Photocurable liquid silicone rubber catalyst with high dispersibility, and preparation method thereof

A liquid silicone rubber, high dispersion technology, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of large consumption and poor catalyst dispersion , to achieve the effect of reducing consumption, good dispersion, convenient and effective recycling

Active Publication Date: 2019-09-20
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a photocurable liquid silicone rubber catalyst with high dispersibility and its prepar...

Method used

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  • Photocurable liquid silicone rubber catalyst with high dispersibility, and preparation method thereof
  • Photocurable liquid silicone rubber catalyst with high dispersibility, and preparation method thereof
  • Photocurable liquid silicone rubber catalyst with high dispersibility, and preparation method thereof

Examples

Experimental program
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Effect test

preparation example Construction

[0025] Such as figure 1 Shown, the preparation method of this catalyst comprises:

[0026] S1 uses chloroplatinic acid as a platinum source and reacts with a strong base at a temperature of 80-100°C (Celsius) to obtain a hexahydroxyplatinic acid metal salt; the strong base is NaOH, KOH or LiOH.

[0027] S2: Reducing tetravalent platinum in hexahydroxyplatinic acid metal salt to divalent platinum, and coordinating with silane-functionalized acetylacetone, stirring and refluxing for 3-12 hours (hours) to suspend solid powder in the solution. Specifically, the silane functionalization of acetylacetone is achieved by combining with alkylsilane after deprotonation of sodium cyanide or methyllithium, and the acetylacetone ligand for silane functionalization is (3-methyldimethoxysilyl) acetylacetone , (3-methyldimethoxysilyl) 1-phenyl-1,3-butanedione, (3-methyldimethoxysilyl) 1,3-diphenyl-1,3- Any one of propylenedione, (3-methyldimethoxysilyl)1,1,1,5,5,5-hexafluoro-2,4-pentanedion...

Embodiment 1

[0029] Example 1: Synthesis of two [(3-methyldimethoxysilyl) acetylacetonate] platinum (II)

[0030] Take 6.0g (gram) H 2 PtCl 6 ·6H 2 O was put into a 100mL (milliliter) single-necked bottle, and 40mL of water was added to dissolve it into a reddish-brown color. After that, 15.6g of NaOH was added, and heated to 110°C for 3h under reflux. In the process of reflux, the solution starts to be yellow, and after half an hour of reaction, the color becomes lighter and gradually becomes transparent and clear; after 1 hour of reaction, yellow suspended powder appears; after 3 hours, the reaction is stopped, and a large amount of yellow powder is precipitated after being cooled in the refrigerator overnight. Sodium hydroxyplatinate (Na 2 Pt(OH) 6). Afterwards, the supernatant was poured out, methanol was added to wash the yellow powder three times, filtered with suction, dried and weighed to obtain 3.8 g of the yellow powder. In this process, the yield reached 95.47%.

[0031] ...

Embodiment 2

[0033] Example 2: Synthesis of two [(3-methyldimethoxysilyl) 1-phenyl-1,3-butanedione] platinum (II)

[0034] Weigh 2.5g of prepared Na 2 Pt(OH) 6 (See Example 1) Place in a three-necked flask, add 20mL of water and shake well, then add 4.86g of (3-methyldimethoxysilyl) 1-phenyl-1,3-butanedione and 200uL of Concentrated sulfuric acid was heated to reflux at 85°C to obtain a milky white turbid solution (mixed solution); after that, dilute 400uL HCOOH in 500mL water, and drop the diluted HCOOH into the mixed solution through a constant pressure dropping funnel. Reaction 3h, in this process, solution becomes black or dark green when reaction 1h, upper layer floats a small amount of yellow powder; Then react overnight, stop reaction and filter to obtain light green powder, i.e. bis[(3-methyldimethoxy silyl) 1-phenyl-1,3-butanedione] platinum (II).

[0035] After weighing, the light green powder was 5.32g, and the yield was 75.20%. ICP analysis of this light green powder reveal...

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Abstract

The invention discloses a photocurable liquid silicone rubber catalyst with a high dispersibility, and a preparation method thereof. The preparation method of the catalyst comprises the following steps: S1, reacting chloroplatinic acid, used as a platinum source, with a strong alkali at a temperature of 80-100 DEG C to obtain a metal hexahydroxyplatinate; S2, reducing tetravalent platinum in the metal hexahydroxyplatinate into divalent platinum, coordinating the divalent platinum with silane-functionalized acetylacetone, performing stirring and refluxing for 3-12 h to suspend solid powder in a solution; and S3, filtering the solid powder suspended in the solution, washes the solid powder with water multiple times, and drying the solid powder at a temperature of 50-70 DEG C to obtain the catalyst for photocuring. The problems of poor dispersibility in a silicone matrix and high consumption of existing catalysts are effectively solved.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a light-curing liquid silicone rubber catalyst and a preparation method thereof. Background technique [0002] With the development of silicone rubber, addition-type liquid silicone rubber products are widely used in food, electronic and electrical components, construction, medical, automobile, aerospace and other fields due to their unique properties. In the process of preparing addition-type silicone rubber materials, silicone rubber catalysts play an important role. At present, silicone rubber catalysts are mainly platinum complexes, which are activated by heat to produce catalytic effects, and are used for cross-linking and curing of silicon components to form silicone rubber. This curing method is called thermal curing. Thermal curing essentially causes the silicon component to undergo a hydrosilylation reaction, that is, the C=C bond and the Si-H bond are heated under th...

Claims

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Application Information

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IPC IPC(8): C08L83/07C08L83/05C08K5/00C08J3/28G01N33/44
CPCC08J3/28B01J31/2213G01N33/445C08J2383/07C08J2483/05C08K5/0091B01J2531/828B01J2531/0238B01J2231/323
Inventor 陈超付林杰陈祥斌赵丹丁顺民
Owner NANCHANG UNIV
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