CN101402616B - Method for producing rubber vulcanization agent 4,4'-disulfuration dimorpholine - Google Patents
Method for producing rubber vulcanization agent 4,4'-disulfuration dimorpholine Download PDFInfo
- Publication number
- CN101402616B CN101402616B CN2008102307288A CN200810230728A CN101402616B CN 101402616 B CN101402616 B CN 101402616B CN 2008102307288 A CN2008102307288 A CN 2008102307288A CN 200810230728 A CN200810230728 A CN 200810230728A CN 101402616 B CN101402616 B CN 101402616B
- Authority
- CN
- China
- Prior art keywords
- solvent
- product
- added
- dimorpholinyl disulfide
- vulcanizing agent
- 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.)
- Expired - Fee Related
Links
Landscapes
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a method for producing rubber vulcanizing agent 4, 4'-dimorpholinyl disulfide, which belongs to the chemical technical field. The method comprises the following steps: prime city naphtha is added in a reaction kettle; sodium hydroxide fine powder is added to the solvent gradually under stirring condition; drewamine is added to the solvent; sulfur chloride is dripped withinthree to four hours at a temperature between 20 and 60 DEG C; after the mixture reacts for half an hour, the stirring is stopped; the mixture is kept stand for delamination; the sodium chloride deposited in the lower layer is discharged out; materials in the kettle are added with small amount of water to wash the materials, and are filtered to reclaim the solvent; the solvent is subjected to centrifuge-dripping to obtain a white crystal product; and the product is dried to obtain rubber vulcanizing agent 4, 4'-dimorpholinyl disulfide. The method can improve the yield and quality of the product, and reduce waste water discharge. The product has a melting point higher than 122 DEG C and ash content less than 0.5 percent.
Description
Technical field
The present invention relates to a kind of production method of vulcanizer, especially a kind of vulcanizer 4,4 '-production method of dimorpholinyl disulfide, belong to chemical technology field.
Background technology
4,4 '-dimorpholinyl disulfide is a kind of thiofide, can be applicable to various dynamic goods as natural gum and various synthetical glue and blended rubber vulcanizing agent thereof, be usually used in high-quality rubber articles manufacturings such as radial tyre, engineering tyre, Bias tyre, the butyl inner tube of a tyre and rubber seal.Existing 4,4 '---the dimorpholinyl disulfide production method is that morpholine and sulfur monochloride are reacting in the mixed solvent of toluene and benzene under the liquid caustic soda existence condition, reaction finishes the back and produces a large amount of trade effluents and a large amount of washes, caused the improvement difficulty of environment, and the existence of water has increased the side reaction of water and sulfur monochloride in the liquid caustic soda, thereby makes that the yield of product is low and of poor quality, and the fusing point of product is low, only reach 118-120 ℃, ash content 0.5%-0.8%.
Summary of the invention
Task of the present invention provide a kind of vulcanizer 4,4 '-production method of dimorpholinyl disulfide, this method can improve the yield and the quality product of product, the fusing point height of product, and reduce discharge of wastewater.
For realizing above-mentioned task, technical solution of the present invention is:
A kind of vulcanizer 4,4 '-production method of dimorpholinyl disulfide, may further comprise the steps: add solvent oil in the reactor, under agitation condition, the sodium hydroxide fine powder is added in the solvent gradually, and add morpholine, under 20-60 ℃ of temperature, in 3-4h, sulfur monochloride is dropwised, behind the reaction 0.5h, stop to stir standing demix, the sodium-chlor of the lower sediment of draining, material adds the less water washing once again in the still, filtered and recycled solvent, centrifuge dripping get the white crystals product, oven dry.
The inventive method can improve the yield and the quality product of product, and the fusing point of product is higher than 122 ℃, and ash content is less than 0.5%, and the minimizing discharge of wastewater.
Embodiment
Example 1, in 2000 liters reactor, add dimethylbenzene 900kg, open and stir, add sodium hydroxide fine powder 111kg in batches, under 20-40 ℃ of temperature, 3.5 hour drip sulfur monochloride 155kg, open the chuck water coolant in the dropping process, after dropwising, continue to stir half an hour, standing demix, the sodium-chlor of the lower sediment of draining continues to stir, and adds the interior material of 100kg water washing still once, the lower layer of water of draining, suction filtration also reclaims solvent, and centrifuge dripping gets the white crystals product, and oven dry obtains the 255kg product under 80 ℃ of temperature.After testing, the product fusing point is 123.5 ℃, and ash content is 0.20%.
Example 2, in 2000 liters reactor, add 120# solvent oil 900kg, open and stir, add sodium hydroxide fine powder 112kg in batches, under 30-50 ℃ of temperature, dripped sulfur monochloride 153kg in 3 hours, open the chuck water coolant in the dropping process, after dropwising, continue to stir half an hour, standing demix, the sodium-chlor of the lower sediment of draining continues to stir, and adds the interior material of 100kg water washing still once, the lower layer of water of draining, suction filtration also reclaims solvent, and centrifuge dripping gets the white crystals product, and oven dry obtains the 260kg product under 100 ℃ of temperature.After testing, the product fusing point is 122.5 ℃, and ash content is 0.25%.
Claims (1)
- A vulcanizer 4,4 '-production method of dimorpholinyl disulfide, may further comprise the steps: add solvent oil in the reactor, under agitation condition, the sodium hydroxide fine powder is added in the solvent gradually, and add morpholine, under 20-60 ℃ of temperature, in 3-4h, sulfur monochloride is dropwised, behind the reaction 0.5h, stop to stir standing demix, the sodium-chlor of the lower sediment of draining, material adds the less water washing once again in the still, filtered and recycled solvent, centrifuge dripping get the white crystals product, oven dry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102307288A CN101402616B (en) | 2008-11-04 | 2008-11-04 | Method for producing rubber vulcanization agent 4,4'-disulfuration dimorpholine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102307288A CN101402616B (en) | 2008-11-04 | 2008-11-04 | Method for producing rubber vulcanization agent 4,4'-disulfuration dimorpholine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101402616A CN101402616A (en) | 2009-04-08 |
| CN101402616B true CN101402616B (en) | 2011-07-27 |
Family
ID=40536798
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008102307288A Expired - Fee Related CN101402616B (en) | 2008-11-04 | 2008-11-04 | Method for producing rubber vulcanization agent 4,4'-disulfuration dimorpholine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101402616B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910102A (en) * | 2015-04-16 | 2015-09-16 | 宜兴市聚金信化工有限公司 | Preparation method of rubber vulcanizing agent dimorpholinyl disulfide |
| CN105367496B (en) * | 2015-12-04 | 2019-03-08 | 山东阳谷华泰化工股份有限公司 | A kind of synthetic method of vulcanizing agent 1,1- dicaprolactam disulfide |
| CN109265414A (en) * | 2017-07-18 | 2019-01-25 | 宜兴市聚金信化工有限公司 | A kind of preparation method of improved vulcanizer dimorpholinyl disulfide |
| CN109265741A (en) * | 2017-07-18 | 2019-01-25 | 宜兴市聚金信化工有限公司 | A kind of improved vulcanizer dimorpholinyl disulfide |
| CN114105904A (en) * | 2021-11-25 | 2022-03-01 | 蔚林新材料科技股份有限公司 | Preparation method of rubber organic polysulfide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121703A (en) * | 2007-09-19 | 2008-02-13 | 濮阳蔚林化工股份有限公司 | Method for producing rubber vulcanizing agent N,N-dithiodimorpholine |
-
2008
- 2008-11-04 CN CN2008102307288A patent/CN101402616B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121703A (en) * | 2007-09-19 | 2008-02-13 | 濮阳蔚林化工股份有限公司 | Method for producing rubber vulcanizing agent N,N-dithiodimorpholine |
Non-Patent Citations (4)
| Title |
|---|
| Alan R. Katritzky et. al..The synthesis of bis（N，N-disubstituted amino）trisulphides.《J. SYNLETT》.1990,第8卷第473-476页尤其第475页. * |
| Medicinal Chemistry》.2000,第8卷第2549-2560页尤其第2558页实验部分第2段. * |
| Walter Beerheide et. al..Inactivation of the Human Papillomavirus-16 E6 Oncoprotein by Organic Disulfides.《Bioorganic & Medicinal Chemistry》.2000,第8卷第2549-2560页尤其第2558页实验部分第2段. |
| Walter Beerheide et. al..Inactivation of the Human Papillomavirus-16 E6 Oncoprotein by Organic Disulfides.《Bioorganic & * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101402616A (en) | 2009-04-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101402616B (en) | Method for producing rubber vulcanization agent 4,4'-disulfuration dimorpholine | |
| CN1080292C (en) | Process for preparing quinacridone pigments | |
| CN1756719A (en) | Novel method and device from rice husk ash silicon-dioxide | |
| CN102348673A (en) | Chemical recycling of pla by hydrolysis | |
| CN101712476A (en) | Method for preparing precipitated silica from tetrachlorosilane | |
| CN105061357A (en) | 2-mercaptobenzothiazole refining method | |
| CN106006676B (en) | A kind of method of NaOH in recovery H soda acid process of smelting | |
| NO158220B (en) | ORGANOTITANATES OR MIXTURES OF ORGANOTITANATES. | |
| CN101717379A (en) | Production method of rubber vulcanizing accelerator CBS | |
| CN102838563A (en) | Synthesis method of rubber vulcanization accelerator TBBS (N-tert-butyl-2-benzothiazolesulfenamide) | |
| CN105152174B (en) | A kind of preparation method of high-purity white carbon | |
| CN1224723C (en) | Processing method for industrial waste material | |
| CN101121703A (en) | Method for producing rubber vulcanizing agent N,N-dithiodimorpholine | |
| CN1077588C (en) | Process for preparing linear unsubstituted beta-phase quinacridone pigments | |
| CN104592161A (en) | Method for producing rubber vulcanization accelerator CBS by crude product MBT | |
| CN101100461B (en) | Thiadiazoles derivative for halopolymer vulcanization crosslinking and synthetic method for the same | |
| CN110743476B (en) | Multifunctional calcium hydroxide preparation tank and preparation method | |
| CN106866468A (en) | A kind of environment-friendly preparation method of 4 ASC | |
| CN110143922A (en) | A kind of synthetic method of 1,1 '-dicaprolactam disulfides | |
| CN105732451B (en) | Thiofide PZ is produced without waste water | |
| CN109354051A (en) | A method of calcium carbonate is prepared in Galuber's salt type brine cleaning procedure using carbide slag substitution lime | |
| WO2021211021A2 (en) | Method for regeneration of rubber | |
| CN104447393B (en) | A kind of method producing azoic coupling component AS and recovery and reuse of waste | |
| CN101081840A (en) | Production method of rubber vulcanization accelerator N-cyclohexyl-2-benzothiazole sulfonamide | |
| WO2014183381A1 (en) | Method for caustic purification of silicon carbide filter cake |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110727 Termination date: 20151104 |
|
| EXPY | Termination of patent right or utility model |