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Bromine-containing pentaerythritol phosphoester retardant and preparation method thereof

A technology of bromopentaerythritol phosphate and pentaerythritol, which is applied in the field of bromopentaerythritol-containing phosphate flame retardant and its synthesis process, can solve the problems of low bromine content of flame retardants, great negative impact on PP mechanical properties, and large addition amount , to achieve the effect of improving moisture absorption performance, good anti-ultraviolet performance and increasing yield

Inactive Publication Date: 2010-12-22
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

See patent application 200710061446.5, it is used for flame retardant modification of polypropylene, and its addition amount needs to be about 30% to achieve the ideal flame retardant effect (UL 94V-0 level). Due to the low bromine content of the flame retardant, it can achieve ideal flame retardant The effect (UL 94V-0 grade) is added in a large amount, so the negative impact on the mechanical properties of PP is also great

Method used

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  • Bromine-containing pentaerythritol phosphoester retardant and preparation method thereof
  • Bromine-containing pentaerythritol phosphoester retardant and preparation method thereof
  • Bromine-containing pentaerythritol phosphoester retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Put pentaerythritol and phosphorus oxychloride in a molar ratio of 1:3 into a reaction vessel equipped with a stirrer and an exhaust gas absorption device, turn on the nitrogen protection, stir at 58°C for 1 hour, then raise the temperature to 103°C and reflux for 9 hours. After reaction finishes, excess phosphorus oxychloride is distilled out under reduced pressure, treats that in container without phosphorus oxychloride existence, add the N-methyl-N-propenyl morpholine quaternary ammonium ion of 100 milliliters / mole pentaerythritol in container liquid and tribromoneopentyl alcohol (the molar ratio of pentaerythritol to pentaerythritol is 1.5:1), start stirring, and heat to reflux at 80° C. for 4 hours under the protection of nitrogen. After the reaction, cool down to room temperature with water at 0°C, rinse twice with toluene, and then rinse twice with distilled water until the product has no odor of phosphorus oxychloride, toluene, etc., and dry for 2 hours to obtain...

Embodiment 2

[0026] Similar to Example 1, put pentaerythritol and phosphorus oxychloride in a molar ratio of 1:10 into a reaction vessel equipped with a stirrer and an exhaust gas absorption device, turn on nitrogen protection, stir at 62°C for 1.5 hours, and then heat up to 107°C Reflux for 11 hours. After the reaction is over, distill off excess phosphorus oxychloride under reduced pressure. After there is no liquid in the container, control the temperature of the system at 75°C, slowly add anhydrous acetonitrile that is twice the volume of the reactant in the container, and mix evenly to form a mixture. solution, distill off 3 / 4 of the volume of the solution under reduced pressure, and distill off the residual phosphorus oxychloride in the reaction vessel.

[0027] Add the N-methyl-N-propenylmorpholine quaternary ammonium salt ionic liquid of 500 milliliters / mole pentaerythritol and tribromoneopentyl alcohol (with the mol ratio of pentaerythritol being 3.0: 1) in the container, start st...

Embodiment 3

[0029] Similar to Example 1, put pentaerythritol and phosphorus oxychloride in a molar ratio of 1:7 into a reaction vessel equipped with a stirrer and a tail gas absorption device, turn on the nitrogen protection, stir at 60°C for 1.5 hours, and then heat up to 105°C Reflux for 10 hours. After the reaction is over, distill off excess phosphorus oxychloride under reduced pressure. After there is no liquid in the container, control the temperature of the system at 75°C, slowly add anhydrous acetonitrile that is 1.9 times the volume of the reactant in the container, and mix evenly to form a mixture. solution, 4 / 5 of the volume of the solution was distilled off under reduced pressure, and the residual phosphorus oxychloride in the reaction vessel was distilled off.

[0030]Add the N-methyl-N-propenylmorpholine quaternary ammonium salt ionic liquid of 300 milliliters / mole pentaerythritol and tribromoneopentyl alcohol (with the mol ratio of pentaerythritol being 1.8: 1) in the conta...

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Abstract

The invention relates to a bromine-containing pentaerythritol phosphoester fire retardant and a preparation method thereof. The bromine-containing pentaerythritol phosphoester fire retardant is pentaerythritol double-spiro phosphoryl double-tribromo neopentyl alcohol ester. The preparation method of the novel bromine-containing pentaerythritol phosphoester comprises the following steps of: 1, reacting pentaerythritol with phosphorus oxychloride to generate an intermediate pentaerythritol double-spiro double-phosphorus oxychloride; and 2, reacting the pentaerythritol double-spiro phosphorus oxychloride with tribromo neopentyl alcohol to generate the pentaerythritol double-spiro phosphoryl double-tribromo neopentyl alcohol ester, wherein in the reaction, quaternary ammonium salt cation ionic liquid serves as a solvent and a catalyst. The invention discloses a new synthesis method of the bromine-containing pentaerythritol phosphoester fire retardant. The ionic liquid serves as the solvent, so the synthesis yield is improved; and a phosphorus-bromine synergistic flame retardant technique is adopted in the design of a molecular structure, so the anti-flaming efficiency of the flame retardant for high molecular materials is improved.

Description

technical field [0001] The invention relates to a bromine-containing pentaerythritol phosphate flame retardant and a synthesis process thereof, in particular to a novel pentaerythritol phosphate flame retardant with synergistic flame retardancy of phosphorus and bromine and a preparation method thereof. Background technique [0002] After the 1950s, polymer materials developed rapidly, and the three major synthetic materials were increasingly used in various sectors of the national economy and in various fields of people's daily life, and fires caused by the ignition of these materials became more and more frequent. Therefore, since the 1960s, some industrially developed countries have begun to produce and apply flame-retardant plastics, flame-retardant rubber and flame-retardant textiles on a large scale, and through the voluntary actions of some manufacturers and special national legislation, they have generally paid attention to and increased flame-retardant materials. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/527C07F9/6574
CPCY02P20/54
Inventor 彭治汉丁文科周易王华平
Owner DONGHUA UNIV
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