CN102391206A - Method for producing rubber vulcanization accelerator DZ - Google Patents
Method for producing rubber vulcanization accelerator DZ Download PDFInfo
- Publication number
- CN102391206A CN102391206A CN201110280127XA CN201110280127A CN102391206A CN 102391206 A CN102391206 A CN 102391206A CN 201110280127X A CN201110280127X A CN 201110280127XA CN 201110280127 A CN201110280127 A CN 201110280127A CN 102391206 A CN102391206 A CN 102391206A
- Authority
- CN
- China
- Prior art keywords
- reaction
- accelerator
- dicyclohexyl amine
- filtration
- product
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for producing rubber vulcanization accelerator DZ. The method comprises the following steps of: adding 100-1000 ml of 10%-30% sulphuric acid into a reaction kettle with 200-1000 g of dicyclohexyl amine; subjecting the sulphuric acid to sufficiently react with the dicyclohexyl amine under the condition that the temperature is 20-80 DEG C and the rotational speed is 200-1500 r/m; after filtering, adding a product into an oxidation reactor, and then, adding 200-800 ml of isopropanol; and then, adding oxidant oxydol with the content of 7.0%-20.0% at the flow velocity of 50-100 ml/m, meanwhile, controlling the pH value of a reacting solution to be 8-11, wherein the time for dropwise adding is 1.5-4.0 hours, the product, i.e. the rubber accelerator DZ is obtained through carrying out suction filtration, water cleaning, filtering and drying after the reaction is finished, the purity of the accelerator DZ reaches over 99%, and the yield reaches to 95%. The method has the advantages that: the method has simple steps; the oxidant is oxydol which has no pollution to the environment, and further, the industrialization is easy to realize; the reaction does not generate a large amount of saliferous waste water; the right amount of the dicyclohexyl amine is used, so that the yield of the synthesized DZ is high, and the quality is good.
Description
Technical field
The present invention relates to a kind of thiofide N, the working method of N-dicyclohexyl-2-[4-morpholinodithio sulphenamide (DZ) belongs to the rubber vulcanization accelerator DZ production technical field.
Background technology
Along with the development of rubber industry, the research of vulcanization accelerator more and more comes into one's own with production.DZ is a delayed action accelerator, is the requisite a kind of primary accelerator of present rubber industry.Be specially adapted to radial, have sulfuration and promote and adhesive effect.This procedure of patent (patent No. 200810053774.5) of delivering on July 8th, 2008 comprises: Virahol and dicyclohexyl amine are joined in the stills for air blowing, under stirring condition, make dicyclohexyl amine fully be dissolved in the Virahol; Add sulfuric acid again; Control pH value simultaneously, drip M-Na salt then, simultaneously the dropping oxidizing agent Youxiaolin; Control pH value in the reaction process, suction filtration, washing, filtration, the dry rubber accelerator DZ product that gets after reaction finishes.Though the DZ quality that the method for this patent obtains has reached 99%, yield does not have concrete numerical value, and operation is gone up and need be dripped simultaneously by three kinds of raw materials, the operation more complicated.Document (scientific and technical information, 2005,7:23) reported the method for the synthetic DZ of big proportioning oxidation style.With stirring in captax, dicyclohexyl amine, the Virahol adding reactor drum, make its salify; React cooling, suction filtration, washing, filtration, the dry product that gets as oxygenant with Youxiaolin.The dicyclohexyl amine amount that this method is used is big, and the yield of accelerator DZ is not high.Document (China Synthetic Rubber Industry, 1996,19:317) reported the fast synthesis method of accelerator DZ.With stirring in captax, dicyclohexyl amine, the Virahol adding reactor drum, make its salify; React cooling, suction filtration, washing, filtration, the dry product that gets as oxygenant with ydrogen peroxide 50.This method accelerator DZ yield is low.Aforesaid method all can produce a large amount of brine wastes, and environment is polluted.
Summary of the invention
The object of the present invention is to provide a kind of be oxygenant with the ydrogen peroxide 50, be the method for raw material production rubber vulcanization accelerator DZ with M-Na salt; This method is simple to operate; Do not produce a large amount of brine wastes, the dicyclohexyl amine consumption is an amount of, and the DZ yield that synthesizes, quality are all than higher.
For achieving the above object, the present invention realizes through following technical proposals:
A kind of method of producing rubber vulcanization accelerator DZ: 10～30% sulfuric acid, 100～1000ml is joined in the reaction kettle of existing 200～1000 gram dicyclohexyl amines; Be under 200～1500 rev/mins the condition at 20～80 ℃, rotating speed; Make the abundant and dicyclohexyl amine reaction of sulfuric acid, join after the filtration in the stills for air blowing, add 200～800ml Virahol again; Adding content with 50～100ml/ minute flow velocity then is 7.0～20.0% oxidant hydrogen peroxide; Control the pH8-11 of reaction soln simultaneously, the dropping time is 1.5～4.0 hours, suction filtration, washing, filtration, the dry rubber accelerator DZ product that gets after reaction finishes.
The invention has the advantages that: this procedure is simple, and what oxygenant used is the ydrogen peroxide 50 that environment is not had pollution, and reaction does not produce a large amount of brine wastes, is easy to industriallization, and the dicyclohexyl amine of use is an amount of, and the purity of the accelerator DZ that synthesizes reaches more than 99%.Yield has reached more than 95%.
Embodiment
Embodiment 1:
500ml 30% sulfuric acid being joined in the reaction kettle of existing 1000 gram dicyclohexyl amines, is under 1500 rev/mins the condition, sulfuric acid fully to be reacted with dicyclohexyl amine at 30 ℃, rotating speed; Join in the stills for air blowing after the filtration; Add the 800ml Virahol again, adding mass content with 100ml/ minute flow velocity then is 20.0% oxidant hydrogen peroxide, controls the PH9 of reaction soln simultaneously; The dropping time is 1.5 hours; Suction filtration, washing, filtration, the dry rubber accelerator DZ product that gets after reaction finishes, the purity of product DZ reaches more than 99%, and yield has reached 95.5%.
Embodiment 2:
200ml15% sulfuric acid being joined in the reaction kettle of existing 500 gram dicyclohexyl amines, is under 600 rev/mins the condition, sulfuric acid fully to be reacted with dicyclohexyl amine at 50 ℃, rotating speed; Join in the stills for air blowing after the filtration; Add the 500ml Virahol again, adding mass content with 60ml/ minute flow velocity then is 13.0% oxidant hydrogen peroxide, controls the PH10 of reaction soln simultaneously; The dropping time is 3.0 hours; Suction filtration, washing, filtration, the dry rubber accelerator DZ product that gets after reaction finishes, the purity of product DZ reaches more than 99%, and yield has reached 95.2%.
Embodiment 3:
100ml10% sulfuric acid being joined in the reaction kettle of existing 200 gram dicyclohexyl amines, is under 500 rev/mins the condition, sulfuric acid fully to be reacted with dicyclohexyl amine at 80 ℃, rotating speed; Join in the stills for air blowing after the filtration; Add the 200ml Virahol again, adding mass content with 50ml/ minute flow velocity then is 7.0% oxidant hydrogen peroxide, controls the PH11 of reaction soln simultaneously; The dropping time is 4.0 hours; Suction filtration, washing, filtration, drying obtained the rubber accelerator DZ product after reaction finished, and the purity of product DZ reaches more than 99%, and yield has reached 95%.
Claims (1)
1. method of producing rubber vulcanization accelerator DZ; It is characterized in that with the ydrogen peroxide 50 being oxygenant, be raw material with M-Na salt: 10～30% sulfuric acid, 100～1000ml joins in the reaction kettle of existing 200～1000 gram dicyclohexyl amines; Be under 200～1500 rev/mins the condition at 20～80 ℃, rotating speed; Make the abundant and dicyclohexyl amine reaction of sulfuric acid, join after the filtration in the stills for air blowing, add 200～800ml Virahol again; Adding content with 50～100ml/ minute flow velocity then is 7.0～20.0% oxidant hydrogen peroxide; Control the pH8-11 of reaction soln simultaneously, the dropping time is 1.5～4.0 hours, suction filtration, washing, filtration, the dry rubber accelerator DZ product that gets after reaction finishes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110280127XA CN102391206A (en) | 2011-09-20 | 2011-09-20 | Method for producing rubber vulcanization accelerator DZ |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110280127XA CN102391206A (en) | 2011-09-20 | 2011-09-20 | Method for producing rubber vulcanization accelerator DZ |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102391206A true CN102391206A (en) | 2012-03-28 |
Family
ID=45858614
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110280127XA Pending CN102391206A (en) | 2011-09-20 | 2011-09-20 | Method for producing rubber vulcanization accelerator DZ |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102391206A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103102327A (en) * | 2012-11-16 | 2013-05-15 | 江苏国立化工科技有限公司 | Preparation method of rubber accelerator DZ (N,N-Dicyclohexyl-2-benzothiazolsulfene amide) |
| CN103524454A (en) * | 2013-09-30 | 2014-01-22 | 科迈化工股份有限公司 | Method for producing rubber vulcanization accelerant DZ by solvent method |
| CN103524450A (en) * | 2013-09-30 | 2014-01-22 | 科迈化工股份有限公司 | Synthetic method for accelerator DZ by using methanol as solvent |
| CN104557769A (en) * | 2014-12-16 | 2015-04-29 | 科迈化工股份有限公司 | Production method of rubber vulcanization accelerator N,N-dicyclohexyl-2-benzothiazole sulfenamide |
| CN104557774A (en) * | 2014-12-16 | 2015-04-29 | 科迈化工股份有限公司 | Synthesis method for producing accelerator N, N-dicyclohexyl-2-benzothiazolyl sulfenamide by taking isopropanol as solvent |
-
2011
- 2011-09-20 CN CN201110280127XA patent/CN102391206A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103102327A (en) * | 2012-11-16 | 2013-05-15 | 江苏国立化工科技有限公司 | Preparation method of rubber accelerator DZ (N,N-Dicyclohexyl-2-benzothiazolsulfene amide) |
| CN103524454A (en) * | 2013-09-30 | 2014-01-22 | 科迈化工股份有限公司 | Method for producing rubber vulcanization accelerant DZ by solvent method |
| CN103524450A (en) * | 2013-09-30 | 2014-01-22 | 科迈化工股份有限公司 | Synthetic method for accelerator DZ by using methanol as solvent |
| CN104557769A (en) * | 2014-12-16 | 2015-04-29 | 科迈化工股份有限公司 | Production method of rubber vulcanization accelerator N,N-dicyclohexyl-2-benzothiazole sulfenamide |
| CN104557774A (en) * | 2014-12-16 | 2015-04-29 | 科迈化工股份有限公司 | Synthesis method for producing accelerator N, N-dicyclohexyl-2-benzothiazolyl sulfenamide by taking isopropanol as solvent |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102391206A (en) | Method for producing rubber vulcanization accelerator DZ | |
| CN104276595A (en) | Preparation method of basic zinc chloride | |
| CN103818944B (en) | A kind of production method of copper chloride hydroxide | |
| CN103193732B (en) | Preparation method of rubber vulcanization accelerator DM | |
| CN102367238A (en) | Method for synthesizing accelerator N,N-dicyclohexyl-2-benzothiazole sulfenamide | |
| CN105037295A (en) | Method for producing sulfenamide rubber vulcanization accelerator | |
| CN102838565A (en) | Production method of rubber vulcanization accelerator DZ | |
| CN101157664A (en) | New method for synthesizing rubber vulcanization accelerator CZ | |
| CN101318942A (en) | Novel method for preparing vulcanized rubber accelerant DZ with cooling-down circulating water system | |
| CN101134748A (en) | Method for producing rubber vulcanization accelerator DM | |
| CN103524450A (en) | Synthetic method for accelerator DZ by using methanol as solvent | |
| CN102311420B (en) | Method for synthesizing epsilon-caprolactone | |
| CN102838561A (en) | Production method of rubber vulcanization accelerator NS (N-tertiary butyl-2-benzothiazole sulfenamide) | |
| CN103305553A (en) | Biological resourceful treatment method for ferrous sulfate | |
| CN102838562A (en) | Method for synthesizing rubber vulcanization accelerator NS (N-tertiary butyl-2-benzothiazole sulfenamide) through two-step method by taking hydrogen peroxide as oxidant | |
| CN104402786B (en) | A kind of 2,2 '-dibenzamidodiphenyl two sulphur preparing process | |
| CN102850294A (en) | Method for synthesizing rubber vulcanizing promoter CZ (N-cyclohexylbenzothiazole-2-sulphenamide) via two-step process by using hydrogen peroxide as oxidant | |
| CN101899020A (en) | DZ synthesized by mixing mother solution | |
| CN102627306A (en) | Novel method for preparing solid aluminum sulfate by using waste | |
| CN109734106B (en) | Method for preparing high-concentration sodium bisulfite solution by using industrial waste | |
| CN101157663A (en) | Method for producing rubber vulcanization accelerator NS | |
| CN101143856A (en) | Method of producing rubber vulcanization accelerator DZ | |
| CN103524454A (en) | Method for producing rubber vulcanization accelerant DZ by solvent method | |
| CN216808418U (en) | Sodium sulfate waste water resourceful treatment system | |
| CN103508977A (en) | Method for producing rubber vulcanization accelerator CZ by adopting double-dripping method using hydrogen peroxide as oxidizing agent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120328 |