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Aryl silicate ester flame retardant plasticizer and preparation method thereof

A technology of flame retardant plasticizer and aryl silicate, which is applied in the direction of silicon organic compounds, can solve problems such as processing problems that limit the development of polysilicon industry, unsynchronized development, waste of resources and the environment, and achieve good application prospects. Good solubility and plasticity, good thermal stability, high flame retardant effect

Inactive Publication Date: 2012-10-10
李兰敏
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the production process of polysilicon, a large amount of by-product silicon tetrachloride will inevitably be produced, and the related supporting facilities for processing silicon tetrachloride have not been developed synchronously, resulting in serious waste of resources and environmental pollution.
Therefore, the problem of dealing with the by-product silicon tetrachloride limits the development of the polysilicon industry

Method used

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  • Aryl silicate ester flame retardant plasticizer and preparation method thereof
  • Aryl silicate ester flame retardant plasticizer and preparation method thereof
  • Aryl silicate ester flame retardant plasticizer and preparation method thereof

Examples

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Comparison scheme
Effect test

preparation example 1

[0020] Preparation Example 1 In a 150ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a hydrogen chloride absorption device connected to the upper mouth of the condenser, pass nitrogen protection, add 0.1 mol of silicon tetrachloride, and start liquid at 20°C. Add 0.1 mol of benzyl alcohol under the surface, the reaction releases hydrogen chloride. After the hydrogen chloride is released, replace with a soft sealing sleeve that can be extremely flexible and expand at the upper mouth of the condenser, stir, and pour 0.3 mol of epoxy under the surface at 20°C. Ethane is cooled in an ice water bath, and the temperature is controlled at the feeding rate. After the feeding, the temperature is maintained at 20°C for 4 hours, and then the temperature is raised to 40°C for half an hour. Heat and reduce pressure to distill the excess reactants and low boiling point substances and recycle them. Filter to obtain tris(chloroethyl)benzyl sil...

preparation example 2

[0021] Preparation Example 2 In a 150ml four-neck flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a hydrogen chloride absorption device connected to the upper mouth of the condenser, pass nitrogen protection, add 0.1 mol of silicon tetrachloride, and start liquid at 20°C. Add 0.1 mol of benzyl alcohol under the surface to release hydrogen chloride. After the hydrogen chloride is released, replace with a soft sealing sleeve that can be extremely stretched and expand at the top of the condenser, stir, and add 0.4 mol of epoxy under the surface at 20°C. Propane is cooled in an ice-water bath, and the temperature is controlled by the dropping rate. After the dropping, the temperature is maintained at 20°C for 8 hours, and then the temperature is raised to 40°C for 1 hour. Heat and reduce pressure to distill out excess reactants and low boiling point substances and recycle them. Filter to obtain tris(chloropropyl)benzyl silicate. The yield is 97%,...

preparation example 3

[0022] Preparation Example 3 In a 150ml four-neck flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser, and a hydrogen chloride absorption device connected to the upper mouth of the condenser, pass nitrogen protection, add 0.1 mol of silicon tetrachloride, and start liquid at 20°C. Add 0.1 mol of benzyl alcohol under the surface to release hydrogen chloride. After the hydrogen chloride is released, add 0.4 mol of epichlorohydrin to the surface of the liquid (gradually increase the temperature as the reaction proceeds), maintain the temperature at about 90°C, and react for 8 hours After that, the excess reactants and low-boiling substances were distilled out under reduced pressure and recycled. After filtration, tris(dichloropropyl)benzyl silicate was obtained. The yield was 95%, the decomposition temperature was 264±5℃, and the flash point (Open cup) is 231±5℃, density is 1.324 (25℃), refractive index is n D 25 = 1.5125.

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Abstract

The invention relates to an aryl silicate ester flame retardant plasticizer and a preparation method thereof. The structure of the compound is expressed with a general formula shown in the specification, wherein R is phenyl, tolyl and benzyl, R' is hydrogen and methyl, and R'' is hydrogen and methyl or chloromethyl. The preparation method comprises the following steps: using nitrogen to protect, and reacting silicon tetrachloride with a hydroxyl compound with an aryl having the same molar ratio as that of the silicon tetrachloride to release hydrogen chloride, and then with alkylene oxide with a certain molar ratio to obtain a target product. The target product also can be obtained through changing the feeding sequence. The compound has the advantages of stable physical and chemical properties, high flame retardant performance, good plasticity, simple process and easiness of large-scale production.

Description

Technical field [0001] The invention relates to an aryl silicate flame-retardant plasticizer and a preparation method thereof, in particular to an aryl silicic acid prepared from silicon tetrachloride, a hydroxyl compound with an aryl group and alkylene oxide as raw materials Ester flame-retardant plasticizer and preparation method thereof. The compound is a silicone-halogen synergistic flame-retardant plasticizer and can be used as a flame-retardant plasticizer for polyvinyl chloride, polyester, polyurethane, epoxy resin, glass fiber reinforced plastic resin, coatings, etc. Background technique [0002] With the large-scale development and utilization of new energy solar energy, the use of polycrystalline silicon as a raw material for photovoltaic cells has become more and more extensive, and the amount used is increasing. my country's polycrystalline silicon industry has developed rapidly in recent years. However, a large amount of by-product silicon tetrachloride is inevitably...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/5415C07F7/06C07F7/04C08L27/06
Inventor 王彦林刁建高王乐然
Owner 李兰敏
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