- hydroxy -3,5di-tert - butylbenzaldehyde as coagulant emulsion rubbers
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(2-n,n-diethylaminoethyl)-4- hydroxy -3,5di-tert - butylbenzaldehyde as coagulant emulsion rubbers

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IPC classes for russian patent (2-n,n-diethylaminoethyl)-4- hydroxy -3,5di-tert - butylbenzaldehyde as coagulant emulsion rubbers (RU 2026858):
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Coagulant for synthetic rubber isolation from liquid media / 2281293
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Method of emulsion rubber recovery from latex Method of emulsion rubber recovery from latex / 2351610
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Described is nitrile rubber which contains repeating units of at least one α,β-unsaturated nitrile and at least one conjugated diene and has chlorine content in the range of 4 to 25 ppm with respect to nitrile rubber. Described is a method of producing said nitrile rubber by emulsion polymerisation of at least one α,β-unsaturated nitrile, at least one conjugated diene and optionally one or more other copolymerisable monomers selected from a group comprising α,β-unsaturated mono- or dicarboxylic acids, esters and amides thereof, in the presence of a molecular weight regulator, with the latex which is obtained during polymerisation and contains nitrile rubber being subjected to coagulation and the coagulated nitrile rubber subsequently being washed, wherein (i) the latex obtained during emulsion polymerisation has a pH of at least 6 before the coagulation, (ii) coagulation of the latex is carried out using at least one salt of a mono-, di- or trivalent metal, which is optionally a chloride, as precipitant, (iii) coagulation of the latex is carried out in the presence of polyvinyl acetate, which is optionally partially or fully saponified, as coprecipitant, and (iv) coagulation of latex and/or treatment of the coagulated latex is carried out using water containing chloride ions under the condition that the salt of the mono-, di- or trivalent metal (ii) is not a chloride. A method of treating nitrile rubber obtained using the method described above is described, wherein nitrile rubber is subjected to (i) either a metathesis reaction only or (ii) a metathesis reaction and subsequent hydrogenation, or (iii) hydrogenation only, to obtain optionally hydrogenated nitrile rubber. Described is use of said nitrile rubber, optionally hydrogenated nitrile rubber, to obtain vulcanised mixtures, obtained by mixing at least one nitrile rubber or at least one optionally hydrogenated nitrile rubber, at least one cross-linking agent and optionally other additives. Described is a method of making moulded articles in form of a seal, a cap, a hose or a diaphragm, in particular an O-ring seal, a flat seal, a dynamic seal, a sealing sleeve, a sealing cap, an oil cooler hose, a hydraulic booster hose, an air conditioner hose, a thermal insulation hose, a diaphragm for hydro bearings or a diaphragm for a diaphragm pump, through vulcanisation during moulding, preferably via pressure casting of said vulcanised mixture.
Method of producing fine polytetrafluorethylene powder Method of producing fine polytetrafluorethylene powder / 2478653
Invention relates to a method of producing fine polytetrafluoroethylene powder, as well as fine powder obtained using said method. The method of producing fine polytetrafluoroethylene powder involves emulsion polymerisation of tetrafluoroethylene in the presence of an aqueous medium, a fluorinated surfactant and a radical polymerisation initiator to obtain an aqueous emulsion of polytetrafluoroethylene and coagulation thereof in the presence of at least one apparent density-reducing compound selected from a group consisting of ammonia, an ammonium salt and urea, in amount ranging from 0.4 to 10 pts.wt per 100 pts.wt polytetrafluoroethylene. The fine polytetrafluoroethylene powder obtained using said method has standard specific mass from 2.140 to 2.180 and paste extrusion pressure from 10 to 25 MPa.

(57) Abstract:

The invention relates to substituted bansilalpet, in particular (2-N,N-diethylaminoethyl)-4-hydroxy-3,5 - di-tert-butylbenzaldehyde with coagulating activity that can be used in the manufacture of synthetic emulsion rubbers. Goal - the creation of new more effective substances of the specified class. Synthesis of lead processing Mannich bases of 2-diethylaminoethylamine at 120 - 130°C and 2 mm RT.article by distillation of the excess amine. Yield 98%; mol.m. 346. A new substance used in the process of coagulation of latex rubber SKS-30 AMIS at 60%, followed by acidification with an aqueous solution of sulfuric acid. Consumption of coagulant is reduced from 3.7 to 2.9 kg/so 1 Il., 5 table.

The invention relates to the production of synthetic rubber by emulsion polymerization method.

It is known that at the present time in the manufacture of IC at the stage of selection of rubber from latex spent 200-250 kg of salt or 30-90 kg aluminum salts or calcium per 1 ton of rubber. The use of large quantities of salts in the allocation of rubber from latex causes salinization of the most valuable freshwater reservoirs, which leads to irreversible changes in their communities and n is atiti or exclude salinization of freshwater reservoirs.

However, firstly, metacid has a high bactericidal and fungicidal action, so its accumulation in serum and lavage leads to disruption of biological wastewater treatment.

Secondly, the coagulation of rubber with metacid is different from the industrial technology selection rubbers using known coagulants - proteins, NaCl and the proposed new coagulant Navy-80.

Known protein coagulant Navy-100A.

When using protein coagulants in industry the UK has found the following disadvantages:
protein hydrolysates in the hot season and warm regions of the country are exposed to bacterial contamination and subsequently rot, forming products of metabolism with an unpleasant odor;
to avoid contamination of the equipment upon receipt, storage, transportation and use of protein hydrolysates required thorough rinsing with water, long-term treatment with live steam and process disinfecting solution of formalin;
protein hydrolysates are not independent stabilizers rubbers, they are applied only in the presence of additional stabilizers, providing pological at the same time the ability of effective coagulant and stabilizer for rubbers.

This goal is achieved using (2-N,N-diethylaminoethyl)-41OK-si-31, 51di-tert-butylbenzaldehyde formula (I) as a coagulant rubber
(I)
The compound of formula (I) are not described in literature. It has the following advantages;
has a simple way to obtain;
at the same time is an effective coagulant and anti-roll rubber;
the offered product is not subject to bacterial contamination and does not require preservatives;
the offered product can be used both independently and in a mixture with known coagulants from a number of proteins, synthetic amines.

The invention is illustrated by the following examples.

P R I m e R 1. In a three-neck flask equipped with a reflux condenser and a thermometer, loads of 52.6 g (0.2 mol) of Mannich bases (TU 38.103368-87) and 29.2 g (0.22 mol) of 2-Diethylaminoethanol [Catalog Handbook of Fine Chemicals, Aldrich Chemical Company. 1986-1987 G., R. 465; Sigma Price List, 1987, 508].

The reaction mixture is heated to a temperature of 120-130aboutC for 5 h and then distilled off the excess 2-diethylaminoethylamine at 2 mm RT.article In the flask remains the finished product, representing masljanistej)-41-hydroxy-31, 51di-tert-butylbenzaldehyde) is a transparent oily liquid with a refractive index (nD20), equal GBPUSD crossed over 1.5100.

Found, %: C 72,1; H 10,4; N 4,1; S 8,8.

Mol. weight 346.

Calculated, %: From 71.8; H 10,5; N 4,0; S 9,1.

Mol. mass 351.

PMR-spectrum, shown in the drawing is cleared spectrometer
EM-390 "Vrian"; working frequency of 90 MHz.

The internal standard tetramethylsilane was (T. M. S.).

Further to simplify the connection - 2-N,N-diethylaminoethyl-41-hydroxy-31, 51di-tert-butylbenzaldehyde, will be presented under the cipher Navy-80.

P R I m m e R 2. In 100 ml best choice (-methylstyrene) latex, pre-heated to 60aboutWith, with stirring, first enter the coagulant Navy-80, and then serves a 1% aqueous solution of H2SO4to pH 3. After 10 minutes of mixing is complete coagulation of the latex serum transparent.

In control experiments using known protein coagulant Navy-100A and known metacid. Coagulation is carried out in the same conditions.

The selected rubber is washed, dried and subjected to tests under heat aging at 140about

COI = 100%.

The results in the consumption of coagulants and their ability to stabilize the rubber under heat aging are given in table. 1.

Results table. 1 confirm that the product Navy-80 is simultaneously effective coagulant and anti-roll rubber.

P R I m e R 3. 100 ml of the production the best choice latex rubber SKS-ARK and SCS-ARKM-15 enters a different dosage of the product offered Navy-80 and docomplete carried out by adding the required amount of protein coagulant Navy-100A acidification with 1% solution of N2SO4to rn.

The obtained rubber was washed, dried and subjected to the tests for resistance to heat aging (COI) and determine the content of gel in the polymer.

In table. 2 shows the results of the tests.

In table. 2 shows that the proposed product causes a significant reduction in coagulant Navy-100A, and the dosage of the Navy-80 3 kg/ton of rubber does not require additional protein coagulant. The resistance of rubbers to heat ageing in a joint application products Navy-100A and Navy-80 is at a high level.

P R I m e R 4. In 100 ml best choice latex cout Navy-80. The latex is heated to 60aboutWith and allocate additional introduction of coagulant Navy-100A acidification 1% N2SO4or without coagulant Navy-100A only using 1% aqueous solution of sulfuric acid.

Control experiments are performed with the product of the Navy-100A and 1% N2SO4.

The results of the expenditure of the coagulants are given in table. 3.

In table. 3 shows that with the decrease of the dispersant lakanal in latex significantly reducing the amount of coagulant Navy-80 allocation rubber as when it is used alone, or in combination with coagulant Navy-100A.

P R I m e R 5. In 100 ml on BNR and polybutadiene latex synthesized in the presence of emulsifier potassium soap of FLC (fraction10-C16and disperser of lakanal, first enter the desired amount of product Navy-80 and 1% N2SO4to pH 3. Rubber has been fully allocated, serum transparent. Control experiments carried out with the coagulant Navy-100A and metaldom.

Ready rubbers are tested for stability against heat aging (COI).

The results in the consumption of coagulants and COI are shown in table. 4.

P R I m e R 6. In pre-heated to 60aboutWith latex when pechanga selection of rubber.

These conditions are optimal allocation only for coagulant metacid.

In table. 5 shows comparative data on the consumption of coagulants - metacid and Navy-80.

The presented results confirm that the expenditure proposed coagulant Navy-80, unlike metacid not depends on how and where to enter it in latex.

(2-N,N-DIETHYLAMINOETHYL)-4'-HYDROXY-3',5'-DI-TERT-BUTYLBENZALDEHYDE AS COAGULANT EMULSION RUBBERS.

(2-N, N-diethylaminoethyl)-4'-hydroxy-3', 5'-di-tert-butylbenzaldehyde formula
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as coagulant emulsion rubbers.

 

 

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