Acyloxy containing hydroxyalkyl polysiloxane and preparation method

A technology containing acyloxy hydroxyalkyl polysiloxane and hydroxyalkyl methacrylate, which is applied in the field of organosiloxane synthesis and can solve the problems affecting the performance of modified polyacrylic acid and polyether, and the breaking of molecular chains. , to achieve the effect that the synthesis conditions are mild and not harsh, and the raw materials are convenient and easy to obtain.

Inactive Publication Date: 2015-11-04
SICHUAN YIXIN TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] For example, they are modified by the condensation reaction of the silanol group in the hydroxyl-terminated polysiloxane with the carboxyl group, hydroxyl group and other groups in the polyacrylate or polyether, but the reaction generates easily hydrolyzed Si—O—C bonds , after hydrolysis, the silicon hydroxyl group will be regenerated, resulting in the breakage of the molecular chain, which will seriously affect the performance of modified polyacrylic acid and polyether.

Method used

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  • Acyloxy containing hydroxyalkyl polysiloxane and preparation method
  • Acyloxy containing hydroxyalkyl polysiloxane and preparation method
  • Acyloxy containing hydroxyalkyl polysiloxane and preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Add 100g terminal hydrogen-containing polysiloxane, 11.6g hydroxyethyl acrylate (C=C:Si—H molar ratio 1.0:1.0), 111.6g toluene ( 100% of the total mass of the reaction raw materials), 0.58g hydroquinone (0.05% of hydroxyethyl acrylate), through N 2 Replace three times, gradually heat up to 90°C, add 11.2g of 1wt% chloroplatinic acid-ethanol solution (378ppm) as a catalyst, the system heats up rapidly, after the system temperature is stable, gradually heat up to 95°C for 3 hours, and drop to At room temperature, wash with water three times to remove unreacted hydroxyethyl acrylate, after water separation, heat up toluene to reflux with water, then raise the temperature to 100°C, remove toluene under reduced pressure at -0.090MPa vacuum, cool down to room temperature, and filter to obtain terminal acyloxy Hydroxyethylpolysiloxane. The infrared spectra of hydrogen-terminated polysiloxane, hydroxyethyl acrylate and acyloxy-terminated hydroxyethyl polysiloxane are as follow...

Embodiment 2

[0048] Add 100g terminal hydrogen-containing polysiloxane, 26.0g hydroxypropyl acrylate (C=C:Si—H molar ratio 2.0:1.0), 63g xylene ( 50% of the total mass of the reaction raw materials), 0.003g hydroquinone (0.01% of hydroxyethyl acrylate), through N 2 Replaced three times, gradually warming up to 90°C, adding 0.334g of 1wt% chloroplatinic acid-isopropanol solution (10ppm), the system heated up rapidly, after the system temperature was stabilized, gradually warming up to 145°C for 5 hours, after the reaction was completed, it dropped to At room temperature, wash with water three times to remove excess hydroxypropyl acrylate, after separating water, raise the temperature to remove water, then raise the temperature to 100°C, remove xylene under reduced pressure at -0.090MPa vacuum, cool down to room temperature, and filter to obtain terminal acyloxyhydroxyethyl base polysiloxane. The infrared spectrum of acyloxy-terminated hydroxyethyl polysiloxane is as follows figure 2 show...

Embodiment 3

[0050] In a 250mL three-necked flask equipped with a thermometer, a stirrer and a condenser tube, add 100g of terminal hydrogen-containing polysiloxane, 26.0g of hydroxypropyl acrylate (C=C:Si—H molar ratio 2.0:1.0), 0.26g of p-phenylene Diphenol (1% of hydroxypropyl acrylate), thru N 2 Replace three times, gradually heat up to 90°C, add 33.46g of 1wt% chloroplatinic acid-isopropanol solution (1000ppm), the system heats up rapidly, after the system temperature is stable, gradually heat up to 100°C for 3 hours, and drop to At room temperature, wash with water three times to remove excess hydroxypropyl acrylate, add an appropriate amount of toluene to remove water after water separation, then raise the temperature to 100°C, remove toluene under reduced pressure at -0.090MPa vacuum, cool down to room temperature, and filter to obtain terminal acyl oxide Hydroxypropyl polysiloxane. The infrared spectrum of terminal acyloxy hydroxypropyl polysiloxane is as follows image 3 shown....

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Abstract

The invention relate to acyloxy containing hydroxyalkyl polysiloxane and a preparation method. The preparation method comprises steps as follows: hydrogen containing polysiloxane and a hydroxyalkyl acrylate or hydroxyalkyl methacrylate compound are taken as raw materials, a polymerization inhibitor is added, and a target product of acyloxy containing hydroxyalkyl polysiloxane is generated through the hydrosilylation reaction of silicon-hydrogen bonds and unsaturated double bonds under the action of a platinum catalyst at the reaction temperature of 80-145 DEG C; after the reaction, the unreacted hydroxyalkyl acrylate or hydroxyalkyl methacrylate compound is washed and removed with water, water and a solvent are removed through reduced pressure distillation, the polymerization inhibitor is removed through filtering, and the target product of acyloxy containing hydroxyalkyl polysiloxane is obtained. Acyloxy containing hydroxyalkyl polysiloxane prepared with the method contains active terminated hydroxyalkyl, and when acyloxy containing hydroxyalkyl polysiloxane is applied to preparation of high polymer materials such as modified polyacrylate and the like, the functional performance of modified siloxane-acrylate copolymers is improved.

Description

technical field [0001] The invention relates to the technical field of organosiloxane synthesis, in particular to an acyloxy hydroxyalkyl polysiloxane and a preparation method. Background technique [0002] Polysiloxane is a polymer material containing Si-O-Si bonds in its macromolecular main chain. The longer bond length and larger bond angle of the Si—O—Si bond make the macromolecular chain have excellent flexibility and gas permeability, and the high bond energy and partial ionization characteristics of the Si—O bond make it have better High temperature resistance, while the side Si—CH on the main chain of the macromolecule 3 The structure makes it have extremely low surface tension and excellent water resistance. These many excellent properties make polysiloxane alone as silicone oil, silicone resin and silicone rubber products in textiles, leather, paper, daily chemicals, automobiles, It can be used in the fields of construction, energy, electronics, medicine and aero...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38
Inventor 樊武厚黄玉华蒲宗耀韩丽娟蒲实吴晋川罗艳辉
Owner SICHUAN YIXIN TECH
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