Method of extracting butadiene-nitrile rubber from latex

FIELD: chemistry.

SUBSTANCE: method of extracting butadiene-nitrile rubber from latex is carried out by feeding sodium sulphite or sodium bisulphite or sodium pyrosulphite in amount of 0.05-0.8 wt % per latex, into a stream of latex degassed beforehand, into which an antioxidant emulsion is also fed. Further, the stream of latex, containing sulphite, is directed into a coagulation apparatus into which aqueous sulphuric acid and an organic amine coagulant in form of a quaternary polymer ammonium salt are also simultaneously fed, said salt being selected from: polydimethyl diallyl ammonium chloride, a methacrylamide and dimethyl aminoethyl methacrylate hydrochloride copolymer, and polydiethyl aminoethyl methacrylate hydrochloride. The amount of the polymer ammonium salt varies from 0.2-0.5 wt %, per rubber, depending on content of leukanol content in latex in the range of 0.1-0.4 wt %, per rubber, at coagulation pH 3-6 and temperature 30-70°C.

EFFECT: invention improves environmental friendliness of the process, specifically reduces content of unreacted monomer - free acrylic acid nitrile, avoids excess synthetic coagulant and the amount of salt used for coagulation.

3 tbl, 7 ex

 

The invention relates to the selection of synthetic rubber from latex and can be used in the petrochemical and refining industries.

The most common industrial method for the selection of synthetic rubber from latex obtained using Soaps of carboxylic acids as emulsifier and dispersant NF (lakanal), is the allocation of rubbers with sodium chloride and sulfuric acid. Consumption of sodium chloride even recycle serum ranges from 200 to 400 kg per ton of rubber. The entire sodium chloride, as well as bio-undegradable lakanal washed into the waste water, which causes environmental problems (Pasiecznik, Lauwarm-Antonovich, Waaarm-Antonovich. Chemistry and technology of synthetic rubber. Chemistry. Leningrad branch., 1970, s-399, 402-403).

There is a method of selection of synthetic rubber from latex mineral acids in the presence of high-molecular aminecontaining coagulating additives of synthetic or natural origin:

polyalkyleneglycol (US No. 3112299, IPC C08F 6/00, C08F 6/02);

lignite sodium and water soluble polyamine (US No. 4025711, IPC C08F 6/22, publ. 24.05.77);

- polyhexamethyleneguanidine (metacid) (RU # 1700007, IPC C08C 1/15, publ. 23.02.91).

The General lack of data technical solution is to clean the necessity of keeping a low pH (1.5 to 2.5), what causes corrosion of the equipment, high concentrations of sulfate in the wastewater, the leaching of coagulants and antioxidants in the serum.

Some of them, such as lignin sodium, impart a dark color to the rubber, which makes it impossible to use them in obtaining bright rubber stamps.

This coagulant, as metacid is strongly hygroscopic substance that makes its storage and preparation of working solutions.

There is a method of selection of synthetic rubber from latex action of organic coagulant, followed by the separation of the resulting crumb rubber from serum and washing and drying. As organic coagulant used protein hydrolyzed collagen content of 0.07-20 wt.% carboxyl groups (A.S. USSR №1065424 with prior. from 09.09.1982, IPC C08C 1/15, publ. 07.01.1984), and how with the use of mixtures of hydrolyzed collagen or fentolamina resin (condensation product of Nonylphenol and hexamethylenetetramine with diethanolamine) antiglomerular, calcium chloride, magnesium chloride or magnesium chloride (bischofite (RU # 2140928 with prior, from 04.02.98. IPC C08C 1/14, C08C 1/15; C08F 6/22, publ. 10.11.99, IB No. 31), as well as input acetic antiglomerular in various units of the cascade of coagulation and washing of the crumb rubber, with additional input of potassium hydroxide or sodium hydroxide and sodium chloride (RU # 2203287 with prior from 24.06.02,, IPC C08C 1/14, C08C 1/15, publ. 27.04.2003, BI No. 12).

The disadvantages of these methods is the ability of the protein substances of animal origin be subjected during storage and transportation decay emitting volatile sharply smelling decomposition products such as hydrogen sulfide, ammonia, etc. in Addition, the contact personnel with the protein product when it is loaded for the operation of the hydrolysis may cause allergic diseases ("bilkozynu" is a dusty powder product).

The relatively high consumption of protein coagulants due to the fact that proteins of animal and vegetable origin are high molecular weight products. In aqueous solutions, macromolecules, typically, are in the form of balls or twisted spirals-fibrils, and access to nitrogen atoms is difficult. As the coagulation effectiveness is largely determined by the speed of interaction between sulfopropyl lakanal with the amino group of the protein, isolation of amino significantly slows down the process and reduces the effectiveness of the coagulant.

A significant disadvantage of these methods is that an aqueous solution of coagulant has an acidic environment. Introduction latex is a local point of premature coagulation. The introduction of additional antiglomerular, hydroxides of potassium, is the atrium and sodium chloride significantly complicates instrumentation and technology selection process rubbers.

There is a method of coagulating a synthetic rubber latex, butadiene-styrene or butadiene-nitrile, followed by the separation of serum and drying the crumb rubber in the air belt dryer in the acidic environment created a 1%solution of acetic or sulfuric acid, used as a coagulant of a saturated aqueous solution of sodium chloride in an amount of 0.1-60 wt.%, counting on the latex, and polydimethyldiallylammonium in the amount of 0.05-0.5 wt.% (DD No. 142345, IPC C08C 1/14).

This method provides getting loose, well dry crumb rubber. However, it has a significant disadvantage: the project would use significant amounts of salt - sodium chloride.

Also known a method of separation of synthetic rubber latex using a water-soluble copolymer epichlorhydrine with dimethylamine with molecular weight of 200-2000, at a pH of 1.5 to 7.0, at a molar ratio of epichlorohydrin: dimethylamine 1:0.75 to 0,98 (US No. 4001486, IPC C08F 6/22).

This method provides effective coagulation without the use of inorganic salts. However, has one significant disadvantage - as the original products, dimethylamine and epichlorohydrin, and the copolymer - toxic substances, and the copolymer is biologically non-biodegradable product.

The closest technical solution to the proposed method is the separation of the Oia synthetic rubber from latex (butadiene-styrene and butadiene-nitrile), stable Soaps of carboxylic acids, by the action of mineral acid and organic amine coagulant is supplied in two steps: the first portion of the coagulant in the amount of 50 to 90 wt.%, stand under stirring at a temperature of 20-70°C for 0.5 hours, a second portion of the coagulant or its mixture with mineral salt mass ratio of amine coagulant: mineral salt from 1.0:0.0 to 1.0:1500,0 injected into the coagulation apparatus together with recycled serum mass ratio of latex: serum from 1.0:1.0 to 1,0:2,0 (RU # 2253656 C1 IPC SS 1/15, publ. 10.06.2005).

This method of selection allows for a salt-free selection of rubber latex, and to use a mixture of amine coagulant in combination with mineral salt. This is bound in insoluble salt biologically non-biodegradable product that is present in the recipe synthesis lakanal, resulting prevented from getting into the waste water. Introduction part coagulant in recycled serum allows you to quickly affect the quality of the coagulant.

But this method is not free from drawbacks:

1. Two-stage variant of coagulation complicates the process.

2. Contained in the latex of unreacted monomer, Acrylonitrile (amount in latex coming coagulation, is 0.01-0.2 wt.%).

3. The number is about amine coagulant is not consistent with the number present in the latex lakanal, and is notorious excess, and in the case of use as an emulsifier of alkylsulfonate sodium in addition to the Soaps of carboxylic acids this excess is particularly significant.

The technical task of the invention is to improve the environmental performance of the process and the more effective management of coagulation.

The problem is solved in that the separation of butadiene-nitrile rubber from latex is fed into the stream of latex, the last degassing, containing from 0.01 to 0.2 wt.% free nitrile of acrylic acid, sodium sulfite or sodium bisulfite, or sodium pyrosulfite in the amount of 0.05 to 0.8 wt.%, considering latex, dispense the solution of sulfuric acid and organic amine coagulant in the form of a polymeric Quaternary ammonium salt selected from the group: polydimethyldiallylammonium, a copolymer of methacrylamide hydrochloride dimethylaminoethylmethacrylate, hydrochloride polydimethylaminoethyl, varying the amount of polymeric Quaternary ammonium salt in the range of 0.2-0.5 wt.%, counting on the rubber, depending on the content in the latex lakanal in the range of 0.1-0.4 wt.%, counting on the rubber, at a pH of coagulation 3-6 units and a temperature of 30-70°C.

This method of allocation provides:

- chemical binding free nitrile of acrylic acid with the formation of nontoxic what about the product tianetidusheti sodium:

CH2=CH2CN + Na2SO3+ H2About → NaSO3-CH2-CH2CN + NaOH;

in the process of coagulation ryanatlantic sodium reacts with polymeric Quaternary ammonium salt:

- formed polymeric ammonium salt (II) is mainly associated with lacunosum and remains in the rubber, not getting into the waste water;

- submission of the polymeric ammonium salt is produced together with the acid in apparatus for coagulation, balanced with the amount of lakanal contained in the latex, and therefore excludes the excess synthetic coagulant and he misses the waste water.

The invention is illustrated by examples of specific performance.

Example 1 (control)

To 5 kg of the latex of butadiene-nitrile rubber Nitrilase-26M, stable emulsifier Edison 1010, add the antioxidant emulsion g-30A from the calculation of 1.0 wt.% on the rubber. The dry matter content in the latex - 20 wt.%. Serves the first portion of the coagulant WMD (the product of the interaction of polyethylenepolyamine with (3,5-di-tert-butyl-4-oxybenzoyl)-dimethylamine) in the form of a 10%emulsion in the amount of 0.025 kg, which is 50% of the total dosage of amine coagulant. The General dosage is 0.5 wt.% on the rubber. Stand for 0.5 hours under stirring at 50°C. the Latex is served in the coagulation apparatus containing chamois is Yu acid and the second portion of WMD. Sulfuric acid is metered in an amount to provide a pH of serum 4,0% Crumb rubber is separated from the serum, washed with softened water, squeezed and dried in an air dryer at a temperature of 80-90°C. the selection Options are shown in table No. 2.

Example 2

Degassed latex rubber Nitrilase-AM synthesized according to the recipe shown in table 1, using as emulsifier Edison 1010, is pumped into the collection, while the flow of latex dispense 40 ml of 10%aqueous solution of sodium sulfite. The latex is heated to a temperature of 60°C, injected emulsion antioxidant SU-30A (1 wt.% on rubber) and served in apparatus for coagulation, simultaneously with the filing heated to a temperature of 60°C solution of polydimethyldiallylammonium in the amount of 0.3 wt.% with sulfuric acid. the pH in the coagulation process is supported to 5.0% by feeding additional portions of sulfuric acid. Released crumb rubber is separated from the serum, washed with softened water, squeezed and dried in an air dryer at a temperature of 80-90°C. the selection Options are shown in table No. 2.

Example 3

Latex was obtained according to the recipe shown in table 1 for rubber Nitrilase-AM using as an emulsifier a mixture of potassium soap disproportionating rosin (Edison 5600) and potassium Soaps of fatty acids of vegetable origin is I (Polinar 1618) in the amount of 2.8 wt.% on the monomers.

Subsequent operations were performed similarly to example 2. As the coagulant used polydimethyldiallylammonium. The coagulant dosage was 0.2 wt.% on the rubber, the dosage of sodium bisulfite was 0.05 wt.% to latex. Selection options are shown in table 2.

Example 4

Latex was obtained according to the recipe shown in table 1 for rubber Nitrilase-AM using as emulsifier Edison 1010 in the amount of 3.2 wt.% on the monomers, the content of the dispersant - lakanal 0.4 wt.% on the monomers and water - 270 wt.% on the monomers.

Subsequent operations were performed similarly to example 2. As the coagulant used polydimethyldiallylammonium. The coagulant dosage was 0.5 wt.% on the rubber, the dosage of sodium pyrosulfite was 0.8 wt.% to latex. Selection options are shown in table 2.

Example 5.

Latex was obtained according to the recipe shown in table 1 for rubber Nitrilase-AM using as emulsifier potassium soap of fatty acids of vegetable origin (Polinar 1618) in the amount of 2.8 wt.% on the monomers, the content of the dispersant - lakanal 0.3 wt.% on the monomers.

Subsequent operations were performed similarly to example 2. As the coagulant used is a copolymer of methacrylamide hydrochloride by dimethylaminoethylmethacrylate (SMGD). Dosage is coagulant amounted to 0.4 wt.% on the rubber, the dosage of sodium sulfite was 0.07 wt.% to latex. Selection options are shown in table 2.

Example 6

Latex was obtained according to the recipe shown in table 1 for rubber Nitrilase-AM using as emulsifier Edison 1010 in the amount of 2.8 wt.% on the monomers, the content of the dispersant - lakanal 0.3 wt.% on the monomers.

Subsequent operations were performed similarly to example 2. As the coagulant used hydrochloride polydimethylaminoethyl. The coagulant dosage was 0.4 wt.% on the rubber, the dosage of sodium sulfite was 0.07 wt.% to latex. Selection options are shown in table 2.

Example 7 (production)

Latex was obtained according to the recipe shown in table 1 for rubber Nitrilase-AM using as emulsifier Edison 1010, the content of the dispersant - lakanal 0.3 wt.% on the monomers.

Polymerization was carried out in a continuously operating polymerization battery consisting of 10 polymerization. Upon reaching the conversion of monomers to polymer of 70% of latex fueled stopper DEG and degirolami in distant columns with moist steam from divinyl under low pressure and from the nitrile of acrylic acid under vacuum, prior to its content in the latex - 0.02 wt.%.

Degassed latex was applied for the selection, with the flow of latex cont the going was injected aqueous solution of sodium sulfite in an amount of 0.07 wt.% for latex.

Latex fueled antioxidant SU-30A in the amount of 1.2 wt.% on the rubber and served in the first coagulation device, which was filed aqueous solution of sulfuric acid and an aqueous solution of coagulant - polydimethyldiallylammonium, in the amount of 0.3 wt.% on the rubber. The temperature was kept 60-65°C, pH (5,0÷5,2) unit Smagulova pulp crumb rubber was applied in the second coagulation device, in which the potassium soap of rosin and fatty acids were converted into the corresponding free acid.

Then crumb rubber was separated from the serum in the hub were washed with water, separated from the water, squeezed, dried and betteraves. The selection modes are shown in table 2.

The analysis of table 2 shows that in the sample obtained on the prototype, the number of wastewater remains unchanged, the ash content of the rubber is at the level of the known technical solutions, the number of amines in waste water decreases with adjustable dosing of coagulant depending on the content of lakanal in latex. In addition, as showed industrial production of rubber Nitrilase-AM according to the proposed scheme, the amount of waste water is substantially reduced by reducing the amount of water for leaching of rubber.

As follows from table 3, the rubber obtained the claimed method, fully complies with the specifications and not ustube the quality of the rubber, obtained in a known manner.

Table 1
The polymerization recipes
№ p/pComponents recipeDosage, wt.%
Nitrilase-AMNitrilase-AMNitrilase-AM
1Butadiene847460
2The nitrile of acrylic acid162640
3Emulsifier:
Edison 10101-2,83,2
Edison 560021,43--
Polinar 161831,432,8-
4Dispersant NF - lakanal40,10,2-0,25-0,30,4
5Gidropress of Pinna0,060,040,03
6Iron sulfate (II), 7-water0,010,0080,006
7Trilon B50,020,0160,012
8Rongalit60,080,070,06
9Tert-dodecylmercaptan0,40,450,6
10Water200200 270
11DEG70,120,110,1
Notes:
1 is a Mixture of potassium salts of disproportionating rosin and fatty acids (TU 2253-038-00278-893-2003), taken in the ratio 1:1;
2 - Potassium soap disproportionating rosin (TU 2253-038-00279-893-2003);
3 is a Mixture of distilled fatty acids of vegetable origin (TU 9146-039-58604719-2005);
4 - the Product of the interaction of naphthalenesulfonate with formaldehyde and neutralized with sodium hydroxide (GOST 6848-79);
5 - Salt disodium ethylene-diamine-tetraoxane acid (TU 2484-005-22657427-99);
6 - Formaldehyde sulfoxylate sodium (TU 6-14-61-79);
7 - Diethylhydroxylamine (TU 38.103528-2000).

As an antioxidant was used SU-30A - product of the interaction of Nonylphenol with isobutylene (TU 38.40367-87)introduced into the latex in the form of a water-base emulsion.

The latexes obtained in polymerization volume is ω 60 DM 3the Stripping was carried out at 60°C, degassing from the nitrile of acrylic acid was carried out in the distant column with water vapor under vacuum.

Table 2
Selection options rubber from latex
№ p/pThe analyzed components and parameters selectionNon examples
1 counter.234567
1.Mark allocated rubberNitrilase-AMNitrilase-AMBOC-18MBOC-40MBOC-AMBOC-AMNitrilase-AM
2The type of coagulantOMPMIC1MICMICSMGG 2GPA3MIC
3Dosage of coagulant, wt.% on rubber0,50,30,20,50,40,40,3
4The content of lakanal in latex, wt.%, on rubber0,250,250,10,40,30,30,2
5The content of free nitrile of acrylic acid in the latex, wt.%0,0250,0250,010,20,020,020,02
6The dosage of sodium sulfite, considering latex, wt.%-0,080,0540,8050,070,07
7the pH of coagulation, units4,05,03,06,04,04,05,0
8The coagulation temperature, °C60607030505065
9The content of lakanal in wastewater, mg/DM3105810795
10Content tianetidusheti in wastewater, mg/DM3-238333
11The content of amines in wastewater, mg/DM 30,290,140,130,150,170,160,13
12The ash content of the rubber, wt.%0,150,150,100,200,140,160,12
13The number of wastewater, m3/tonne rubber17171717171710
Note: 1 - VPK-402 - polydimethyldiallylammonium;
2 - SMGT - copolymer methacrylamide hydrochloride by dimethylaminoethylmethacrylate;
3 - GPA - hydrochloride polydimethylaminoethyl;
4 - this example uses sodium bisulfite;
5 - in this example, use sovan sodium pyrosulphite.

Table 3
The qualitative characteristics of the obtained rubber
№ p/pIndicatorsStandard on THE*The index value example:
1256
1Stiffness in Defoe, N.of 5.8 to 8.37,17,17,57,7
2Conditional tensile strength, MPa, not less than25,526,527,027,527,4
3Elongation at break, %, not less than625640650645650
4 The change in mass of the vulcanizate in an isooctane/toluene, %, max3428292829
5Weight loss during drying,%1,00,50,50,450,40
6Mass fraction of ash, %, max0,60,150,140,150,12
7Mass fraction of organic acids, %, max6,5of 5.45,35,55,6
8Mass fraction of Soaps of organic acids, %, max0,40,20,250,20,18
* Analysis performed across 38.40350-99

The allocation method butadiene-nitrile the rubber from latex, stable lacunosum and potassium Soaps of carboxylic acids, selected from the group of synthetic and natural fatty acids with the number of carbon atoms from 12 to 18, or a mixture thereof, kanifolnye acid or mixture of fatty acids with infolevin, by the action of mineral acid and organic amine coagulant, characterized in that the flow past the degassing latex serves sodium sulfite or sodium bisulfite, or sodium pyrosulphite in the amount of 0.05 to 0.8 wt.%, counting on the latex, the flow of latex containing sulfite, direct coagulation apparatus, which simultaneously serves aqueous solution of sulfuric acid and organic amine coagulant in the form of a polymeric Quaternary ammonium salt selected from the group: polydimethyldiallylammonium, a copolymer of methacrylamide hydrochloride dimethylaminoethylmethacrylate, hydrochloride polydimethylaminoethyl varying the amount of polymeric Quaternary ammonium salt in the range of 0.2-0.5 wt.%, counting on the rubber, depending on the content in the latex lakanal in the range of 0.1-0.4 wt.%, counting on the rubber, at a pH of coagulation 3-6 units and a temperature of 30-70°C.



 

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