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Platinum complex resistant to sulfur poisoning and applications thereof

A complex and sulfur poisoning technology, applied in the direction of platinum group organic compounds, platinum group organic compounds, compounds of elements of Group 4/14 of the periodic table, etc., can solve the problems of easy sulfur poisoning, unstable catalytic performance, etc. The effect of long storage period, stable catalyst activity and high production efficiency

Active Publication Date: 2018-09-11
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the defects and deficiencies of existing platinum catalysts, which are prone to sulfur poisoning and unstable catalytic performance, and provide a platinum complex resistant to sulfur poisoning

Method used

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  • Platinum complex resistant to sulfur poisoning and applications thereof
  • Platinum complex resistant to sulfur poisoning and applications thereof
  • Platinum complex resistant to sulfur poisoning and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] An anti-sulfur poisoning platinum complex Pt-1, the chemical formula is: C 34 h 50 Si 2 S 8 PtO 2 (Theoretical value: C 40.92%, H5.01%, O 3.21%), Found: C 41.06%, H 4.86%, O 3.54%, its structural formula is as follows:

[0073]

[0074] Concrete preparation process is as follows:

[0075]

[0076] Its preparation method is as follows:

[0077] S1. Preparation of intermediate AC of 1,3-dithiane-containing benzene derivatives 12 h 15 CLS 2 (Theoretical value: C 55.42%, H5.77%), Found: C 54.96%, H 5.62%, 2.02g, 90.15wt.%, structural formula is as follows:

[0078]

[0079] In a four-neck flask equipped with a condenser tube and a constant pressure funnel, add 1,3-dithiane (1.20g, 0.01mol), dichloromethane (6.72g) and N-chlorosuccinimide (1.34g , 0.01mol) in an ice-water bath, stirred for 30min, then added ferric chloride (0.1460g, 0.0009mol) and styrene (1.04g, 0.01mol), and reacted at room temperature for 15h at 25-30°C, then added ice Water (6.72g) was...

Embodiment 2

[0089] A kind of anti-sulfur poisoning platinum complex Pt-2, chemical formula is: C 44 h 54 Si 2 S 8 PtO 2 (Theoretical value: C 47.10%, H4.82%, O 2.85%), Found: C 47.06%, H 4.36%, O 2.84%, 0.63g, 95.58wt.%, its structural formula is as follows:

[0090]

[0091] Its preparation method is as follows:

[0092] S1. Preparation of intermediate AC of 1,3-dithiane-containing benzene derivatives 13 h 17 CLS 2 (Theoretical value: C 57.25%, H6.24%), Found: C 56.99%, H 6.42%, 2.47g, 93.69wt.%, structural formula is as follows:

[0093]

[0094] In a four-necked flask equipped with a condenser tube and a constant pressure funnel, add 1,3-dithiane (1.20g, 0.01mol), dichloroethane (10.48g) and N-chlorosuccinimide (1.47 g, 0.011mol) in an ice-water bath, stirred for 40min, then added ferric chloride (0.1622g, 0.001mol) and 4-methylstyrene (1.42g, 0.012mol), and reacted at room temperature for 20h at 30°C , add ice water (10.48g) in the reaction system, after stirring for 50...

Embodiment 3

[0104] A kind of anti-sulfur poisoning platinum complex Pt-3, chemical formula is: C 52 h 58 Si 2 S 8 PtO 2 (Theoretical value: C 51.10%, H4.75%, O 2.62%), Found: C 51.01%, H 4.16%, O 2.87%, 0.70g, 97.36wt.%, its structural formula is as follows:

[0105]

[0106] Its preparation method is as follows:

[0107] S1. Preparation of intermediates A and C of 1,3-dithiane-containing benzene derivatives 13 h 17 CLS 2 (Theoretical value: C 57.25%, H6.24%), Found: C 57.10%, H 6.20%, 2.27g, 95.36wt.%, structural formula is as follows:

[0108]

[0109] In a four-neck flask equipped with a condenser tube and a constant pressure funnel, add 1,3-dithiane (1.20g, 0.01mol), carbon tetrachloride (11.9g) and N-chlorosuccinimide (1.61 g, 0.012mol) in an ice-water bath, stirred for 60min, then added ferric chloride (0.1782g, 0.0011mol) and 2-methylstyrene (1.18g, 0.012mol), and reacted at room temperature for 24h at 25°C , add ice water (7.14g) to the reaction system, stir for 60m...

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Abstract

The invention discloses a platinum complex resistant to sulfur poisoning and applications thereof. The platinum complex has a complexing symmetric structure, which comprises a 1,3-dithiane benzene containing derivative group and symmetric unsaturated epithio-silane; wherein the 1,3-dithiane benzene containing derivative group comprises a benzene ring and a symmetric epithio- six-membered ring. ThePt catalyst has a highly symmetrical complexing structure and a very good effect on resisting sulfur poisoning. The catalytic activity is 92% or more. The catalytic effect in a sulfur system is basically the same as that in a non-sulfur system. The Pt catalyst has a good performing on resisting sulfur poisoning, is very stable at a room temperature, and can be stored for a long term. Solved are the problems that in the prior art, the storage time of a conventional Pt catalyst is short, the conventional Pt catalyst should be strictly sealed, and the catalytic activity of the Pt catalyst is lost after the Pt catalyst is poisoned by sulfur containing compounds. The Pt catalyst can be widely used in silicon-hydrogen addition reactions.

Description

technical field [0001] The invention belongs to the technical field of platinum catalysts, and more specifically relates to a sulfur-poisoning-resistant platinum-gold complex and an application thereof. Background technique [0002] The hydrosilylation reaction is the most important synthesis route for organosilicon coupling agents and functionalized organosilicon compounds. Rubber, anti-stick coating, silicone rubber and special silicone oil and other fields. Transition metals are commonly used as catalysts for hydrosilylation reactions, among which platinum-gold complexes are the most active and widely used. [0003] At present, platinum complexes on the market are mainly prepared by Speier catalyst and Karstedt catalyst. Speier catalysts are generally H 2 PtCl 6 ·H 2 O is dissolved in solvents such as isopropanol, tetrahydrofuran (THF) or ethanol, and the water of crystallization is removed to obtain a Pt complex. Karstedt catalyst refers to the Pt complex formed by...

Claims

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Application Information

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IPC IPC(8): C07F15/00B01J31/22C07F7/18
CPCB01J31/2208B01J31/2291B01J2231/645B01J2531/828C07F7/1876C07F15/0086
Inventor 李鹏斌程永奇张鹏刘珠刘峰
Owner GUANGDONG UNIV OF TECH
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