Preparation method of anti-sulfur poisoning platinum complex

A complex and sulfur poisoning technology, which is applied in the direction of platinum group organic compounds, platinum organic compounds, chemical instruments and methods, etc., can solve the problems of unstable catalytic performance and easy sulfur poisoning, and achieve stable activity and long storage period , the effect of product stability

Inactive Publication Date: 2018-11-13
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved in 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 preparation method of platinum complexes resistant to sulfur poisoning

Method used

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  • Preparation method of anti-sulfur poisoning platinum complex
  • Preparation method of anti-sulfur poisoning platinum complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 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:

[0049]

[0050] The specific preparation process is as follows:

[0051]

[0052] The preparation method is as follows:

[0053] S1. Preparation of 1,3-Dithiane benzene derivative intermediate AC 12 H 15 ClS 2 (Theoretical value: C 55.42%, H5.77%), Found: C 54.96%, H 5.62%, 2.02g, 90.15wt.%, the structural formula is as follows:

[0054]

[0055] In a four-neck flask equipped with a condenser and a constant pressure funnel, add 1,3-dithiane (1.20g, 0.01mol), methylene chloride (6.72g) and N-chlorosuccinimide (1.34g) , 0.01mol) in an ice water bath, stir for 30min, then add ferric chloride (0.1460g, 0.0009mol) and styrene (1.04g, 0.01mol), and react at room temperature 25~30℃ for 15h, then add ice Water (6.72g) in the reaction system, after stirring for 30 minu...

Embodiment 2

[0065] An anti-sulfur poisoning platinum complex Pt-2, the 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:

[0066]

[0067] The preparation method is as follows:

[0068] S1. Preparation of 1,3-Dithiane benzene derivative intermediate AC 13 H 17 ClS 2 (Theoretical value: C 57.25%, H6.24%), Found: C 56.99%, H 6.42%, 2.47g, 93.69wt.%, the structural formula is as follows:

[0069]

[0070] In a four-neck flask equipped with a condenser 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, stirring for 40min, then adding ferric chloride (0.1622g, 0.001mol) and 4-methylstyrene (1.42g, 0.012mol), and reacting at room temperature 30℃ for 20h , Add ice water (10.48g) to the reaction system, stir for 50min, then add petroleum ether (39.6g) (divided into 4...

Embodiment 3

[0080] An anti-sulfur poisoning platinum complex Pt-3, the 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:

[0081]

[0082] The preparation method is as follows:

[0083] S1. Preparation of 1,3-Dithiane benzene derivative intermediates A, C 13 H 17 ClS 2 (Theoretical value: C 57.25%, H6.24%), Found: C 57.10%, H 6.20%, 2.27g, 95.36wt.%, the structural formula is as follows:

[0084]

[0085] In a four-neck flask equipped with a condenser 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, stirring for 60min, then adding ferric chloride (0.1782g, 0.0011mol) and 2-methylstyrene (1.18g, 0.012mol), and reacting at room temperature 25℃ for 24h , Add ice water (7.14g) to the reaction system, stir for 60min, then add tetrahydrofuran (33.32g) (divid...

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Abstract

The invention provides a preparation method of an anti-sulfur poisoning platinum complex. The preparation method comprises the following steps: preparing a 1,3-dithiane benzene containing derivative intermediate A, preparing an unsaturated symmetrical epithio-silane intermediate B, connecting the 1,3-dithiane benzene containing derivative intermediate A to Pt through a phase transfer substitutionbond, then firstly substituting and then chelating the unsaturated symmetrical epithio-silane intermediate B to Pt, and obtaining the anti-sulfur poisoning platinum complex. The preparation method issimple and convenient, the reaction condition is mild, the production efficiency is high, the cost is low, and the industrial production is realized. A prepared catalyst has a highly symmetric complexstructure, the anti-sulfur poisoning platinum complex is stable at the room temperature, can be stored for long and has an excellent anti-sulfur poisoning catalytic effect, the catalytic activity ismore than 92%, the curing degrees of a sulfur-containing system and a non-sulfur system are basically the same and both reach more than 90%, and the anti-sulfur poisoning platinum complex has an excellent anti-sulfur poisoning capability, and is widely applied to the hydrosilylation.

Description

Technical field [0001] The invention belongs to the technical field of platinum catalysts, and more specifically, relates to a method for preparing a platinum complex with resistance to sulfur poisoning. Background technique [0002] The hydrosilylation reaction is the most important synthesis route for silicone coupling agents and functional silicone compounds. It occupies an important position in silicone chemistry and silicone industry, such as silicone glue, LED packaging glue, and silicone pressure sensitive. Glue, anti-stick coating, silicone rubber and special silicone oil. Transition metals are commonly used as catalysts in the hydrosilylation reaction, among which platinum complexes are the most active and most widely used. [0003] Currently, platinum complexes on the market are mainly prepared by two methods, Speier catalyst and Karstedt catalyst. Speier catalyst generally combines H 2 PtCl 6 ·H 2 O is dissolved in isopropanol, tetrahydrofuran (THF) or ethanol and othe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00B01J31/22
CPCB01J31/2291B01J2231/641B01J2531/828C07F15/0086
Inventor 李鹏斌程永奇张鹏刘珠刘茜
Owner GUANGDONG UNIV OF TECH
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