Filled butadiene-styrene rubber manufacturing process

FIELD: rubber industry.

SUBSTANCE: invention relates to production of butadiene-styrene rubbers obtained via emulsion (co)polymerization, in particular to methods for isolation thereof out of latexes. A process for manufacturing filled butadiene-styrene rubber is described comprising butadiene-styrene copolymerization in emulsion in presence of radical initiators, stopping the process, adding oil filler and antioxidant, and degassing and isolating rubber out of latexes utilizing coagulation technique. Process is characterized by that, as filler and antioxidant, fiber-oil-antioxidant composite is used, obtained by preliminarily mixing milled garneted fibers with hydrocarbon solution of a low-molecular weight polymer material. The latter is prepared on the basis of still residue of styrene rectification in production of styrene from ethylbenzene, wherein styrene contains amine- or phenol-type antioxidant. Thus obtained composite is grinded and dispersed in surfactant-containing aqueous phase, after which low-boiling hydrocarbon fraction is distilled off and low-molecular weight polymer material and fibrous filler are added in amounts, respectively, 2-6 and 0.1-1.0% based on the weight of rubber.

EFFECT: reduced loss of rubber and environmental pollution at higher physicochemical characteristics of vulcanizates.

2 tbl, 11 ex

 

The invention relates to the production of butadiene-styrene rubbers, the emulsion (co)polymerization, in particular to methods of filling them on stage latexes, and can be used in the petrochemical industry.

The closest in technical essence is a method of obtaining a filled styrene-butadiene rubbers on stage latex using as fillers naphthenic, paraffinic oils, followed by separation of the filled rubber water-salt solution and acidifying agent [Kirpichnikov P.A., Averko-A. L.A., Averko-Antonovich CREATING Chemistry and technology of synthetic rubber: a Textbook for high schools. - 3rd ed., Rev. - L.: Chemistry, 1987. - 424 S., ill.].

The main disadvantages of this method of receipt of filled styrene-butadiene rubber are:

- formation of fine crumb rubber, which is blown away with the serum and leaching waters from plants selection, which reduces the performance of the process;

- violation of the stability of the process;

- environmental pollution rubber products;

- low resistance thermal-oxidative effects.

The problem to which this invention is directed, is to stabilize the process of separating rubber from latex, less waste rubber obrazovash is the action scene crumbs from the shops of the selection reduction of environmental pollution, rubber products, improvement of physico-mechanical properties of vulcanizates.

This object is achieved in that in a method of producing a filled styrene butadiene rubber by copolymerization of butadiene with styrene in emulsion in the presence of radical initiators, stoppelman process, the introduction of a filler and an antioxidant, decontamination and separation of rubber from the latex by coagulation method, what is new is that as filler and antioxidant use voloknistotsementnye composite, preliminary mixing crushed spongy fibers, with a hydrocarbon solution of a low molecular weight polymeric material derived from the cubic residue of the distillation of styrene from a styrene production from ethylbenzene containing antioxidant amine or phenolic type, milling the obtained composite by dispersing it in the aqueous phase containing surfactants, distillation of low-boiling hydrocarbon fraction and the introduction in the amount of 2-6% low molecular weight polymeric material and 0.1 to 1.0% of the fibrous filler in the rubber.

The proposed method of producing a filled styrene butadiene rubber stabilizes the process of coagulation, reduce the loss of rubber, SN is to diminish environmental pollution and improve the physico-mechanical properties of vulcanizates.

The method is as follows.

The copolymerization of butadiene with styrene is carried out in a battery consisting of 10-12 polymerization apparatus, in the presence of radical initiators type (for example, cumene Pinna). After reaching a conversion of 65-70% is entered in the system stopper radical process (sodium nitrite, rongalit and others) and the resulting latex is fed to the degassing, where the distillation nesupykit.vasara monomers (styrene, butadiene and other low-boiling products. From the Department of degassing latex comes coagulation, where it is mixed with melaniestarmelanie emulsion and agents, providing a selection of rubber latex (an aqueous solution of sodium chloride and sulfuric acid). The resulting crumb rubber is fed to the washing, dehydration, drying and packaging (Raspopov IV, Nikulin S., Garshin A.P. and other Improvements equipment and technologies for extraction of butadiene-(α-methyl)styrene rubber from latex. M: NIITA-Neftekhim, 1997. 68 C.). This process corresponds to the restrictive part of the claims.

Low molecular weight polymeric material (NPM) was obtained by copolymerization of unsaturated compounds contained in the VAT residue of the distillation of styrene with maleic anhydride. This process was implemented on an industrial scale, and the obtained N The M used in the manufacture of paints called "Lacquer KORS" (Nikulin S., Butenko TR, Rylkov A.A., Fazlioglu RG, purer S.M. Perspective of application bottoms production vinylaromatic monomers. M: Tsniiteneftehim. 1996. 64 C.). Properties NPM obtained on the basis of VAT residue of styrene: color by iodometric scale (IMS) - 200-400; mass fraction of residual styrene - not more than 0.5%; viscosity VZ-4 - 25-50; molecular weight of 1600-2300.

Fibrous materials that are wastes of various industries (scraps of fabrics, yarns, potency and others), podvergaut razvlecheniy and grinding to the size of 2-10 mm and mixed with a hydrocarbon solution of a low molecular weight polymer material (NPM), obtained on the basis of VAT residue formed during the production of styrene from ethylbenzene containing amine or phenolic antioxidants. The resulting composite is mixed in a high speed mixer for 10-15 minutes at 60-90°and subjected to further milling for 1-3 hours. The result of these operations is rubbing NPM fibrous material and dehydration. The resulting composite at a constant high speed stirring is dispersed in an aqueous phase containing a surfactant, at 40-60°C for 1-3 hours. The dosage of fibrous filler can withstand 0,1-1,0% rubber, NPM - from 2% to 6% on the rubber. Note the imposition of higher dosages of fibrous filler (more than 1.0% rubber) leads to a sharp increase in the viscosity of the system, that affects her mobility and transportability through pipelines. After distillation of low-boiling hydrocarbon fraction (solvent, nezapominayuschiesya monomers and other low-boiling products) odnopolyarizatsionnogo variance (WPAD) is mixed with the latex rubber SKS-30 ark. Rubber latex containing VITAL, served on coagulation.

The butadiene-styrene latex rubber SKS-30 ark containing VITAL, pour in the capacity for coagulation, equipped with a stirrer and placed in a thermostat to maintain desired temperature. Maintained at a predetermined temperature for 10-15 minutes, enter the coagulating agent is a 24% aqueous solution of sodium chloride and stirred for 5-10 minutes. The allocation process complete input 1-2% aqueous solution of sulfuric acid. the pH of coagulation withstand 2.0 to 2.5. The resulting coagulum separated from the serum, washed with water and dried at a temperature of 80-85°C. Completeness coagulation assessed visually (serum transparent - coagulation full), and the weight of the resulting coagulum.

The method is illustrated by the following examples.

The copolymerization of butadiene with styrene is carried out on a continuous circuit on the battery, consisting of 12 polymerization. In the first as the process polymerizaton served water and hydrocarbon phase (a mixture of 70% butadiene and 30% styrene), the radical is first initiator (of cumene hydroperoxides, Pinna and others) and the molecular weight regulator (tertiary dodecylmercaptan). An additional amount of molecular weight regulator is introduced into the process before the fifth and ninth polymerization. Polymerizaton equipped with agitators. The copolymerization of butadiene with styrene is carried out at 4-8°C. the Process is carried out until the conversion of 65-68%. When you exit the last polymerizate latex continuously dressed stopper - dimethyldithiocarbamate solution of sodium with a sodium nitrite. Seasoned stopper latex passes through the filter and is directed to the Stripping nesupykit.vasara monomers in the upper part of the column prior degassing, where the distillation of the main quantity of butadiene. After the column degassing of the latex is directed into the vacuum distant apparatus, where the distillation of styrene and the remainder butadiene. The latex from the Department of degassing is served on coagulation.

In capacity, equipped with a mixing device, enter 60 g NPM, 40 g of solvent (toluene) and antioxidants amine or phenolic type in quantities that meet the requirements of technical specifications for manufactured brand of rubber. The mixture with constant stirring is heated to a temperature of 60-90°and introducing the fibrous filler (cotton, rayon, nylon), subjected to razvlecheniy and grinding. Mix poluchenno the mixture for 10-15 minutes. Pereir the obtained composite is carried out in a ball mill for 1-3 hours. After milling the resulting composite is mixed with a water solution containing a surfactant - rosin soap, soap-based fatty acids, tall oil in quantities of 6% and lakanal of 0.5% on the dispersible phase and homogenize for 1-3 hours at 40-60°With the equipment, equipped with high-speed mixing device. Simultaneously carry out the distillation under vacuum volatile hydrocarbon fraction (solvent, unreacted monomers and other) from the obtained dispersion. The dry residue is in the range of 30-40 wt.%.

The resulting dispersion is fed to the mixing with the latex of styrene-butadiene rubber SKS-30 ark in the capacity for coagulation, equipped with a mixing device and placed to maintain a predetermined temperature in thermostat. Maintained at a predetermined temperature for 10-15 minutes and at a constant stirring impose a 24% aqueous solution of sodium chloride. To complete the process of coagulation enter acidifying agent, in the form of a 1-2% aqueous solution of sulfuric acid. The consumption of sulfuric acid - 15,0 kg/ton of rubber. the pH of coagulation 2-2,5. After coagulation of the resulting coagulum separated from the serum, washed with water and dried at a temperature of 80-85°C. Completeness coagulation assessed visually (ser the m transparent - coagulation full), and the weight of the resulting coagulum.

Table 1 gives examples of the influence of temperature, dosage NPM and fibrous material (%) rubber) on the process of separation of rubber from latex.

The experimental data presented in table 1 show that the introduction of more VITAL in latex before feeding it to the coagulation allows you to increase the weight (yield, %) resulting coagulum that may be associated with the introduction of NPM and fibrous material, and by reducing losses resulting fine crumbs out from the stage separation and washing with serum and leaching waters.

Selected after coagulation crumb rubber SKS-30 ark, filled with NPM and fibrous fillers, were subjected to drying in a drying Cabinet at a temperature of 80-85°C. further, based on filled rubber SKS-30 ark was prepared rubber mixture according to standard recipes and vulcanizates based on it.

Table 2 shows the performance of rubbers, rubber compounds and vulcanizates standard rubbers on the basis of selected rubber SKS-30 ark.

From the above results show that the additional introduction of the formed coagulum NPM and fibrous material in an amount of 0.1-1.0% for rubber and NPM in the amount of 2-6% on the rubber provides the best efficiency is t, being to achieve a maximum yield of coagulum and improve such properties of the vulcanizates as: resistance to repeated tension, thermal aging and temperature resistance.

Table 1
The influence of the dosage of the fibrous filler and the NPM, the coagulation temperature on the consumption of sodium chloride and output the resulting coagulum
The number of experiments1234567891011
Mass fraction of fiber, % rubber:
Cotton00,050,10,51,01.2--0,50,50,5
Viscose0-----0,5----
Caprona the CSO 0------0,5---
Mass fraction of NPM,%
rubber01246844444
The temperature of coagulation, °6060606060606060408060
Consumption of sodium chloride, kg/ton of rubber175178183185185186181180178179183
The output of the resulting coagulum, %94,796,097,297,598,0of 98.296,896,497,796,497,3
Mass fraction of antio is sidhanta, %: MTC-1501,21,21,21,21,21,21,21,21,21,2-
SU-30A----------1,5

Table 2
Properties of rubbers, rubber compounds and vulcanizates prepared on the basis of rubber SKS-30 ark, filled with NPM fibrous fillers
IndicatorsType of fibrous filler and its dosage, % rubber
control, oil MO-6 without fibercottonviscosenylon
2,04,06,00,10,51,00,10,51,00,10,51,0
Dosage oil NPM, % rubber---2,04,06,02,04,0 6,02,04,06,0
The Mooney viscosity
rubber52,049,046,052,5a 50.548,053,052,0a 50.554,050,049,0
rubber compound57,056,055,058,056,054,058,057,056,059,056,054,0
Plasticity in the Carrera R/cm usled0,350,380,410,360,380,400,360,370,390,350,390,40
Conditional tensile strength, MPa23,821,719,225,226,224,126,325,524,425,924,825,0
Relative untinen is at break, %680690710690695700675680690660655650
Relative residual deformation, %111214111113111210121113
Resistance to repeated tension, testicles60,258,261,373,378,580,480,488,085,6to 78.379,779,4
The ageing factor (100°C, 72 h):
- strength0,510,470,450,700,680,700,680,660,710,670,650,64
- relative elongation0,330,300,31 0,460,450,480,400,410,490,430,410,40

The method of obtaining a filled styrene butadiene rubber by copolymerization of butadiene with styrene in emulsion in the presence of radical initiators, separirovannoe process, the introduction of the oil filler and antioxidant, decontamination and extraction of rubber from the latex by coagulation method, characterized in that the filler and antioxidant use molochnokonsernij composite, preliminary mixing crushed spongy fibers, with a hydrocarbon solution of a low molecular weight polymeric material derived from the cubic residue of the distillation of styrene from a styrene production from ethylbenzene containing antioxidant amine or phenolic type, milling the obtained composite by dispersing it in the aqueous phase containing surfactant by distillation of low-boiling hydrocarbon fraction and the introduction in the amount of 2-6% low molecular weight polymeric material and 0.1 to 1.0% of the fibrous filler in the rubber.



 

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FIELD: rubber industry.

SUBSTANCE: invention relates to production of butadiene-styrene rubbers obtained via emulsion (co)polymerization, in particular to methods for isolation thereof out of latexes. A process for manufacturing filled butadiene-styrene rubber is described comprising butadiene-styrene copolymerization in emulsion in presence of radical initiators, stopping the process, adding oil filler and antioxidant, and degassing and isolating rubber out of latexes utilizing coagulation technique. Process is characterized by that, as filler and antioxidant, fiber-oil-antioxidant composite is used, obtained by preliminarily mixing milled garneted fibers with hydrocarbon solution of a low-molecular weight polymer material. The latter is prepared on the basis of still residue of styrene rectification in joint styrene/propylene oxide production, wherein styrene contains amine- or phenol-type antioxidant. Thus obtained composite is grinded and dispersed in surfactant-containing aqueous phase, after which low-boiling hydrocarbon fraction is distilled off and oil and fibrous filler are added in amounts, respectively, 2-6 and 0.1-1.0% based on the weight of rubber.

EFFECT: reduced loss of rubber and environmental pollution at higher physicochemical characteristics of vulcanizates.

2 tbl, 11 ex

FIELD: rubber industry.

SUBSTANCE: invention relates to production of butadiene-styrene rubbers obtained via emulsion (co)polymerization, in particular to methods for isolation thereof out of latexes. A process for manufacturing filled butadiene-styrene rubber is described comprising butadiene-styrene copolymerization in emulsion in presence of radical initiators, stopping the process, adding filler and antioxidant, and degassing and isolating rubber out of latexes utilizing coagulation technique. Process is characterized by that, as filler and antioxidant, fiber-polymer-antioxidant composite is used, obtained by preliminarily mixing milled garneted fibers with hydrocarbon solution of a low-molecular weight polymer material. The latter is prepared on the basis of (i) still residue of recycled solvent (toluene) purification process in production of polybutadiene rubber and (ii) styrene containing amine- or phenol-type antioxidant. Thus obtained composite is grinded and dispersed in surfactant-containing aqueous phase, after which low-boiling hydrocarbon fraction is distilled off and low-molecular weight polymer material and fibrous filler are added in amounts, respectively, 2-6 and 0.1-1.0% based on the weight of rubber.

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2 tbl, 11 ex

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SUBSTANCE: invention relates to production of butadiene-styrene rubbers via emulsion butadiene-styrene copolymerization process, in particular to isolating rubbers from their latexes in presence of radical initiators. Process is stopped by adding oil filler and antioxidant, after which follows degassing and isolation of rubber from latex by coagulation method. Process is distinguished by that, as filler and antioxidant, fiber/oil/antioxidant composite is used, which is prepared by preliminarily mixing divided unwound fibers with hydrocarbon solution of oil PN-6 containing amine- or phenol-type antioxidant, grinding resulting composite, dispersing it in aqueous phase containing surfactants, and introducing it into rubber in amounts of 2-6% oil and 0.1-1.5% fibrous filler based on the weight of rubber.

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3 tbl, 11 ex

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4 cl, 11 ex, 1 tbl

FIELD: chemical industry; glass industry; methods of production of the sheet double-layer colored Plexiglas for the color filters.

SUBSTANCE: the invention is pertaining to the field of production of the sheet double-layer colored Plexiglas on the basis of the methacrylic esters intended for production of color filters including fluorescing color filters. The invention presents the method of production of the sheet double-layer Plexiglas used for manufacture of the color filters and providing for the preliminary polymerization of the methyl metacrylate (MMA) or the mixture of MMA with 1-5 mass % of methacrylic acid (MCA) admixed with the colorant at presence of the azodinitroisoisobutyric acid. The produced colored prepolymer having the conversion level of 3-5 mass % and viscosity 20-50 cSt is solidified in the plane-parallel mold at presence of 0.03-0.04 mass shares per 100 mass shares of the monomer of the azodinitroisoisobutyric acid, 0.4-2.0 mass shares of the coupling agent, 0.5-2.0 mass shares of the light-absorbing additive - the mixture of the dry-rolled paste on the basis of chlorinated polyvinyl chloride and industrial carbon and 0.01-0.1 mass shares of the antiadhesion agent- sodium dioctylsuccinate. Then the preliminary produced prepolymer MMA colored by the coloring agent, which is distinct from the coloring agent of the first layer and having conversion level of 7-10 mass % and viscosity of 70-110 cSt is cast in the mold on the first layer of the Plexiglas and solidified at presence of the initiator, the coupling agent, the light-absorbing additive and the antiadhesion agent used at production of the first layer. The offered method allows production of the double-layer uniformly colored optically uniform Plexiglas with the homogeneous boundary layers non-upsetting the spectral characteristics of the neutrally-gray color filters.

EFFECT: the invention ensures production of the double-layer uniformly colored optically uniform Plexiglas with the homogeneous boundary layers non-upsetting the spectral characteristics of the neutrally-gray color filters.

4 cl, 11 ex, 1 tbl

FIELD: polymer production.

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EFFECT: increased catalytic activity and enabled preparation of polymer for films at lower partial pressure of ethylene.

15 cl, 5 dwg, 3 tbl, 7 ex

FIELD: polymer production.

SUBSTANCE: invention relates to supported catalytic compositions, methods for preparing such compositions, and polymer preparation processes using these compositions. In particular, invention provides supported catalytic composition including interaction product of: (i) catalyst precursor composition comprising product of reaction of magnesium halide, an ether, electronodonor compound, in particular linear or branched aliphatic C1-C25-alcohol, and transition metal compound, in particular compound of group IV element; (ii) porous inert carrier; and (iii) cocatalytic composition; wherein supported catalytic composition contains less than 1% electronodonor compounds other than those including linear or branched aliphatic or aromatic alcohol having from 1 to 25 carbon atoms and wherein molar ratio of electronodonor compound to magnesium is less than or equal to 1.9. Described are also method of preparing supported catalytic composition, method of preparing polymer comprising reaction of at least one olefin monomer in presence of above-mentioned supported catalytic composition. Described are also supported catalyst precursor composition, supported catalytic composition, method of preparing supported catalytic composition, and method of preparing polymer comprising reaction of at least one olefin monomer in presence of supported catalytic composition, and supported catalyst precursor composition.

EFFECT: increased catalytic activity and enabled preparation of polymer for films at lower partial pressure of ethylene.

15 cl, 5 dwg, 3 tbl, 7 ex

FIELD: rubber industry.

SUBSTANCE: invention relates to production of butadiene-styrene rubbers obtained via emulsion (co)polymerization, in particular to methods for isolation thereof out of latexes. A process for manufacturing filled butadiene-styrene rubber is described comprising butadiene-styrene copolymerization in emulsion in presence of radical initiators, stopping the process, adding oil filler and antioxidant, and degassing and isolating rubber out of latexes utilizing coagulation technique. Process is characterized by that, as filler and antioxidant, fiber-oil-antioxidant composite is used, obtained by preliminarily mixing milled garneted fibers with hydrocarbon solution of a low-molecular weight polymer material. The latter is prepared on the basis of still residue of styrene rectification in joint styrene/propylene oxide production, wherein styrene contains amine- or phenol-type antioxidant. Thus obtained composite is grinded and dispersed in surfactant-containing aqueous phase, after which low-boiling hydrocarbon fraction is distilled off and oil and fibrous filler are added in amounts, respectively, 2-6 and 0.1-1.0% based on the weight of rubber.

EFFECT: reduced loss of rubber and environmental pollution at higher physicochemical characteristics of vulcanizates.

2 tbl, 11 ex

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