a viscosity of 150–180 P may be action of intermolecular forces at the interface; AD is the
processed, while extrusion at a shear rate of work spent for deformation of the film during its peel-
1000−10000 s–1 is employed for processing of plasti- ing; and AS is the work of residual stresses.
sols with viscosities ranging from 200 to 250 P [3].
For plastisol-based adhesion coatings, a part of
The spraying processing is employed when the vis- work spent for deformation of coatings is the most sub-
cosities of plastisols are reduced from 10000 to 110 P stantial [27–32]. In some cases, the proportion of AA or
with an increase in the shear rate from 0.1 to 150 s–1. inherent adhesion may be also rather high and equal up
For example, anticorrosive and antinoise coatings are to 60% of the total adhesion strength of plastisol coat-
deposited on body bottom plates of cars via this method ings [17, 33–36, 38].
[3, 25, 26].
Spreading is most widely used in the manufacture of Thus, the adhesion strength of plastisol coatings and
artificial leathers. This method consists in the smearing adhesives may be controlled by changing deformation
of a plastisol on a moving fabric by means of a roller or and adhesive constituents.
a knife. The screen printing technique is used for pro- On the basis of an analysis of patent publications,
cessing of low- and middle-viscosity plastisols. adhesives for plastisols may be divided into four main
Any method of plastisol deposition needs heat treat- groups, namely: unsaturated compounds, nitrogen-con-
ment as the final stage. In the course of heat treatment, taining additives, phenolic resins, and epoxy resins [23].
gelation and fusion of PVC particles proceed. As a Among unsaturated compounds, oligo(ester acry-
result, plastisols turn into a rather strong material lates) (OEAs) are widely applied as adhesives.
whose characteristics are primarily determined by their Earlier [28–33], we have studied plastisols contain-
composition. ing oligo(ester acrylates) TGM-3 (triethylene glycol
In brief, the mechanism of heat treatment may be α,ω-dimethacrylate) and 7-1 (α,ω-bis(trimethacryl
outlined as follows: with a rise in temperature, a plasti- pentaerythrite) adipinate) crosslinked with cumyl
cizer penetrates into PVC particles that, in turn, grow in hydroperoxide (CHP) as adhesive systems.

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8 RYBACHUK et al.

Ap × 10–2, J/m2 115

86 115
5 100 Chalk, phr

6 115
87
4
70 Chalk, phr
117°
96
40 Chalk, phr

4 97°
122 20 Chalk, phr
2'
1'
6 122

2
3' 2 103°
1 5 Chalk, phr

3 Without chalk

108°
0 20 40 60 80 100 120
Content of filler, phr Fig. 2. DTA curves for plastisols containing 20 phr of
OEA 7-1 and different amounts of chalk.
Fig. 1. Effect of fillers on the peel work (Ap) of plas-
tisol coatings from aluminum: (1, 4) chalk,
(2, 5) kaolin, and (3, 6) aerosil. (1–3) without OEA 7-1
and (4–6) in the presence of 20 phr of OEA 7-1, concentrated on the chalk surface, whereon their local
respectively; (1'–3') are theoretical curves (given the concentrations become higher compared to that in the
effects of the filler and OEA 7-1 on Ap are additive). bulk. As evidenced by the IR data, filling is accompa-
nied by the formation of H complexes between OH
groups of the filler surface, carbonyl groups of the oli-
When chalk, kaolin, or aerosil is added into such gomer, and hydroperoxide groups of CHP.
plastisols, the synergistic effect of fillers and polymer-
izing oligomers on the peel work of polymer coatings is Thus, oligomer cure occurs on the filler surface. As
observed (Fig. 1). a result, the polymer–oligomer boundary layer forms
around the filler particles and the rigidity of this layer is
In our opinion, this phenomenon may be explained higher than that of the matrix. It is of significance that
in the following way. the introduction of OEA into plastisols allows one to
The differential thermal analysis (DTA), IR spec- artificially create a polymer–oligomer jacket on parti-
troscopy measurements, and studies of the heat effects cles of even such inactive filler as chalk. In the absence
of wetting of fillers with liquid components have shown of reactive additives, no such a jacket was formed.
that, regardless of the PVC and OEA compatibility, the An increase in the rigidity of the polymer–oligomer
selective adsorption of a part of an oligomer and hydro- boundary layer around filler particles results in a rise in
peroxide on the surface of mineral fillers proceeds in the rigidity of the whole plastisol system. As a conse-
the course of filling. quence, the deformation constituent and, hence, the
Figure 2 depicts the DTA curves of plastisols con- total adhesion strength of the plastisol coating grow.
taining OEA 7-1 and different amounts of chalk as an
example. A somewhat different situation was observed when
the fillers were introduced into plastisols based on
As is seen, the addition of chalk initially leads to nitrogen-containing adhesives [17, 34–36].
splitting of the DTA peak corresponding to the poly-
merization of OEA. Upon a further increase in the As such adhesives in PVC-based plastisols,
degree of filling, the peak completely shifts toward poly(ethylenimines), modified poly(amino amides),
lower temperatures. Probably, in the course of plastisol polyalkylene polyamines, and other compounds were
filling, greater amounts of the oligomer and CHP are employed.

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 PVC PLASTISOLS: PREPARATION, PROPERTIES, AND APPLICATION 9

Figure 3 (curve Ap) shows the typical curve demon- A, J/m2

strating the effect of nitrogen-containing additives 1000
(NCAs) (in our case, polyethylene polyamines) on the
900
work of peeling of the plastisol coating. As is seen, the Ap
adhesion strength grows not proportionally to the adhe- 800
sive concentration but only to a concentration of 5–8 700
phr. Upon a further increase in the adhesive concentra- 600
tion, the adhesion strength remains almost invariable. 500
The above results may be explained with due regard 400
for the calorimetry data. It turned out that the heats of As
wetting of an aluminum powder and of the hardened 300
EF-083 primer powder that model the substrate surface 200
with nitrogen-containing additives are higher by a fac- 100
tor of 6–70 than the heat of their wetting with dioctyl
phthalate (DOP). This fact indicates that nitrogen-con- 0 2 4 6 8 10 12 14 16 18
taining additives are characterized by a much higher Content of PE-PA, phr
affinity to the studied substrates than DOP and provides
explanation for their preferential adsorption on the sub- Fig. 3. Peel work (Ap) and quasi-equilibrium peel
strate surface. work (As) of coatings vs. the PE-PA content in the
plastisol.
Hence, because of thermodynamic reasons, the sub-
strate surface will be enriched with NCA molecules (in
this case, PE-PA) responsible for the formation of adhe- Ap × 10–2, J/m2
sive bonds. Probably, the substrate surface becomes
saturated with the adhesive even at a concentration of 7
5–8 phr. Therefore, a further increase in the content of 4
PE-PA in the plastisol slightly affects a change in the
quasi-equilibrium peel work As (Fig. 3) that character- 6
izes adhesion [37] and a gain in the total peel work. 3 2
It is noteworthy that, upon the introduction of PE- 5
PA in plastisols, the rigidity of the coating and, conse-
quently, the deformation constituent of adhesion work 1
remain unchanged. This is the reason why the curves 4
obtained for the adhesion constituent and for the total
peel work of plastisol coatings follow similar patterns.
Previous experiments showed that, when fillers 3
0 2 4 6 8 10 12 14 16 18
were introduced into plastisols based on oligo(ester
acrylates), these compounds showed the synergistic Content of filler, phr
effect on the adhesive strength of the filled plastisols
Fig. 4. Effect of fillers on the peel work (Ap) of plas-
owing to the growth of the deformation constituent. A
tisol coatings containing PE-PA: (1) white carbon
similar effect could be expected for plastisol filling with black BS-30, (2) white carbon black BS-100,
NCAs. (3) aerosil A-175, and (4) aerosil A-300.
However, in the case of nitrogen-containing addi-
tives, a more complicated situation was observed.
Figure 4 demonstrates the effects of nonmodified quence, the adhesion constituent of work decreases and
aerosils and white carbon blacks of different brands on the peel work of the coating diminishes at low degrees
the peel work of plastisol coatings. As is seen, these of filling.
curves show minima. This tendency may be explained On the other hand, as a result of selective adsorption
as follows. of PE-PA by the filler surface, the coating gains in rigid-
According to calorimetric measurements [36], the ity, the deformation constituent increases, and eventu-
heats of wetting of the aerosol and white carbon black ally, the total peel work grows.
substantially surpass the heat of wetting of these fillers It should be emphasized that the redistribution of the
by the plasticizer. Therefore, because of thermody- adhesive in the coating appears to be appreciably
namic reasons, the surface of filler particles should be dependent on the surface area of the filler. As is seen
enriched with adhesive molecules. from Fig. 4, the higher the dispersity of filler particles,
Such a selective adsorption of PE-PA by filler parti- the more pronounced the minimum in the peeling
cles brings about redistribution of the adhesive between curves. At the same time, the minimum shifts to lower
surfaces of the filler and the substrate. As a conse- filler concentrations. However, after passing the mini-

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10 RYBACHUK et al.

Ap, J/m2 With an increase in the content of anilinophenol-

600 1 formaldehyde oligomers (PFOs) of SF-340A, SF-
341A, and SF-342A brands, the peel work (Ap) of plas-
500 tisol coatings changes in a similar manner: the value of
2
400 Ap grows not proportionally to the adhesive content but
passes through a maximum when the content of adhe-
300 3 sive falls in the range 10–20 phr (Fig. 5). However, the
200 maximum values for these three resins are different: the
plastisol coating based on the SF-342A additive has the
100
highest adhesive strength (Fig. 5, curve 1).
0 5 10 15 20 25 30 The behavior of the quasi-equilibrium peel work
Content of PFO, phr
(As) in the studied concentration range does not depend
on the PFO brand: for all three resins, As grows until a
Fig. 5. Total peel work (Ap) of plastisol coatings as concentration of ~8 phr is achieved and then remains
a function of PFO concentration: (1) SF-342A, virtually constant. PFOs contain adhesion-active phe-
(2) SF-341A, and (3) SF-340A. noxyl hydroxyl and methylol groups capable of chemi-
cal bonding to the surface of an aluminum foil. Owing
to interaction between hydroxyls that remained intact
A5%, J/m2 after PFO curing and hydroxyl groups of the surface
500 oxide film, hydrogen bonds are formed. With an
1 increase in the amount of these bonds, the adhesion
400 characterized by the quasi-equilibrium peel work is
2 enhanced.
300
3 At the optimal PFO concentration (~15 phr), the
200 part of the quasi-equilibrium peel work is no more than
30% of Ap. The rest part of the adhesion work (different
100 for three oligomers) is associated with the contribution
0 10 20 30 due to the deformation work constituent since the cure
Content of PFO, phr of PFO may facilitate an increase in the rigidity of com-
positions. It was found that plots obtained for the rigid-
Fig. 6. The rigidity of polymer films (A5%) as a function ity of plastisol films (estimated as work A5% required
of PFO concentration: (1) SF-342A, (2) SF-341A, and
(3) SF-340A. for the 5% extension of the films) versus the content of
PFO (Fig. 6) are similar to the corresponding plots
obtained for Ap (Fig. 5).
mum, the greater the dispersity of filler particles, the Note that the plastisol coating based on the SF-342A
more pronounced the increase in the adhesive strength, oligomer exhibits the highest rigidity and the largest
Since the adhesive strength depends on the distribu- adhesive strength.
tion of adhesives between substrate and filler surfaces, It is suggested that the introduction of PFO into the
it was of interest to study compositions filled with mod- plastisol has an effect similar to that of fillers and assists
ified aerosils having different degrees of lyophilicity of the transition of a certain part of the polymer to the
the surface with respect to nitrogen-containing addi- boundary layer. The adsorption interaction of the sur-
tives. face of PFO particles with PVC causes a reduction in
It turned out that, regardless of the nature of adhe- the molecular mobility of PVC chains in the boundary
sive and modifiers, on the surface of aerosil, the work layer and leads to a decrease in the relaxation rate of the
of coating peeling from all studied substrates increases whole system.
to 20 × 10–3 J/kg with an increase in the heats of aerosol Thus, the relationship between of the peel work of
wetting by adhesives. Upon a further rise in the heat of coatings and the content of aniline-phenolformalde-
wetting, the peel work changes insignificantly. It hyde resins in the plastisol composition follows the
appears that the heats of interaction of the filler with extremum pattern. Here, the growth of the adhesive
nitrogen-containing additives larger than 20 × 10–3 J/kg strength, when the content of PFO is no more than 8–
provide the optimal distribution of the adhesive 10 phr, is associated with a simultaneous increase in
between the surface of aerosil and the area of adhesive both molecular and deformation constituents. With a
contact. This circumstance ensures the maximum pos- further increase in the content of PFO in the composi-
sible adhesive strength for the given system. tion, the molecular constituent remains invariable,
The interaction of ingredients also plays the key role whereas the behavior of the deformation constituent is
in the adhesive properties of plastisols with phenol- similar to that of the total adhesive strength of the plas-
formaldehyde adhesive additives [38–40]. tisol coating.

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 PVC PLASTISOLS: PREPARATION, PROPERTIES, AND APPLICATION 11

6 compositions, as is evident from the negative values of

∆H (Fig. 7).
∆H, J/g Ap, J/m2
4
2 The finding that the adhesive strength of plastisol
0
coatings and the heat of interaction of the plasticized
PVC and PFO (Fig. 7) change in the extremum pattern
–2 with the PFO content (with the maximum adhesive
–4 strength and the minimum interaction heat at the same
–6 content of the oligomer) provides additional evidence
0 0.05 0.10 0.15 that interaction between the components significantly
Weight fraction of SF-342A affects the adhesive strength of plastisol coatings.
Thus, the study of a large amount of adhesives of
Fig. 7. The peel work (Ap) of plastisol coatings and
different nature showed that the adhesive properties of
the enthalpy of interaction (∆H) of plasticized PVC
with SF-342A as a function of the weight fraction of the plastisol coatings may be efficiently controlled
SF-342A. The fusion schedule: 200°C for 7 min. through their targeted distribution in the plasticized
PVC matrix with due regard for the interfacial interac-
tion of ingredients.
The study of the heat of interaction of the plasticized Our studies led to the development of plastisols with
PVC with SF-342A as a function of the content of PFO desired adhesive properties. Striking examples of such
in the sample showed that, at the temperature of plasti- products are plastisols of D-25A and D-26A brands that
sol fusion, there is a strong energy interaction between are currently in much demand [41]. These plastisols
these components within the whole range of the test were designed for bonding of filtration paper sheets to
zinc-plated metal caps in the manufacture of air, oil,
and fuel filters of cars. However, they are successfully
Characteristics of plastisols and related samples prepared
under heat treatment employed for deposition of protective coatings on
metal surfaces and sealing of gaps between parts of
D-25A D-26A agricultural machines. The plastisols are produced by
Characteristic the Kargin Polymer Chemistry and Technology
plastisol plastisol
Research Institute pilot plant according to TU (techni-
Appearance Homogenous mass. cal specifications) 2241-402-00208947-2003; a sani-
Clots and delamina- tary-epidemiological certificate for these products is
tion are not admitted available. The formulations of the plastisols in point are
Brookfield apparent viscosity 6±3 35 ± 15 covered by patents [42–44].
at (25 ± 0.2)°C, Pa s
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