CN101081828A - Production method of rubber vulcanization accelerator dibenzyl aminodithioformic acid zinc - Google Patents
Production method of rubber vulcanization accelerator dibenzyl aminodithioformic acid zinc Download PDFInfo
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- CN101081828A CN101081828A CN 200710054720 CN200710054720A CN101081828A CN 101081828 A CN101081828 A CN 101081828A CN 200710054720 CN200710054720 CN 200710054720 CN 200710054720 A CN200710054720 A CN 200710054720A CN 101081828 A CN101081828 A CN 101081828A
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Abstract
The present invention is process of producing rubber accelerator zinc dibenzyl dithiocarbamate as one kind of chemical product. The materials include dibenzyl amine, carbon bisulfide, sodium hydroxide, zinc chloride and sulfuric acid in the molar ratio of 1 to 0.95-1.35 to 0.95-1.25 to 0.48-0.65 to 0.005 -0.015. The production process includes the following steps: adding dibenzyl amine and sodium hydroxide successively to reactor holding pure water while stirring; cooling to 10-20 deg.c and dropping carbon bisulfide within 7 hr; stirring for certain time, controlling the temperature and dropping zinc chloride for metathetical reaction; regulating pH value of the reacted liquid to finish reaction; stirring for 1 hr, solid-liquid separating, eliminating liquid, stoving solid, crushing, sieving and packing.
Description
One, technical field: the present invention relates to a kind of production method of Chemicals, especially the production method of rubber vulcanization accelerator dibenzyl aminodithioformic acid zinc
Two, background technology: in recent years, along with the fast development of Rubber processing industry, the fast development of domestic automobile industry, communication industry drives the Rubber processing industry and increases fast, unprecedented good opportunity is provided for the development of Rubber Chemicals Industries.Since the entry to WTO,, compared, still have very big gap at aspects such as product inner quality and " green " green technologies with developed countries though the production of China's rubber accelerator product is improved largely.China's Auxiliaries Industry will enlarge the market share green, nontoxic auxiliary agent product, cut down significantly to contain the promotor that can produce carcinogenic substance in nitrosamine, the reprocessing process.To advancing cleaner production, the green auxiliary agent of development to give great attention, particularly eliminate the understanding that produces nitrosamine carcinogens product gradually and be rooted in the hearts of the people, and obtain first-stage success.Rubber vulcanization accelerator dibenzyl aminodithioformic acid zinc (ZBDC) is exactly a kind of green environmental protection thiofide, is widely used in the sulfuration processing of natural rubber, polyisoprene rubber, styrene-butadiene rubber(SBR), cis-1,4-polybutadiene rubber, terpolymer EP rubber and paracril etc.In modern green tire sizing material, can be used for substituting the carcinogenic ZDBC of generation nitrosamine, products such as ZDEC, PZ.
The production method of rubber vulcanization accelerator dibenzyl aminodithioformic acid zinc (ZBDC), domestic do not have bibliographical information at present, and the product major part depends on import, and the first fusing point (178 ℃) on the low side of the main quality index of product of report.The production method of the rubber vulcanization accelerator dibenzyl aminodithioformic acid zinc (ZBDC) of my company research be with water as solvent, under alkaline condition, carry out replacement(metathesis)reaction and a kind of method of synthetic with inorganic zinc salt.This method is with short production cycle, safety coefficient is high, almost do not have exhaust gas emission, and product fusing point height, outward appearance are white, and comprehensive cost is low, can satisfy the domestic and international market demand.
Three, summary of the invention: the purpose of this invention is to provide a kind of production method of producing rubber vulcanization accelerator dibenzyl aminodithioformic acid zinc, it has overcome the shortcoming that other method exists, the object of the present invention is achieved like this, raw-material stoichiometry mol ratio is dibenzylamine: dithiocarbonic anhydride: sodium hydroxide: zinc chloride: sulfuric acid=1: 0.95-1.35: 0.95-1.25: 0.48-0.65: 0.005-0.015mol; Its production process is: in the reactor that fills purified water, add dibenzylamine, the sodium hydroxide of specified amount under the whipped state successively; Be cooled under the 10-20 ℃ of temperature, begin to drip the dithiocarbonic anhydride liquid of specified amount, 7 hours periods; After dropwising, certain hour is stirred in the back, and the control optimal temperature drips liquor zinci chloridi, carries out replacement(metathesis)reaction; Reaction is an OK range with sulfuric acid conditioned reaction liquid pH value after finishing, i.e. reaction finishes.Stirred 1 hour the back, carries out solid-liquid separation, and liquid is given up, and solid dries, pulverize, sieve, pack and get final product.
1, the present invention is raw materials used
1.1, dibenzylamine: a kind of colourless or flaxen transparent oily liquid, have the trace bitter almond odor, not volatile, be alkalescence, in air, deposit color for a long time and can increase the weight of.
1.2, dithiocarbonic anhydride: colourless or little yellow volatility transparent liquid, relative density 1.265, pure product have aromatising flavour, raw product is because of containing sulphur and other impurity is faint yellow, and foul smelling.Boiling point: 46.3 ℃, lightning :-30 ℃.Be slightly soluble in water (22 ℃, 0.22g/100ml; 50 ℃, 0.14g/ml) be dissolved in pure and mild ether, high refractivity is arranged, easily flow severe toxicity.Has very strong dissolving power, solubilized fat, wax, resin, untreated rubber, sulphur, phosphorus etc.Its steam and air mixed are easy to catch fire and explode, threshold concentration 30mg/ml.
1.3, sodium hydroxide: have another name called sheet alkali, a kind of white plates solid.Density 2.130g/cm
3318.4 ℃ of fusing points.1390 ℃ of boiling points.Industrial goods contain a spot of sodium-chlor and yellow soda ash, are the solids of White-opalescent, and dilution property is strong, reveal when putting in the air, easily absorb airborne moisture deliquescence gradually, and last full one-tenth solution easily absorbs airborne CO
2Be transformed into soda ash, the aqueous solution is strong basicity, is dissolved in glycerine and ethanol, is not dissolved in acetone, and severe corrosive is arranged.
1.4, sulfuric acid: pure product are colourless, odorless, transparent colourless liquid, the acidity of flaunting the superiority.Commercially available industrial sulphuric acid is colourless to little yellow, even reddish-brown.Relative density: 98% sulfuric acid is 1.8365 (20 ℃), and 93% sulfuric acid is 1.8276 (20 ℃), and fusing point is 10.35 ℃, and boiling point is 338 ℃.Very strong adsorptive power is arranged, can mix by different ratios with water, and emit a large amount of heat, be inorganic acid, corrodibility is very strong, very alive group of chemical property.Almost can generate salt with all metals and oxide compound thereof, light oxide compound reaction, can also with the salt effect of other mineral acid.When dilute sulphuric acid, can only annotate sour entry, the sour accident of spray of blasting in case the acid solution surface local is overheated.Concentration is lower than 76% sulfuric acid and metal reaction meeting releasing hydrogen gas.
1.5, zinc chloride: pure product are white powder, odorless, easily deliquescence.Fusing point (℃): 365 boiling points (℃): 732, relative density (water=1): 2.91.Water-soluble, ethanol, ether, glycerine are insoluble to liquefied ammonia.Main application:, also be used for industries such as battery, plating, medicine as dewatering agent, condensing agent, mordant, oil scavenging agent.This product has to stimulate and corrosive nature, sucks zinc chloride smog and can cause bronchopneumonia, and high density sucks and can cause death.
2, the advantage of product of the present invention:
This product has the following advantages with its corresponding product contrast:
(1), the toxic gas quantity discharged is few in the process of producing product, environmental pollution is little.Wastewater flow rate is few, with short production cycle.
(2), product appearance is white than other similar product color, the grain warp is thin, loose.
(3), the first fusing point 〉=183 ℃ of product, purity 〉=more than 98%.
(4), shelf life of products is long, more stable at ambient temperature.
(5), in vulcanization of rubber experiment: curing time is short, and time of scorch is long, shows superior curability than similar product.
Four, description of drawings: Fig. 1 is the process flow sheet of the production method of tetra benzyl thiuram disulfide as rubber vulcanizing accelerator, and its technological process is: in the reactor that fills purified water, add dibenzylamine, the sodium hydroxide of specified amount under the whipped state successively; Be cooled under the 10-20 ℃ of temperature, begin to drip the dithiocarbonic anhydride liquid of specified amount, 7 hours periods; After dropwising, certain hour is stirred in the back, and the control optimal temperature drips liquor zinci chloridi, carries out replacement(metathesis)reaction; Reaction is an OK range with sulfuric acid conditioned reaction liquid pH value after finishing, i.e. reaction finishes; Stirred 1 hour the back, carries out solid-liquid separation, and liquid is given up, and solid dries, pulverize, sieve, pack and get final product.
Five, embodiment: the used raw-material stoichiometry mol ratio of the present invention is, dibenzylamine: dithiocarbonic anhydride: sodium hydroxide: zinc chloride: sulfuric acid=1: 0.95-1.35: 0.95-1.25: 0.48-0.65: 0.005-0.015mol, its production process is: in the reactor that fills purified water, add dibenzylamine, the sodium hydroxide of specified amount under the whipped state successively; Be cooled under the 10-20 ℃ of temperature, begin to drip the dithiocarbonic anhydride liquid of specified amount, 7 hours periods; After dropwising, certain hour is stirred in the back, and the control optimal temperature drips liquor zinci chloridi, carries out replacement(metathesis)reaction; Reaction is an OK range with sulfuric acid conditioned reaction liquid pH value after finishing, i.e. reaction finishes.Stirred 1 hour the back, carries out solid-liquid separation, and liquid is given up, and solid dries, pulverize, sieve, pack and get final product.
Claims (1)
1, the production method of rubber vulcanization accelerator dibenzyl aminodithioformic acid zinc, it is characterized in that: raw-material stoichiometry mol ratio, dibenzylamine: dithiocarbonic anhydride: sodium hydroxide: zinc chloride: sulfuric acid=1: 0.95-1.35: 0.95-1.25: 0.48-0.65: 0.005-0.015mol; Production process: in the reactor that fills purified water, add dibenzylamine, the sodium hydroxide of specified amount under the whipped state successively; Be cooled under the 10-20 ℃ of temperature, begin to drip the dithiocarbonic anhydride liquid of specified amount, 7 hours periods; After dropwising, certain hour is stirred in the back, and the control optimal temperature drips liquor zinci chloridi, carries out replacement(metathesis)reaction; Reaction is an OK range with sulfuric acid conditioned reaction liquid pH value after finishing, i.e. reaction finishes; Stirred 1 hour the back, carries out solid-liquid separation, and liquid is given up, and solid dries, pulverize, sieve, pack and get final product.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101955452A (en) * | 2010-04-29 | 2011-01-26 | 濮阳蔚林化工股份有限公司 | Method for preparing zinc dibenzyl dithiocarbamate (ZBDC) thiofide |
| CN102264817A (en) * | 2008-12-30 | 2011-11-30 | 聂洱 | Methods for making organozinc salts and compositions containing the same |
| WO2016083733A1 (en) | 2014-11-25 | 2016-06-02 | Mlpc International | Method for producing zinc dithiocarbamates |
| CN106827605A (en) * | 2016-12-14 | 2017-06-13 | 安徽德耐孚汽车减震科技技术有限公司 | A kind of production technology of automobile-used rubber tyre |
| CN107141510A (en) * | 2017-06-26 | 2017-09-08 | 常州市五洲环保科技有限公司 | Easy decentralized zinc-base vulcanization accelerator and preparation method thereof |
-
2007
- 2007-07-05 CN CN 200710054720 patent/CN101081828A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102264817A (en) * | 2008-12-30 | 2011-11-30 | 聂洱 | Methods for making organozinc salts and compositions containing the same |
| CN102264817B (en) * | 2008-12-30 | 2013-05-15 | 聂洱 | Methods for making organozinc salts and compositions containing the same |
| CN101955452A (en) * | 2010-04-29 | 2011-01-26 | 濮阳蔚林化工股份有限公司 | Method for preparing zinc dibenzyl dithiocarbamate (ZBDC) thiofide |
| CN101955452B (en) * | 2010-04-29 | 2011-11-02 | 濮阳蔚林化工股份有限公司 | Method for preparing zinc dibenzyl dithiocarbamate (ZBDC) thiofide |
| WO2016083733A1 (en) | 2014-11-25 | 2016-06-02 | Mlpc International | Method for producing zinc dithiocarbamates |
| CN106827605A (en) * | 2016-12-14 | 2017-06-13 | 安徽德耐孚汽车减震科技技术有限公司 | A kind of production technology of automobile-used rubber tyre |
| CN107141510A (en) * | 2017-06-26 | 2017-09-08 | 常州市五洲环保科技有限公司 | Easy decentralized zinc-base vulcanization accelerator and preparation method thereof |
| CN107141510B (en) * | 2017-06-26 | 2019-07-12 | 常州市五洲环保科技有限公司 | Easily dispersing type zinc-base vulcanization accelerator and preparation method thereof |
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