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Synthesis method of epoxy group modified polyorganosiloxane flax soft finishing agent

A soft finishing agent and polysiloxane technology, which is applied in fiber treatment, textiles and papermaking, etc., can solve the problems of structure discrepancy and impact on the yield of final products, etc., and achieve sufficient addition reaction, moderate price, and simple reaction route Effect

Inactive Publication Date: 2014-02-19
QIQIHAR UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the modification of polysiloxane at home and abroad mostly starts from small molecular silane or siloxane, introduces active groups, and then obtains the required modified polysiloxane through equilibrium, but this The method requires several steps to obtain the target product, which affects the yield of the final product, and the final product may also differ from the designed structure
However, directly modifying the polymethylhydrogensiloxane of macromolecules can reduce the occurrence of unnecessary by-products in the reaction process, and the yield of the target product is relatively high. The functional group of the epoxy hydrocarbon group is introduced into the polysiloxane chain to obtain the synthesis method of the epoxy group modified silicone product. There is no public report in China.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Step 1: Add polymethyl hydrogen siloxane 13.26g, toluene 30.27g, polymerization inhibitor phenothiazine in a 150mL four-necked flask equipped with a reflux condenser and dropping funnel. 0.05% of the quality, the chloroplatinic acid-isopropanol catalyst solution quality is 60ppm of the graft modified monomer gross mass;

[0014] Step 2: Open condensed water, pass nitrogen gas for 5 minutes, heat and stir to dissolve polymethylhydrogensiloxane in toluene, and raise the temperature of the reaction system to 80°C;

[0015] Step 3: Use a constant pressure dropping funnel to add dropwise a mixed solution containing 5.0g of toluene and 3.27g of allyl glycidyl ether, control the time to add dropwise within 1~1.5h, heat the reaction system to 120°C, continue stirring and Keep the reaction at constant temperature for 15 hours to stop the reaction and measure the conversion rate; detect the conversion rate of the hydrosilylation reaction, and the reaction conversion rate reaches ...

Embodiment 2

[0017] Step 1: Add polymethyl hydrogen siloxane 13.26g, toluene 29.32g, polymerization inhibitor phenothiazine in a 150mL four-necked flask equipped with a reflux condenser and dropping funnel. 0.05% of the quality, the chloroplatinic acid-isopropanol catalyst solution quality is 50ppm of the graft modified monomer gross mass;

[0018] Step 2: Open condensed water, pass nitrogen gas for 5 minutes, heat and stir to dissolve polymethylhydrogensiloxane in toluene, and raise the temperature of the reaction system to 80°C;

[0019] Step 3: Add the mixed solution containing 5.0g of toluene and 3.52g of allyl glycidyl ether dropwise with a constant pressure dropping funnel, control the time to add dropwise within 1~1.5h, heat the reaction system to 110°C, continue stirring and Keep the reaction at a constant temperature for 15 hours to stop the reaction and measure the conversion rate; detect the conversion rate of the hydrosilylation reaction, and the reaction conversion rate reache...

Embodiment 3

[0021] Step 1: Add polymethyl hydrogen siloxane 13.26g, toluene 27.03g, polymerization inhibitor phenothiazine in a 150mL four-neck flask equipped with a reflux condenser and dropping funnel. 0.05% of the quality, the chloroplatinic acid-isopropanol catalyst solution quality is 40ppm of the graft modified monomer gross mass;

[0022] Step 2: Open condensed water, pass nitrogen gas for 5 minutes, heat and stir to dissolve polymethylhydrogensiloxane in toluene, and raise the temperature of the reaction system to 80°C;

[0023] Step 3: Add the mixed solution containing 5.0g of toluene and 3.73g of allyl glycidyl ether dropwise with a constant pressure dropping funnel, control the time to add dropwise within 1~1.5h, heat the reaction system to 100°C, continue stirring and Keep the reaction at constant temperature for 15 hours to stop the reaction and measure the conversion rate; detect the conversion rate of the hydrosilylation reaction, and the reaction conversion rate reaches mo...

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PUM

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Abstract

The invention discloses a synthesis method of an epoxy group modified polyorganosiloxane flax soft finishing agent, and belongs to the technical field of synthesis of flax finishing agents. According to the synthesis method, polymethylhydrosiloxane and allyl glycidyl ether serve as raw materials and have wide sources and moderate price, addition reaction is complete, and separation and purification of products are practical, so the obtained epoxy group modified polyorganosiloxane flax soft finishing agent has high yield. The finishing agent is an organic silicon modified product with a stable structure, has high biological ageing resistance, avoids the rejecting phenomenon with animal bodies, does no harm to the environment, is environment-friendly, and enables flax fabrics to have a durable finishing effect and high softening property. The method utilizes hydrosilylation and is simple in reaction route and high in conversion rate.

Description

technical field [0001] The invention relates to a method for synthesizing an epoxy-modified polysiloxane flax softening agent, and belongs to the technical field of flax finishing agent synthesis. Background technique [0002] Polysiloxane has a low surface tension and has the excellent property of being easy to spread and form a film on the surface of the fabric, so that the finished fabric has a unique finishing style and feel. The epoxy hydrocarbon group has reactivity, softness and good adsorption The characteristics make it widely used in fabric softening, coating, tackifying, antifouling, medicine and resin modification. Combining the advantages of epoxy groups and silicones, it can endow flax fabrics with excellent finishing effects. At the same time, the active epoxy hydrocarbon groups on the polysiloxane chains can endow polysiloxane chains with reactivity with flax fibers, enhancing the softness of silicones. Long-term finishing effect of finishing agents on linen...

Claims

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Application Information

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IPC IPC(8): C08G77/38D06M15/65
Inventor 宋秘钊郝诚诚张慧君赵欣王硕任志会孙颖
Owner QIQIHAR UNIVERSITY