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A kind of synthetic method of polysiloxane

A synthesis method and polysiloxane technology, which are applied in the field of polysiloxane synthesis, can solve problems such as unseen polysiloxane, and achieve the effects of stable storage performance, reduced sewage discharge, and shortened technological process.

Active Publication Date: 2016-01-13
埃肯有机硅材料(中山)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are no relevant documents and patents on the use of aluminum organic complexes for the synthesis of polysiloxanes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1: 49.6g (0.25mol) of phenyltrimethoxysilane, 122.2g (0.5mol) of diphenyldimethoxysilane, and 180.3g (1.5mol) of dimethyldimethoxysilane were added to a 1L three-necked flask. ), after stirring evenly, add 1.76g of aluminum acetylacetonate toluene solution with a mass fraction of 10%; after stirring and mixing, add 64.1g (3.57mol) of water dropwise within 5min, after adding water, stir and hydrolyze at room temperature for 1h, and heat to 70 ℃ reflux reaction for 4 hours; after the reaction, continue to heat, and distill off the methanol and excess water generated by the reaction under normal pressure. Under vacuum condition, keep at 110℃~120℃ for 1.5h to remove residual methanol, water and low boilers to obtain polysiloxane.

[0037] The polysiloxane obtained in Example 1 is colorless and transparent, and has a viscosity of 230 mPa·s. The sample was analyzed by Fourier transform infrared spectrometer at 1000cm -1 ~1130cm -1 There is a strong absorption peak ...

Embodiment 2

[0038] Example 2: Add 89.2g (0.45mol) of phenyltrimethoxysilane, 110.0g (0.45mol) of diphenyldimethoxysilane, and 108.2g (0.90mol) of dimethyldimethoxysilane into a 1L three-necked flask. ), after stirring evenly, add 1.54g of aluminum acetylacetonate toluene solution with a mass fraction of 10%; after stirring and mixing, add 54.7g (3.04mol) of water dropwise within 5min, after adding the water, stir and hydrolyze at room temperature for 1h, then heat up to Reflux reaction at 70°C for 4 hours; continue to heat after the reaction, and distill off the methanol and excess water generated by the reaction under normal pressure. When the temperature of the material rises above 100°C, change to vacuum distillation, and the vacuum degree is -0.075MPa Maintain 1.5h at 110°C to 120°C under absolute vacuum conditions to remove residual methanol, water and low boilers to obtain 194g of polysiloxane.

[0039] The polysiloxane obtained in Example 2 is a colorless and transparent liquid wit...

Embodiment 3

[0040] Example 3: Add 89.2g (0.45mol) of phenyltrimethoxysilane, 110.0g (0.45mol) of diphenyldimethoxysilane, and 108.2g (0.90mol) of dimethyldimethoxysilane into a 1L three-necked flask. ), after stirring evenly, add 0.15g of aluminum acetylacetonate toluene solution with a mass fraction of 10%; after stirring and mixing, add 54.7g (3.04mol) of water dropwise within 5min; Reflux reaction at 70°C for 4 hours, continue heating after the reaction, and distill off the methanol and excess water generated by the reaction under normal pressure, and change to vacuum distillation when the temperature of the material rises above 80°C, and the vacuum degree is -0.075MPa Maintain at 80°C to 90°C for 1.5h under absolute vacuum conditions to remove residual methanol, water and low boilers to obtain polysiloxane.

[0041] The polysiloxane obtained in Example 3 was a colorless and transparent liquid with a viscosity of 570 mPa·s. The sample was analyzed by Fourier transform infrared spectro...

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Abstract

The invention discloses a method for synthesizing polysiloxane. The method comprises the following steps and process conditions: adding at least one kind of siloxane to a reactor; uniformly stirring, and then adding organic aluminum complexes which account for 0.0001%-5% of the total weight of the siloxane as catalysts; uniformly stirring and mixing, and then dropping water which is 0.0001-10.0 times more than the quantity of alkoxy substances added to the siloxane; after the water is dropped, heating for reflux reaction, then continuously heating, and distilling alcohols generated in the reflux reaction and redundant water at ordinary pressure; when the temperature of materials is increased to more than 100 DEG C, carrying out reduced pressure distillation to remove residual alcohols, water and low-boiling-point substances so as to obtain the polysiloxane. The method disclosed by the invention is environmental-friendly, reduces the pollution, reduces the cost, is greatly shortened in process flow and increases the production efficiency; a polysiloxane product is stable in storage performance.

Description

【Technical field】 [0001] The invention relates to a method for synthesizing polysiloxane, which belongs to the technical field of organic polymer materials. 【Background technique】 [0002] Polysiloxane is a kind of polymer with repeated silicon-oxygen-silicon bonds as the main chain, and organic groups are directly connected to silicon atoms. Its general structure is expressed as follows: [0003] [R n SiO (4-n) / 2 ] m [0004] In the formula, R is an organic group, such as methyl, phenyl, etc.; n is the number of organic groups connected to the silicon atom, ranging from 1 to 3; m is the degree of polymerization, and the range is m≥2. R in polysiloxane is mostly methyl and phenyl, because the siloxane monomer raw materials of methyl and phenyl are cheap and easy to get, and have good versatility. [0005] The structure of polysiloxane is relatively complex. According to the different synthetic raw material monomers, it can contain monofunctional chain segments, bifuncti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/08C08G77/18
Inventor 马汉喜吴超马汉永
Owner 埃肯有机硅材料(中山)有限公司