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Titanate siloxane catalyst, and method for preparing Si-O-C type polyether silicone wax by using catalyst

A technology of ester siloxane and titanate, which is applied in the field of titanate siloxane catalyst and its preparation of Si-O-C polyether silicone wax, can solve the problem of strong toxicity, inapplicability and difficult separation of organotin catalysts Eliminate other problems, achieve good absorption, improve safety, and improve reaction efficiency

Active Publication Date: 2017-07-04
GUANGZHOU TINCI MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these alkyltin-based catalysts are very effective, they have a very fatal defect that the toxicity of organotin catalysts is too strong, and it is difficult to separate and remove after the reaction
Personal care products have strict requirements on toxicity, so organotin catalysts are not suitable for the synthesis of personal care products

Method used

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  • Titanate siloxane catalyst, and method for preparing Si-O-C type polyether silicone wax by using catalyst
  • Titanate siloxane catalyst, and method for preparing Si-O-C type polyether silicone wax by using catalyst
  • Titanate siloxane catalyst, and method for preparing Si-O-C type polyether silicone wax by using catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The preparation method of titanate siloxane catalyst and Si-O-C type polyether silicone wax in this embodiment, the specific preparation steps are as follows:

[0032] (1) Mix 10g of ethyl titanate, 24.7g of tetramethyldihydrodisiloxane (Ti(OCH 2 CH 3 ) 4 Medium-OCH 2 CH 3 The molar ratio of the Si-H bond in tetramethyldihydrodisiloxane is 1:1.05) and 10.4 g of isopropanol are mixed and added to a four-necked flask. Under the protection of nitrogen, react at 75 ° C for 4 h, and finally The isopropanol was distilled off under reduced pressure at ℃ to obtain the self-made titanate siloxane catalyst Ti-Si-1.

[0033] (2) In a four-necked flask equipped with a reflux condenser, a mechanical stirrer, nitrogen protection and a thermometer, add 10g of tetramethyldihydrodisiloxane (Si-H bond content is 0.15%) and 163.3g of polyether (CH 3 (OCH 2 CH 2 ) 20 OH) (the molar ratio of Si-H bond to -OH in the polyether is 1:2), stirred and heated to 60°C under the protection ...

Embodiment 2

[0035] The preparation method of the titanate siloxane catalyst and Si-O-C type polyether silicone wax of the present embodiment, the specific preparation steps are as follows:

[0036] (1) 10g of isopropyl titanate, 135.3g of terminal hydrogen-containing polydimethylsiloxane (HMe 2 SiO(Me 2 SiO) 10 SiMe 2 H; where Ti(OCH 2 CH 3 ) 4 Medium-OCH 2 CH 3 The molar ratio of the Si-H bond in the hydrogen-containing polydimethylsiloxane is 1:1.1) and 53.6g of isopropanol are mixed and added to a four-necked flask, and reacted at 75°C for 4h under the protection of nitrogen, and finally The isopropanol was distilled off under reduced pressure at 70°C to obtain the self-made titanate siloxane catalyst Ti-Si-2.

[0037] (2) In a four-necked flask equipped with a reflux condenser, a mechanical stirrer, nitrogen protection and a thermometer, add 5g of terminal hydrogen-containing polydimethylsiloxane (HMe 2 SiO(Me 2 SiO) 10 SiMe 2 H, wherein the Si-H bond content is 0.11%), 18...

Embodiment 3

[0039] The preparation method of the titanate siloxane catalyst and Si-O-C type polyether silicone wax of the present embodiment, the specific preparation steps are as follows:

[0040] (1) 10g of n-butyl titanate, 303.1g of side chain hydrogen-containing polydimethylsiloxane (Me 3 SiO(Me 2 SiO) 20 (MeHSiO) 10 SiMe 3 ; where Ti(OCH 2 CH 3 ) 4 Medium-OCH 2 CH 3 The molar ratio of the Si-H bond in the hydrogen-containing polydimethylsiloxane is 1:1.15) and 26.8 g of isopropanol are mixed and added to a four-necked flask, and reacted at 75 ° C for 4 h under the protection of nitrogen, and finally The isopropanol was distilled off under reduced pressure at 70°C to obtain the self-made titanate siloxane catalyst Ti-Si-3.

[0041] (2) In a four-necked flask equipped with a reflux condenser, a mechanical stirrer, nitrogen protection and a thermometer, add 100 g of terminal hydrogen-containing polydimethylsiloxane (HMe 2 SiO(Me 2 SiO) 40 SiMe 2 H, Si-H bond content is 0.0...

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PUM

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Abstract

The invention belongs to the field of organosilicone materials, and discloses a titanate siloxane catalyst, and a method for preparing Si-O-C type polyether silicone wax by using the catalyst. The titanate siloxane catalyst is obtained by reacting titanate with hydrogen-containing group-terminated polydimethylsiloxane at 60-80 DEG C. The method for preparing Si-O-C type polyether silicone wax by using the titanate siloxane catalyst comprises the following steps: adding hydrogen-terminated polydimethylsiloxane and polyether into a reactor, heating the hydrogen-containing group-terminated polydimethylsiloxane and polyether to 60-70 DEG C, adding the titanate siloxane catalyst, carrying out a reaction for 2-10 h, and cooling the obtained reaction product to obtain the Si-O-C type polyether silicone wax. The titanate siloxane catalyst Ti-Si obtained in the invention improves the conversion rate of the hydrogen-containing group-terminated polydimethylsiloxane and the polyether at a low dosage, avoids the toxicity brought by organotin catalysts, and improves the safety of the target product.

Description

technical field [0001] The invention belongs to the field of organosilicon materials, and in particular relates to a titanate siloxane catalyst and a method for preparing Si-O-C polyether silicone wax therefrom. Background technique [0002] At present, there are mainly two synthetic methods of polyether silicone wax, one is hydrolyzed polyether silicone wax (Si-O-C polyether silicone wax), which is mainly prepared by condensation reaction; the other is non-hydrolyzed polyether modified polyether wax. Silicone wax (Si-C type polyether silicone wax) is mainly prepared by hydrosilylation reaction. At present, domestic polyether silicone wax products are mainly non-hydrolyzable polyether silicone wax (Si-C type polyether silicone wax), among which hydrolyzed polyether silicone wax (Si-O-C type polyether silicone wax) products are relatively Less, mainly due to the low product conversion rate and high catalyst toxicity, it is difficult to meet the stringent requirements of down...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/46C08G77/08C08G77/398
CPCC08G77/08C08G77/398C08G77/46
Inventor 秦文雷秋芬
Owner GUANGZHOU TINCI MATERIALS TECH