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A kind of preparation method of high molecular weight mq silicone resin

A technology of MQ silicone resin and high molecular weight, applied in the field of preparation of high molecular weight MQ silicone resin, can solve the problems of data disclosure without transparency, low molecular weight of MQ silicone resin, complicated preparation process, etc., and achieve excellent spreading performance, strong Marketing value, the effect of uniform particle size

Active Publication Date: 2021-10-22
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

Although the weight-average molecular weight of MQ silicone resin can reach more than 100,000, it is necessary to prepare the polymer prepolymer components of A and B in advance, and the preparation process is complicated and the cost is high
[0009] Especially, in the field of MQ silicone resin as personal home care products and cosmetics, MQ silicone resin has been used in CN107468542A, CN108366924A, US6340466, WO97 / 17058, but the MQ silicone resin disclosed by these patents has a low molecular weight and a low film-forming property. Bad and no data on its transparency disclosed
Patent CN1914251B discloses a class of MQ-T propylsiloxane resin. Although the obtained resin has a high molecular weight, the preparation process is complicated, and xylene is used as a solvent, so it is limited in skin care products and cosmetics.

Method used

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  • A kind of preparation method of high molecular weight mq silicone resin
  • A kind of preparation method of high molecular weight mq silicone resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Keep the temperature of the system at 10°C, add 1.5mol trimethylchlorosilane and 3.5mol ethyl orthosilicate into the reaction vessel, and stir to obtain a colorless and transparent system;

[0037] (2) Maintain the reaction temperature at 10°C, within 1 hour, slowly add 1.2 mol of deionized water with a feeder at a constant speed under stirring, and continue the reaction for 30 minutes after the addition;

[0038] (3) Add 3 mol of ethanol, heat up to 70°C, react for 3 hours, and let stand to separate layers;

[0039] (4) Remove the pre-polymerized resin layer obtained from the lower layer, concentrate it at 120°C to a resin content of 60wt%, add 0.92g trifluoromethanesulfonic acid as a catalyst, stir and heat up to 100°C, react for 3h, let stand to separate layers, and remove the lower layer aqueous layer;

[0040] (5) The upper organic layer was washed with deionized water until neutral, filtered to obtain a colorless transparent liquid, concentrated at 130°C unti...

Embodiment 2

[0042] (1) Keep the temperature of the system at 10°C, add 1.5mol dimethylethylchlorosilane and 4.8mol ethyl orthosilicate into the reaction vessel, and stir to obtain a colorless and transparent system;

[0043] (2) Maintain the reaction temperature at 10°C, within 2 hours, slowly add 1.8mol deionized water with a feeder at a constant speed under stirring, and continue the reaction for 10 minutes after the addition;

[0044] (3) Add 4 mol of isopropanol, heat up to 75°C, react for 4 hours, and let stand to separate layers;

[0045] (4) Remove the pre-polymerized resin layer obtained from the lower layer, concentrate it to a resin content of 60wt% at 120°C, add 1.23g of trifluoromethanesulfonic acid as a catalyst, stir and heat up to 110°C, react for 3h, let stand to separate layers, and remove the lower layer aqueous layer;

[0046] (5) The upper organic layer is washed with deionized water to neutrality, filtered to obtain a colorless transparent liquid, concentrated to a r...

Embodiment 3

[0048] (1) Keep the temperature of the system at 5°C, add 1.5mol dimethylphenylchlorosilane and 4.2mol methyl orthosilicate into the reaction vessel, and stir to obtain a colorless and transparent system;

[0049] (2) Maintain the reaction temperature at 5°C, within 1 hour, slowly add 2.1mol deionized water with a feeder at a constant speed under stirring, and continue the reaction for 20 minutes after the addition;

[0050] (3) Add 3.7 mol of isobutanol, heat up to 70°C, react for 4 hours, and let stand to separate layers;

[0051] (4) Remove the pre-polymerized resin layer obtained from the lower layer, concentrate it to a resin content of 55 wt% at 120°C, add 6.7g of potassium hydroxide as a catalyst, stir and heat up to 100°C, react for 3h, let stand to separate layers, and remove the lower aqueous phase layer;

[0052] (5) The upper organic layer was washed with deionized water until neutral, filtered to obtain a colorless transparent liquid, concentrated at 120°C until ...

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Abstract

The invention provides a preparation method of high molecular weight MQ silicone resin. The specific steps are to pre-mix Q monomer silicate and M monomer chlorosilane, control the flow rate of adding water and maintain the reaction temperature at a low temperature of 5‑15°C in the first prepolymerization step, and then undergo the second prepolymerization step, The prepolymer is obtained, and then the catalyst is added for condensation to obtain MQ silicone resin with a weight average molecular weight > 20,000, high transparency, good molecular weight dispersion, and controllable particle size. This product has the advantages of less addition and high stability in practical applications. , fast dissolution, good dispersion, strong film-forming properties, etc., can be used in pressure-sensitive adhesives, liquid silicone rubber, electronic potting adhesives, personal care and cosmetic products and other fields.

Description

technical field [0001] The invention relates to the technical field of organic silicon resin synthesis, in particular to a preparation method and application of high molecular weight MQ silicone resin. Background technique [0002] MQ silicone resin is composed of monofunctional (M group) chain link R 3 SiO 1 / 2 and four-functional group (Q group) chain link SiO 4 / 2 Polysiloxane with special structure obtained by hydrolysis and condensation. It is generally believed that the MQ silicone resin double-layer three-dimensional structure is a compact spherical body, the center of the sphere is connected by Si-O chains, and the cage-like SiO with higher density 2 ; The spherical shell part is covered with a smaller density R 3 SiO 1 / 2 surrounded by layers. The special structure of MQ silicone resin makes it an ideal reinforcing filler for polymers in composite materials. The current research is mainly used in silicone pressure-sensitive adhesives and liquid silicone rubber. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/06C08J3/12
Inventor 张生李鹏翀叶丹
Owner 埃肯有机硅材料(中山)有限公司