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Carboxylic silicone grease compounds preparation method

A technology of silicon carboxylate and compounds, which is applied in the field of organic compound preparation, can solve problems such as difficult separation, unsatisfactory synthesis of silicon carboxylate polymers, and low product purity, and achieve simple process, easy scale production, and reduced The effect of production costs

Inactive Publication Date: 2008-09-03
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The physical properties of unsaturated silicon carboxylate and the by-product saturated silicon carboxylate are similar, the boiling point is almost the same, it is difficult to separate, and the product purity is low, which cannot meet the needs of synthetic silicon carboxylate polymer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: in the three-necked bottle of 100 milliliters, install thermometer, stirrer, add benzoic acid (0.1 mol, 12.2 gram), triethylsilane (0.1mol, 11.6g), tributylphosphine (0.001mol, 0.118 g), N,N-dimethylformamide (40 ml), then heated to 100°C with stirring. Stirring was continued at this temperature for a further 48 hours. Then it was cooled to room temperature, the solvent was distilled off, and the product was distilled under reduced pressure to obtain the product triethylsilyl benzoate with a yield of 85%.

Embodiment 2

[0019] Embodiment 2: In the three-necked bottle of 100 milliliters, install thermometer, stirrer, add benzoic acid (0.1 mol, 12.2 gram), tributylphosphine (0.002mol, 0.236g), triethylsilane (0.1mol, 11.6 g), N,N-dimethylformamide (45 ml), then heated to 120°C with stirring. Stirring was continued at this temperature for a further 24 hours. Then it was cooled to room temperature, the solvent was distilled off, and the product was distilled under reduced pressure to obtain the product triethylsilyl benzoate with a yield of 92%.

Embodiment 3

[0020] Embodiment 3: in the three-necked bottle of 100 milliliters, install thermometer, stirrer, add phenylacetic acid (0.1 mol, 13.6 gram), tri-tert-butylphosphine (0.001mol, 0.118g), tripropylsilane (0.1mol, 15.8 g), N, N-dimethylacetamide (50 ml), and then heated to 110° C. with stirring. Stirring was continued at this temperature for a further 29 hours. Then it was cooled to room temperature, the solvent was distilled off, and the product was distilled under reduced pressure to obtain the product triethylsilyl benzoate with a yield of 95%.

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PUM

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Abstract

The invention discloses a carboxylic silicon ester compound making method in the organic compound technological domain, which comprises the following steps: adding organic phosphor compound in the solvent of carboxyl acid and trialkyl silane compound; filling nitrogen in the reactor; heating to 60-130 deg.c through stirring; reacting the carboxyl acid and trialkyl silane to produce carboxylic silicon ester compound hydrogen under the catalyst of zinc and its compound; adopting unsaturated carboxylic silicon ester compound as important monomer raw material to make carboxylic silicon ester compound. The invention can be applied in the metabolic medical material as Helen paint, which forms rather smooth film to reduce shipping oil consumption.

Description

technical field [0001] The invention belongs to the technical field of organic compound preparation, in particular to a preparation method of silicon carboxylate compounds. Background of the invention [0002] Silicone carboxylate polymers are widely used in metabolizable medical materials, coatings for marine vessels, etc. As a coating for seagoing ships, due to the formation of a relatively smooth film, it can prevent seashells from being adsorbed on the ship's hull, reduce shipping fuel consumption, and reduce costs. So far, organotin compounds are mainly used to coat the surface of the hull of seagoing ships to poison the sea shellfish adsorbed on the hull of the ship. Due to the toxicity of organotin compounds, they seriously pollute the ocean and marine organisms. At the same time, through the food chain, humans also ingest a large amount of toxic and harmful organotin compounds, which seriously endanger human health. The 2009 World Ocean Convention prohibits the use...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18B01J31/24
Inventor 刘国斌
Owner FUDAN UNIV