Method for synthesizing organic fluorine modified polysiloxane linen finishing agent

A technology of polysiloxane and synthesis method, which is applied in fiber processing, textile and papermaking, plant fiber and other directions, can solve the problems affecting the yield of the final product, the structure is different, and achieves moderate price, sufficient addition reaction, and high yield. high rate effect

Inactive Publication Date: 2011-09-07
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 macromolecular polymethylhydrogensiloxane can reduce the occurrence of unnecessary by-products in the reaction process, and the yield of the target product is relatively high. There is no public report on the synthesis method of organic fluorine-modified silicone products by introducing functional groups containing organic fluorine and carboxyl groups into polysiloxane chains

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Step 1: Add polymethyl hydrogen siloxane 16.68g, toluene 32.27g, the quality of polymerization inhibitor phenothiazine in the 150mL four-neck flask that reflux condenser and dropping funnel are housed are methyl methacrylate and fluorine 0.05% of the total mass of olefins, the quality of chloroplatinic acid-isopropanol catalyst solution is 60ppm of the total mass of graft modified monomers;

[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 3.21g of methyl methacrylate containing 5.0g of toluene solution dropwise, control the time to add dropwise within 1~1.5h, heat the reaction system to 120°C, continue to stir and maintain constant temperature reaction 15h to stop the reaction and measure the conversion rate;

[0016] Step 4: Lower the reaction temperature to 80°...

Embodiment 2

[0019] Step 1: Add polymethyl hydrogen siloxane 16.68g, toluene 29.82g, the quality of polymerization inhibitor phenothiazine in the 150mL four-neck flask that reflux condenser and dropping funnel are housed are methyl methacrylate and fluorine 0.05% of the total mass of alkenes, the quality of chloroplatinic acid-isopropanol catalyst solution is 50ppm of the total mass of grafted modified monomers;

[0020] 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;

[0021] Step 3: Use a constant pressure dropping funnel to add 3.46g of methyl methacrylate containing 5.0g of toluene solution dropwise, control the time to add dropwise within 1~1.5h, heat the reaction system to 130°C, continue to stir and maintain a constant temperature reaction 15h to stop the reaction and measure the conversion rate;

[0022] Step 4: Lower the reaction temperature to...

Embodiment 3

[0025] Step 1: Add polymethyl hydrogen siloxane 16.68g, toluene 27.15g, the quality of polymerization inhibitor phenothiazine in the 150mL four-neck flask that reflux condenser and dropping funnel are housed are methyl methacrylate and fluorine 0.05% of the total mass of olefins, the quality of the chloroplatinic acid-isopropanol catalyst solution is 40ppm of the total mass of the graft modified monomer;

[0026] 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;

[0027] Step 3: Use a constant pressure dropping funnel to add 3.68g of methyl methacrylate containing 5.0g of toluene solution dropwise, control the time to add dropwise within 1~1.5h, heat the reaction system to 110°C, continue to stir and maintain constant temperature reaction 15h to stop the reaction and measure the conversion rate;

[0028] Step 4: Lower the reaction temperature...

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PUM

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Abstract

The invention relates to a method for synthesizing organic fluorine modified polysiloxane linen finishing agent, belonging to the technical field of linen finishing agent. Polymethyl hydrogen polysiloxane, methyl methacrylate and fluorinated olefin are used as raw materials which have wide sources and moderate price and ensure sufficient addition reaction, easy reaction product separation and purification and high yield of organic fluorine modified polysiloxane linen finishing agent. Being the organic fluorine modified product with a stable structure, the finishing agent has good biological aging resistance, dose not repel the animal body, has no harmful effect on the environment, is green and environmental friendly and ensures that the linen fabric has durable finishing effect, resists water, oil and foul. The method adopts the hydrosilylation reaction and the simple reaction route and ensures high conversion rate.

Description

technical field [0001] The invention relates to a method for synthesizing an organofluorine-modified polysiloxane linen finishing agent, which belongs to the technical field of synthesizing linen finishing agents with water-repelling, oil-repelling and antifouling functions. Background technique [0002] Polysiloxane has a low surface tension and has the excellent performance 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. Combining the advantages of organic fluorine and silicone, it can endow the linen fabric with excellent finishing effect. At the same time, the active carboxyl group on the polysiloxane chain can endow the reactivity between the polysiloxane chain and the flax fiber, and strengthen the silicone Long-term finishing effect of finishing agents on linen fabrics. The research and application of organic fluorine and amino-modified polysiloxane by directly using macromolecul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/12D06M15/657D06M101/06
Inventor 宋秘钊张慧君赵欣王硕孙颖郑文星
Owner QIQIHAR UNIVERSITY
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