Method for preparing annular phosphonate or annular phosphate flame retardant

A cyclic phosphate and cyclic phosphonate technology, which is applied in the manufacture of fire-retardant and flame-retardant filaments, chemical instruments and methods, compounds of elements of Group 5/15 of the periodic table, etc. The problems of volatilization of phosphorus chloride and high acid value of the final product can achieve the effect of simple operation, low acid value and good viscosity

Inactive Publication Date: 2008-07-30
NANJING NORMAL UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Method one, a solvent is used in the reaction process, which increases the production cost. The raw material adopts phosphorus trichloride, and hydrogen chloride will be produced in the reaction process, which will cause the acid value of the final product to be too high and increase the difficulty of post-processing of the product; method two, the same It will cause the acid value of the product to be too high, and adding phosphorus trichloride dropwise when the trimethylolpropane is in a molten state will cause the phosphorus trichloride to volatilize and make the reaction insufficient, resulting in the impurity of the final product

Method used

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  • Method for preparing annular phosphonate or annular phosphate flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1 In a four-necked flask equipped with a stirrer, an atmospheric distillation unit, a thermometer, and an air duct, add 62.5g of trimethylolpropane, 63g of trimethyl phosphite, and 1.8g of triethylamine, heat and pass Nitrogen, the temperature was slowly raised to 80°C, and the reaction was carried out at this temperature for 8 hours to obtain the intermediate and methanol, and the methanol was distilled off. Then add 92.5 g of dimethyl methylsulfate to the intermediate, react at 170-190°C for 26 hours, and remove excess dimethylmethylsulfate (applied mechanically) under reduced pressure to obtain a colorless, transparent, highly viscous Liquid 127.5g, yield 95.7%.

Embodiment 2

[0021] Example 2 In a four-necked flask equipped with a stirrer, an atmospheric distillation unit, a thermometer, and an air duct, add 62.5g of trimethylolpropane, 63g of trimethyl phosphite, and 1.8g of triethylamine, heat and pass Nitrogen, slowly warming up to 80 ° C, at this temperature for 6 hours to obtain intermediates and methanol, the methanol was distilled off. Then add 92.5 g of dimethyl methylsulfate to the intermediate, react at 160-180°C for 22 hours, remove excess dimethylmethylsulfate (applied) under reduced pressure, and obtain a colorless, transparent, highly viscous Liquid 123.0g, yield 92.3%.

Embodiment 3

[0022] Example 3 In a four-necked flask equipped with a stirrer, an atmospheric distillation unit, a thermometer, and an air duct, add 62.5g of trimethylolpropane, 63g of trimethyl phosphite, and 1.8g of diethylamine, heat and pass Nitrogen, slowly warming up to 60 ° C, at this temperature for 8 hours to obtain intermediates and methanol, the methanol was distilled off. Then add 92.5 g of dimethyl methylsulfate to the intermediate, react at 165-185°C for 26 hours, and remove the excess dimethylmethylsulfate (applicable) under reduced pressure to obtain a colorless, transparent, highly viscous Liquid 120.0g, yield 90.1%.

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Abstract

The invention provides a preparation method of annular phosphonate or annular organic phosphate flame retardant. The steps are that (1) trimethylolpropane and trimethyl phosphate or triethyl phosphate are taken as the material, and react to synthesize into midbody under the condition of catalyzer; (2) phosphonate or organic phosphate is added into the midbody and is heated, and then the product of annular phosphonate or annular organic phosphate flame retardant can be obtained. The phosphite ester is selected from trimethyl phosphate and triethyl phosphate. The phosphonate is selected from dimethyl-phosphine and diethyl ethyl phosphine. The organic phosphate is selected from trimethyl phosphate, triethyl phosphate, phosphate propyl, tributyl phosphate and tricresyl aromatic ester. The invention overcomes the shortcomings of the prior art, the new preparation method of annular phosphonate or annular organic phosphate flame retardant is environment-friendly, solution is not needed, and the operation is simple. The termination product has excellent color and luster, low acid value and excellent viscosity; and does not need additional decoloration.

Description

technical field [0001] The invention relates to a preparation method of a cyclic phosphonate or cyclic phosphate flame retardant. Background technique [0002] Cyclic phosphonate and cyclic phosphate are additive fabric flame retardants with excellent performance, which are mixtures containing phosphine (phosphate) ester structure. Compared with traditional fabric flame retardants, this flame retardant has high thermal stability, good hydrolytic stability, low volatility and toxicity, and small addition amount, and it has good effects on the original properties of fabrics such as strength, elastic recovery, and color fastness. etc. have little impact. The flame retardant is widely used in pure polyester, cotton, rayon and synthetic fibers. [0003] According to the information currently available, there are two synthetic methods for this substance: (1) trimethylolpropane and phosphorus trichloride react to synthesize an intermediate under the conditions of a solvent cataly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K21/12C07F9/6574D01F1/07
Inventor 杨锦飞章庚柱严慧顾慧丹
Owner NANJING NORMAL UNIVERSITY
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