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A kind of polymer containing polysulfide structure and preparation method thereof

A polysulfide and polymer technology, applied in the field of polymers containing polysulfide structure and its preparation, can solve the problems of reducing production process safety, loss of raw materials, long reaction time, etc., and achieve improved anti-vulcanization reversion performance , good repeatability, simple and easy preparation process

Active Publication Date: 2016-01-20
BEIJING RED AVENUE INNOVA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since 1,6-dichlorohexane in the reaction raw material is insoluble in water, the reaction is a two-phase reaction, and the reaction time is longer. In addition, 1,6-dichlorohexane is easy to escape from the reaction system under heating conditions. Cause loss of raw materials, and, 1,6-dichlorohexane is a flammable chemical, reducing the safety of the production process

Method used

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  • A kind of polymer containing polysulfide structure and preparation method thereof
  • A kind of polymer containing polysulfide structure and preparation method thereof

Examples

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preparation example Construction

[0030] Sodium disulfide (Na 2 S 2 ) Preparation of aqueous solution

[0031] Use a 250mL four-neck flask equipped with a mechanical stirring device, a thermometer, and a reflux condenser as a reaction vessel, add 31.6g of sodium sulfide nonahydrate and 100g of water, stir and dissolve, add 12.7g of sulfur, stir and react at 50°C for 3.5h, then stop stirring , to obtain a sodium disulfide aqueous solution with a mass percentage concentration of 10%, which can be further diluted into a mass percentage concentration of 5-9% Na 2 S 2 aqueous solution.

[0032] Sodium tetrasulfide (Na 2 S 4 ) Preparation of aqueous solution

[0033] Use a 250mL four-necked flask equipped with a mechanical stirring device, a thermometer and a reflux condenser as a reaction vessel, add 43.2g of sodium sulfide nonahydrate and 85g of water, stir and dissolve, add 17.4g of sulfur, and stir at 60°C for 4 hours, then stop stirring. The obtained mass percent concentration is 30% sodium tetrasulfide ...

Embodiment 1～12

[0035] Examples 1-12: Using sodium sulfide nonahydrate and hexamethylene dihydrate 1,6-dithiosulfate disodium salt (HTS) as raw materials

Embodiment 1

[0037] Purge and stir the 500ml four-necked flask with nitrogen, and install a thermometer, a reflux condenser, and a stirrer. Add 39.0 g of HTS and 156.0 g of deionized water into the flask, turn on the stirrer, increase the internal temperature of the reactor, and completely dissolve the HTS in the water. The upper space of the reactor was purged with nitrogen again, and 120.0 g of 20% by mass aqueous solution of sodium sulfide nonahydrate was added. Then continue to raise the internal temperature of the reactor to 100° C., and stir the reaction at this temperature. During the reaction, the reaction solution gradually changed from transparent and clear to turbid, and the pH value of the reaction solution was controlled to be 12.0. After reacting for 60 minutes, a gelatinous substance was formed in the reactor, and the reaction liquid became transparent and clear, and the reaction was stopped and naturally cooled to room temperature. The reaction solution was poured out, an...

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Abstract

The invention provides a polymer containing an ether polysulfide structure and a safe and efficient preparation method thereof. According to the preparation method of the polymer containing the ether polysulfide structure, organic thiosulfate and sodium sulfide serve as raw materials and carry out homogeneous reaction in an aqueous solution or a mixed solvent of a water-soluble organic solvent and water so as to obtain a polymer containing an ether polysulfide structure, wherein a molecular structure of the polymer comprises a plurality of alkyl sulfide chain segments. The polymer containing the ether polysulfide structure can be used as a sulfurizing reagent and added in a rubber material; the alkyl sulfide in the polymer participates in a sulfuration reaction process of the rubber and can effectively carry out cross-linking reaction with the rubber material to form stable monosulphur bonds or disulphur bonds; and meanwhile, flexible alkyl chains are insertd into macromolecules of the rubber, so that anti-reversion performance of the rubber material is improved.

Description

technical field [0001] The invention belongs to the field of processing aid materials for the rubber industry, and in particular relates to a polymer containing a polysulfide structure and a preparation method thereof. Background technique [0002] Sulfur is the most commonly used vulcanizing agent for unsaturated rubbers such as natural rubber (NR), butadiene rubber (BR) and styrene-butadiene rubber (SBR). When sulfur vulcanizes rubber, sulfur forms single-sulfur bonds (bond energy 227KJ / mol), disulfide bonds (bond energy 167KJ / mol) and polysulfide bonds (bond energy 115KJ / mol) between rubber macromolecules, and also generates internal macromolecules. monosulfide or polysulfide bonds. Compared with polysulfide bonds, monosulfide bonds and disulfide bonds have greater energy, better heat resistance and aging resistance, but due to the shorter length of the sulfur chains of monosulfide bonds and disulfide bonds, its tensile properties, Poor fatigue resistance and flexural p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/02C08L21/00C08L81/02
Inventor 甄博鸣赵丽丽董栋
Owner BEIJING RED AVENUE INNOVA
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