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Method for preparing tris(1,3-dichloropropyl) phosphate

A technology of dichloropropyl and dichloropropanol is applied in the field of preparing phosphoric acid triester, which can solve the problems of complex preparation process, difficult catalyst handling and high cost, achieve high reactivity, improve raw material conversion rate, and mild process conditions. Effect

Active Publication Date: 2019-03-08
山东泰和科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the problems of the above-mentioned method for preparing tris(1,3-dichloropropyl)phosphate with complex preparation process, high cost, low yield and difficult catalyst handling, the present invention provides a method for preparing tris(1,3-dichloropropyl)phosphate Chloropropyl) ester method

Method used

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  • Method for preparing tris(1,3-dichloropropyl) phosphate

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Experimental program
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Effect test

Embodiment 1

[0021] At room temperature, add 153g of phosphorus oxychloride and 774g of 1,3-dichloropropanol (molar ratio: 1:6) into the reaction kettle, stir and raise the temperature to 115°C. After reacting at this temperature for 1 hour, under negative pressure Remove the hydrogen chloride gas generated by the reaction to the hydrogen chloride absorption device under the condition of -0.002MPa, and at the same time, the temperature is gradually increased to 180°C at a rate of 15°C / h, and the reaction is continued for 1 hour. The crude product after cooling is alkali washed, washed with water, and distilled to obtain triphosphate The (1,3-dichloropropyl) ester has a purity of 98.87% and a yield of 85.79%. The 1,3-dichloropropanol recovered by distillation is recycled as the reaction raw material.

Embodiment 2

[0023] At room temperature, 153g of phosphorus oxychloride and 903g of 1,3-dichloropropanol (molar ratio: 1:7) were added to the reaction kettle and stirred and heated to 110°C. After reacting at this temperature for 1.5 hours, it was heated under negative pressure. Remove the hydrogen chloride gas generated by the reaction to the hydrogen chloride absorption device under the condition of -0.003MPa, and at the same time, the temperature is gradually increased to 180°C at a rate of 20°C / h, and the reaction is continued for 2 hours. The crude product after cooling is alkali washed, washed with water, and distilled to obtain triphosphate The (1,3-dichloropropyl) ester has a purity of 99.01% and a yield of 87.42%. The 1,3-dichloropropanol recovered by distillation is recycled as the reaction raw material.

Embodiment 3

[0025] At room temperature, add 153 g of phosphorus oxychloride and 645 g of 1,3-dichloropropanol (molar ratio: 1:5) into the reaction kettle, stir and raise the temperature to 120°C. After reacting at this temperature for 1 hour, under negative pressure Remove the hydrogen chloride gas generated by the reaction to the hydrogen chloride absorption device under the condition of -0.003MPa, and at the same time, the temperature is gradually increased to 180°C at a rate of 30°C / h, and the reaction is continued for 2 hours. The crude product after cooling is alkali washed, washed with water, and distilled to obtain triphosphate The (1,3-dichloropropyl) ester has a purity of 98.77% and a yield of 86.83%. The 1,3-dichloropropanol recovered by distillation is recycled as the reaction raw material.

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Abstract

The invention discloses a method for preparing tris(1,3-dichloropropyl) phosphate. The method specifically comprises the following steps: adding phosphorus oxychloride and 1,3-dichloropropanol into areaction kettle at a time, stirring the phosphorus oxychloride and the 1,3-dichloropropanol, raising the temperature to 110 DEG, performing a reaction on the phosphorus oxychloride and the 1,3-dichloropropanol for 1-3h, raising the temperature to 180 DEG according to the 15-30-DEG C gradient, removing generated hydrogen chloride gas under a negative pressure condition and reducing the temperature,so as to obtain a crude product; washing the crude product with alkali and water in sequence and distilling, so as to obtain the tris(1,3-dichloropropyl) phosphate. Under a catalyst-free condition, the method has the advantages of being high in product purity, high in conversion rate, mild in process conditions, and simple in operation, avoiding a problem of aftertreatment of a catalyst and lowering the production cost.

Description

Technical field [0001] The invention belongs to the field of chemical synthesis, and specifically relates to a method for preparing tris(1,3-dichloropropyl) phosphate. Background technique [0002] Tris (1,3-dichloropropyl) phosphate as a good flame retardant and flame retardant plasticizer is widely used in unsaturated polyester, rigid and flexible polyurethane foam, epoxy resin, phenolic resin , Soft PVC, etc. [0003] The synthesis of tris(1,3-dichloropropyl) phosphate at home and abroad is mainly based on the study of the reaction of epichlorohydrin and phosphorus oxychloride under different catalysts. The Stauffer Chemical Company of the United States and the Daihachi Chemical Company of Japan have already produced them. In recent years, many scholars in my country have conducted research on the synthesis of tris(1,3-dichloro-2-propyl) phosphate. The Chinese patents with publication numbers CN102863468A, CN107556338A, and CN102807581B respectively introduced the use of epich...

Claims

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Application Information

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IPC IPC(8): C07F9/09
CPCC07F9/091
Inventor 周荣奇程终发陆久田赵坤王宁宁齐晓婧
Owner 山东泰和科技股份有限公司
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