Anti-sulfur poisoning platinum catalyst and preparation method thereof

A platinum catalyst, platinum catalyst technology, applied in the field of anti-sulfur poisoning platinum catalyst and its preparation, can solve the problems of platinum catalyst poisoning, loss of catalytic activity, etc.

Active Publication Date: 2021-01-26
SHENZHEN ANPIN SILICONE MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the preparation process of high refractive index sulfur-containing polysiloxane resin, synthesis by hydrosilylation reaction is a common synthesis method. Since the synthetic raw materials include sulfur-containing monomers, it is easy to cause the platinum catalyst commonly used in hydrosilylation reaction Poisoning, loss of catalytic activity, currently there is no platinum catalyst product with good anti-poisoning effect on the market, which needs to be developed urgently

Method used

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  • Anti-sulfur poisoning platinum catalyst and preparation method thereof
  • Anti-sulfur poisoning platinum catalyst and preparation method thereof
  • Anti-sulfur poisoning platinum catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] The preparation method of anti-poisoning platinum catalyst (Pt-1) comprises the following steps:

[0052] A, get nano-graphite (1.00g, average particle diameter 30nm, manufacturer is Kramer's reagent) ultrasonic dispersion in 75g toluene and 25g ethanol, then add 3.00g 3-aminopropyltriethoxysilane (APTS) ( 0.0135mol), stirred for 10min, slowly heated to 90°C, added 1.00g trifluoromethanesulfonic acid and 0.36g water (0.02mol), stirred and reacted at 90°C for 48h, then washed with 100g water, 75g toluene and 25g ethanol in sequence, pumped After filtration, vacuum-dry at 100°C for 24 hours, and grind to obtain modified nano-graphite;

[0053] B. Add 75.08g benzene, 37.54g ethanol, 30.45g 2,5-dihydroxy-1,4-dithiane to a four-neck flask with condenser, nitrogen inlet and constant pressure funnel (0.2mol) and 44.63g cis-dichlorobis(diethylsulfide) platinum (II) (0.1mol), stirred for 20min, added 0.75g dichloroacetic acid (0.0058mol) and 0.75g concentrated sulfuric acid (m...

Embodiment 2

[0056] The preparation method of anti-poisoning platinum catalyst (Pt-2) comprises the following steps:

[0057] A, get 3.00g nano white carbon black (average particle diameter is 12nm, manufacturer is Cabot) ultrasonic dispersion in the mixed solvent of 80g xylene and 20g isopropanol, then add 5.00g N-aminoethyl-3 - Aminopropylmethyldimethoxysilane (0.024mol) was stirred for 20min, slowly heated to 100°C, 2g of trifluoromethanesulfonic acid and 0.52g of distilled water (0.03mol) were added, stirred at 100°C for 36h, and then 100g of Wash with water, 80g xylene and 20g isopropanol, suction filter, then vacuum dry at 100°C for 20h, and grind to obtain modified nano activated carbon;

[0058] B. Add 168.59g of petroleum ether, 59.01g of isopropanol, and 40.65g of 4-(1,3-dithiolane)phenol into a four-neck flask with a condenser, nitrogen inlet and constant pressure funnel (0.205mol) and 44.63g trans-dichlorobis(diethylsulfide) platinum (II) (0.1mol), stirred for 30min, added 1....

Embodiment 3

[0061] The preparation method of anti-poisoning platinum catalyst (Pt-3) comprises the following steps:

[0062] A. Take 5.00g nanometer SiC (the average particle size is 50nm, the manufacturer is Shanghai Yaotian New Material Co., Ltd.) and ultrasonically disperse it in a mixed solvent of 82.00g cyclohexane and 18.00g tetrahydrofuran, and then add 8.00g p-aminophenyl Trimethoxysilane (0.0375mol), stirred for 30min, slowly heated to 110°C, added 2.00g of strongly acidic cationic resin and 1.62g of distilled water (0.09mol), stirred and reacted at 110°C for 24h, then successively added 100g of water, 82.00g of cyclohexane alkane and 18.00g tetrahydrofuran, and then vacuum-dried at 100°C for 12 hours, and ground to obtain modified nano-SiC;

[0063] B. Add 215.65g cyclohexane, 71.88g acetone, 28.61g 1,3-dithiapentane-2-ylmethanol in a four-neck flask with a condenser, nitrogen inlet and constant pressure funnel (0.21mol) and 44.63g cis-dichlorobis(diethylsulfide) platinum (II)...

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Abstract

The invention discloses an anti-sulfur-poisoning platinum catalyst and a preparation method thereof, the preparation method comprises the following steps: A, a carrier material is dispersed into a 0#solvent, amino alkoxyl silane is added for mixing, an acid catalyst and water are added, and the mixture is in reaction to obtain a modified carrier material; B, the solvent, epithio-heterocyclic monomers and modified platinum dichloride (II) are mixed and stirred, an acid stabilizer and an acid catalyst are added, and water is added dropwise for reaction to obtain a modified platinum catalyst; C,under the condition that the inert gas is fed, the solvent, the modified carrier material and a modified platinum catalyst solution are mixed, warming reaction is conducted, reaction is performed under the vacuumizing condition, then the temperature is reduced to 0 DEG C sharply and standing is performed, and the anti-sulfur-poisoning platinum catalyst is obtained after separation. According to the platinum catalyst, the catalytic activity and the stability are improved remarkably, the poisoning effect is reduced greatly when the platinum catalyst is used in synthesis of sulfur-containing silicone oil and silicon resin, and the anti-poisoning effect is remarkable.

Description

technical field [0001] The invention belongs to the technical field of organosilicon materials, and relates to a sulfur poisoning-resistant platinum catalyst and a preparation method thereof. [0002] technical background [0003] Introducing sulfur-containing groups into the molecular structure of polysiloxane resin is one of the effective ways to synthesize high-refractive-index sulfur-containing polysiloxane, and then can prepare high-refractive-index optical materials. At present, the application prospects of optical materials are increasing. The wider the range, the higher the requirements for the corresponding high refractive index resin materials. [0004] In the preparation process of high refractive index sulfur-containing polysiloxane resin, synthesis by hydrosilylation reaction is a common synthesis method. Since the synthetic raw materials include sulfur-containing monomers, it is easy to cause the platinum catalyst commonly used in hydrosilylation reaction Poiso...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/08C08G77/28
CPCC08G77/08C08G77/28
Inventor 刘珠祝琳丁小卫
Owner SHENZHEN ANPIN SILICONE MATERIAL
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