Unlock instant, AI-driven research and patent intelligence for your innovation.
A rapid manufacturing method of dicyclohexyl disulfide
What is Al technical title?
Al technical title is built by PatSnap Al team. It summarizes the technical point description of the patent document.
A dicyclohexyl disulfide, fast technology, applied in the chemical field, can solve the problems of productivity bottleneck, long reaction time, elevated temperature and reaction pressure, etc., and achieve the effect of fast reaction speed, fast reaction rate and mild reaction conditions
Active Publication Date: 2015-05-27
TANGYIN YONGXIN CHEM CO LTD
View PDF4 Cites 0 Cited by
Summary
Abstract
Description
Claims
Application Information
AI Technical Summary
This helps you quickly interpret patents by identifying the three key elements:
Problems solved by technology
Method used
Benefits of technology
Problems solved by technology
[0002] Dicyclohexyl disulfide is the intermediate raw material for the manufacture of rubber vulcanization anti-scorch agent. The method of using chlorocyclohexane and sodium disulfide to react is the existing known and common technology of dicyclohexyl disulfide manufacturing technology, such as: Northwest University "Synthesis of Dicyclohexyl Disulfide" in 1977; Qingdao Chemical Industry "Synthesis of Dicyclohexyl Disulfide" in 1995; Nanjing University "Synthesis Process Analysis of Dicyclohexyl Disulfide" in 2005, Chinese patent 200710102258.2 and Chinese patent 201110276725.X and other technical documents have relatively detailed disclosures and publications on this technical solution, but these technical solutions generally have a defect that the reaction time is too long. In order to shorten the synthesis reaction of chlorocyclohexane and sodium disulfide Time, some techniques use elevated temperature and reaction pressure, and some choose different polar solvents, but even after using these means, the reaction cycle is still more than 8 hours, and even 15 hours, which has caused a great deal of increase in productivity. the bottleneck
Method used
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more
Image
Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
Click on the blue label to locate the original text in one second.
Reading with bidirectional positioning of images and text.
Smart Image
Examples
Experimental program
Comparison scheme
Effect test
example 1
[0012] In a 1L reactor, put 64g of mixed solvent into the mixture, which is prepared from 32g of water and 32g of DMSO, add 35g of 60% sodium sulfide under heating and stirring, containing 0.269 mole of sodium sulfide, 9.5g of sulfur, 0.297 mole of sulfur, 3g of caustic soda, 0.075 mol, stir and heat at 60°C for 0.5 hours, then add 47g of chlorocyclohexane with a purity of 97%, containing 0.385 mol of chlorinated cyclohexane, seal and heat to 105°C, pressure 0.05-0.1Mpa, keep stirring for 1 hour , cooling, standing for stratification, and liquid separation to obtain 43.3g of oil layer, and its composition (GS) was measured by gas chromatography:
[0013]
example 2
[0015] In a 1L reaction kettle, put 53g of a mixed solvent, which is prepared from 21g of water and 32g of DMSO, add 35g of 60% sodium sulfide under heating and stirring, containing 0.269 moles of sodium sulfide, 9.5g of sulfur, 0.297 moles, and 3g of caustic soda , 0.075 moles, stirred and heated at 60°C for 0.5 hours; then added 47g of chlorocyclohexane with a purity of 97%, containing 0.385 moles of chlorocyclohexane, sealed and heated to a temperature of 105°C, a pressure of 0.05Mpa to 0.1Mpa, and kept warm Stir for 1 hour, cool, let stand to separate layers, and separate liquid to obtain 43.2 g of oil layer, and its composition is measured by gas chromatography (GC):
[0016]
example 3
[0018] In a 1L reaction kettle, put 53g of mixed solvent, which is prepared from 21g of water and 32g, add 35g of 60% sodium sulfide under heating and stirring, containing 0.269 moles of sodium sulfide, 10g of sulfur, 0.3125 moles, 3g of caustic soda, 0.075 Mole, stirred and heated at 60°C for 0.5 hours, then added 47g of chlorocyclohexane with a purity of 97%, containing 0.385 moles of chlorocyclohexane, sealed and heated to 105°C, 0.05Mpa~0.1Mpa, kept stirring for 1 hour, Cooling, standing for stratification, and liquid separation to obtain 43.3g of oil layer, its composition was measured by gas chromatography (GC):
[0019]
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More
PUM
Login to View More
Abstract
The invention discloses a rapid manufacturing method of dicyclohexyl disulfide, and belongs to the chemical field. According to the method, sodium disulfide and chlorocyclohexane are reacted, wherein the reaction is performed in a mixed solvent, the mixed solvent is prepared by mixing a polar solvent and a polar aprotic solvent, the polar solvent is water or methanol or ethanol, the polar aprotic solvent is sulphone or sulfoxide or dimethylformamide, and the volume ratio of the polar solvent to the polar aprotic solvent is 1:1-2. The method has advantages of low reaction temperature, good environment, safe operation, rapid reaction speed, high conversion rate, high selectivity and conversion rate of disulphide, great benefit for enterprises and the society, and broad market prospect.
Description
technical field [0001] The invention relates to a method for manufacturing dicyclohexyl disulfide, an intermediate raw material of a rubber vulcanization anti-scorch agent, in particular to a method for rapidly manufacturing dicyclohexyl disulfide, which belongs to the field of chemistry. Background technique [0002] Dicyclohexyl disulfide is the intermediate raw material for the manufacture of rubber vulcanization anti-scorch agent. The method of using chlorocyclohexane and sodium disulfide to react is the existing known and common technology of dicyclohexyl disulfide manufacturing technology, such as: Northwest University "Synthesis of Dicyclohexyl Disulfide" in 1977; Qingdao Chemical Industry "Synthesis of Dicyclohexyl Disulfide" in 1995; Nanjing University "Synthesis Process Analysis of Dicyclohexyl Disulfide" in 2005, Chinese patent 200710102258.2 and Chinese patent 201110276725.X and other technical documents have relatively detailed disclosures and publications on th...
Claims
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More
Application Information
Patent Timeline
Application Date:The date an application was filed.
Publication Date:The date a patent or application was officially published.
First Publication Date:The earliest publication date of a patent with the same application number.
Issue Date:Publication date of the patent grant document.
PCT Entry Date:The Entry date of PCT National Phase.
Estimated Expiry Date:The statutory expiry date of a patent right according to the Patent Law, and it is the longest term of protection that the patent right can achieve without the termination of the patent right due to other reasons(Term extension factor has been taken into account ).
Invalid Date:Actual expiry date is based on effective date or publication date of legal transaction data of invalid patent.
Login to View More 
Login to View More