CN1159321C - Synthesizing method for di-(gamma-triethyloxy silico propyl) disulphide compound - Google Patents
Synthesizing method for di-(gamma-triethyloxy silico propyl) disulphide compound Download PDFInfo
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- CN1159321C CN1159321C CNB021159882A CN02115988A CN1159321C CN 1159321 C CN1159321 C CN 1159321C CN B021159882 A CNB021159882 A CN B021159882A CN 02115988 A CN02115988 A CN 02115988A CN 1159321 C CN1159321 C CN 1159321C
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- gamma
- disulfide
- synthesizing method
- propyl
- triethyloxy
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Abstract
The present invention relates to a synthesizing method for di-(gamma-triethoxy silicane propyl) disulphide compounds. Sodium disulfide and gamma-chloropropyltriethoxysilane are used as raw materials, absolute alcohol is used as a solvent, and the required di-(gamma-triethoxy silicane propyl) disulphide compound is obtained by a back flow reaction. The synthesizing method provided by the present invention has the advantages of simplicity, no pollution, low product cost, high yield and high purity.
Description
Technical Field
The invention relates to a method for synthesizing a bis- (gamma-triethoxysilylpropyl) disulfide compound.
Background
The bis- (gamma-triethoxysilylpropyl) disulfide compound is an important variety in a silane coupling agent family, and the product can be used as a coupling agent of rubber, can improve the mechanical property of the rubber, improves the tensile strength, the tear resistance, the wear resistance and other strengths of the rubber, and has good application prospect. At present, no literature report exists on the synthesis method of the bis- (gamma-triethoxysilylpropyl) disulfide compound.
Disclosure of Invention
The invention aims to provide a method for synthesizing a bis- (gamma-triethoxysilylpropyl) disulfide, which is simple, low in cost and high in yield.
The chemical structural formula of the bis- (gamma-triethoxysilylpropyl) disulfide compound is as follows:
the technical scheme provided by the invention is as follows: a process for synthesizing bis- (gamma-triethoxysilylpropyl) disulfide includes reflux reaction between sodium disulfide and gamma-chloropropyltriethoxysilane as raw materials and absolute alcohol as solvent.
The sodium disulfide can be obtained by mixing sodium sulfide and sulfur, heating and melting to 350-400 ℃, and cooling in a dryer.
The synthesis method provided by the invention is simple and pollution-free, and the obtained product has high yield and purity and low cost.
Detailed Description
The method comprises the steps of reacting sodium sulfide with 0.9-1.1 times of sulfur (molar ratio), heating and melting to 350-400 ℃, and cooling in a dryer to obtain sodium disulfide solid. And then reacting gamma-chloropropyltriethoxysilane with 0.5-0.6 times of sodium disulfide (molar ratio), heating and refluxing with 3-4 times (volume of gamma-chloropropyltriethoxysilane) of absolute ethyl alcohol or methanol, propanol and the like as solvents for 3 hours, filtering to remove inorganic salt solids after the reaction is finished, distilling to recover the absolute ethyl alcohol or the methanol and the propanol, cooling and filtering to obtain the product. The yield is more than or equal to 90 percent.
The chemical reaction formula in the synthesis process is as follows:
example (b): adding 0.35mol of industrial sodium sulfide and 0.37mol of industrial sulfur into a crucible, stirring and heating by using an electric furnace in a fume hood to perform chemical reaction at the reaction temperature of 350-400 ℃, then quickly pouring the product into a vessel in a dryer, cooling, crushing the product under a dry condition, and drying and storing for later use. Adding 70ml of anhydrous industrial ethanol into a reactor, rapidly adding 25g of self-made sodium disulfide (or adopting a commercially available product), dropwise adding 0.28mol of gamma-chloropropyltriethoxysilane within 20-30 minutes while stirring and heating, boiling and refluxing for 3-4 hours, and controlling the temperature at 70-80 ℃. Then cooling and filtering, removing inorganic salt filter residue, heating and distilling the filtrate, recovering anhydrous industrial ethanol, and cooling and filtering to obtain filtrate, namely the required product. The yield is more than 90%, the disulfide content is 79-83%, and the trisulfide and polysulfide content is 13-16%.
Claims (2)
1. A method for synthesizing a bis- (gamma-triethoxysilylpropyl) disulfide compound is characterized by comprising the following steps: the required bis- (gamma-triethoxysilylpropyl) disulfide compound is prepared by taking sodium disulfide and gamma-chloropropyltriethoxysilane as raw materials and absolute ethyl alcohol as a solvent through reflux reaction.
2. The method of synthesis according to claim 1, wherein: the sodium disulfide is obtained by mixing sodium sulfide and sulfur, heating and melting to 350-400 ℃, and cooling in a dryer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021159882A CN1159321C (en) | 2002-06-17 | 2002-06-17 | Synthesizing method for di-(gamma-triethyloxy silico propyl) disulphide compound |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021159882A CN1159321C (en) | 2002-06-17 | 2002-06-17 | Synthesizing method for di-(gamma-triethyloxy silico propyl) disulphide compound |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1392150A CN1392150A (en) | 2003-01-22 |
| CN1159321C true CN1159321C (en) | 2004-07-28 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021159882A Ceased CN1159321C (en) | 2002-06-17 | 2002-06-17 | Synthesizing method for di-(gamma-triethyloxy silico propyl) disulphide compound |
Country Status (1)
| Country | Link |
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| CN (1) | CN1159321C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6378100B2 (en) * | 2015-01-28 | 2018-08-22 | 住友ゴム工業株式会社 | Rubber composition for tire and tire |
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2002
- 2002-06-17 CN CNB021159882A patent/CN1159321C/en not_active Ceased
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| Publication number | Publication date |
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| CN1392150A (en) | 2003-01-22 |
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| IW01 | Full invalidation of patent right |
Decision date of declaring invalidation: 20071101 Decision number of declaring invalidation: 10399 |