Method for using load type platinum catalyst for preparing perfluoroalkyl group ethyl silane and method for preparing load type platinum catalyst

A technology of perfluoroalkylethylsilane and perfluoroalkylethylene is applied in the field of preparing the supported platinum catalyst, which can solve the problems that the catalyst cannot be reused and the reaction yield is high, and achieve good waterproofness, high reaction yield, cost reduction effect

Inactive Publication Date: 2016-01-06
QUZHOU FLUORIDE & SILICON RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method has the following advantages: (1) overcomes the defect that the previous hydrosilylation requires high temperature and high pressure harsh conditions, the reaction can be carried out under relatively mild conditions, and the operation is safe; (2) the reaction yield is high; (3) It overcomes the defect that previous catalysts cannot be reused, and the supported platinum catalyst can be reused more than five times without a significant decrease in yield; (4) The reuse of the catalyst greatly reduces the cost and reduces environmental pollution at the same time

Method used

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  • Method for using load type platinum catalyst for preparing perfluoroalkyl group ethyl silane and method for preparing load type platinum catalyst
  • Method for using load type platinum catalyst for preparing perfluoroalkyl group ethyl silane and method for preparing load type platinum catalyst
  • Method for using load type platinum catalyst for preparing perfluoroalkyl group ethyl silane and method for preparing load type platinum catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Add 446g of heptadecafluorooctylethylene in a 1L three-necked flask, and then add 1.2g (10ppm) of silica gel-supported platinum catalyst. The platinum loading in the silica gel-supported platinum catalyst is 0.5%. 135g of trichlorosilane was added dropwise for 1 hour, then stored at temperature for 5 hours, filtered to obtain a filter residue as a supported platinum catalyst after the reaction was completed, and finally the crude product filtrate was subjected to rectification treatment, and finally 523g of the product perfluorodecyltrichlorosilane was obtained, Yield 96.5%.

Embodiment 2～15

[0056] Using the same synthesis steps as in Example 1, see Table 1 for the specific formula, and see Table 2 for the specific process conditions and product yield.

[0057] Table 1

[0058]

[0059]

[0060] Table 2

[0061] project

Reaction temperature (°C)

Reaction time (h)

yield

[0062] Example 2

75

5

97.1％

Example 3

85

5

97.3％

Example 4

95

5

97.3％

Example 5

110

5

97.1％

Example 6

120

5

97.6％

Example 7

85

1

97.9％

Example 8

85

3

98.3％

Example 9

85

4

97.3％

Example 10

85

6

98.1％

Example 11

85

8

98.6％

Example 12

90

5

98.3％

Example 13

85

6

98.3％

Example 14

100

5

98.5％

Example 15

85

6

97.2％

[0063] According to the same formulation and process conditions as in Examples 1, 4...

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PUM

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Abstract

The invention discloses a method for using a load type platinum catalyst for preparing perfluoroalkyl group ethyl silane and a method for preparing the load type platinum catalyst. The method for preparing perfluoroalkyl groups comprises the following steps that 1, perfluoroalkyl group ethyl and the catalyst are added into a reaction flask at first and stirred uniformly; 2, chloride silane is dripped continuously, and dripping time is controlled to be 0.5-1 h; 3, after feeding is finished, reaction temperature is controlled, and reaction time is 1-8 h; 4, after reaction is finished, cooling is carried out to reach room temperature, and filtering is carried out to obtain load type platinum catalyst filter residues; 5, coarse product filter liquor is rectified to obtain perfluoroalkyl group ethyl silane. The method for preparing the load type platinum catalyst comprises the steps that chloroplatinic acid is thrown into a reaction flask at first and dissolved into solvent, a carrier is added, and after standing for 24 h, the mixture is dried at the temperature of 120 DEG C to obtain the load type platinum catalyst finally. The preparing method overcomes the defect that in the past, hydrosilylation demands severe high-temperature and high-pressure conditions, the reaction can be carried out under the mild condition, and operation is safe.

Description

technical field [0001] The invention relates to a method for preparing perfluoroalkylethylsilane with a supported platinum catalyst and a method for preparing the supported platinum catalyst. Background technique [0002] Perfluoroalkylfluorosilane has good water, oil, and anti-fouling properties, and is widely used in the glass industry, automotive industry, electronics, and special surface coating treatment fields. It has good anti-fingerprint, anti-fouling, and anti-fog properties. At present, the commonly used waterproofing agents are mainly water-based crystalline osmotic waterproofing agents and silicone waterproofing agents. Water-based crystalline waterproofing agents are expensive, while silicone waterproofing agents cannot meet the needs of projects because of their permeability and ability to block larger pores. . Perfluoroalkylfluorosilane contains both fluorine and silicon. It combines the properties of organic fluorine and silicone. It has the characteristics ...

Claims

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Application Information

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IPC IPC(8): C07F7/08B01J23/42
Inventor 杨建荣刘坤李建向德轩周强
Owner QUZHOU FLUORIDE & SILICON RES INST
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