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Preparation method of bisphenol-A-bis(diphenyl phosphate) flame retardant

A technology of diphenyl phosphate and flame retardant, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as poor catalysts, and achieve less side reactions, The effect of high content and high yield

Active Publication Date: 2019-06-21
NANTONG JIANGSHAN AGROCHEM & CHEM LIMITED LIABILITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Purpose of the invention: In order to overcome the problem of poor catalysts in the prior art, a new catalyst is provided to synthesize bisphenol A-bis(diphenyl phosphate). This method has simple process, high content and high yield, and does not need to add mixed Solvent for pickling, alkali washing and water washing, excellent environmental performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The content of 99.3% POCl 3 225.39g, SO 4 2- / Fe 2 o 4 -Al 2 o 3 Put 0.03g of catalyst into the reaction bottle, raise the temperature to about 80°C, and put 75g of 99% bisphenol A in sealed batches (about 3h), the pressure is 0.04MPa, after feeding, raise the temperature to 90-95°C for 3.5h, and the reaction is over Distill the excess POCl3, then add 120 g of 99% phenol dropwise (add 130°C after melting), drop it for about 3 hours, keep it at 160°C for 3.5 hours, until no hydrogen chloride is released, after the heat preservation is completed, remove the hydrogen chloride in a vacuum, and the excess phenol is obtained Qualified BDP with a monomer content of 90.45% was 215.48 g.

Embodiment 2

[0031] The content of 99.3% POCl 3 676.17g, SO 4 2- / TiO 2 Put 0.1g of catalyst into the reaction bottle, raise the temperature to about 80°C, seal and put in 225 g of 99% bisphenol A in batches (about 3h), the pressure is 0.04MPa, after feeding, raise the temperature to 90-95°C for 3.5h, and the reaction is over Distill excess POCl 3 , then add 360 g of 99% phenol dropwise (add 130°C after melting), drop it for about 3 hours, keep warm at 160°C for 3.5 hours, until no hydrogen chloride is released, after the heat preservation is completed, hydrogen chloride is removed in vacuum, and excess phenol is obtained to obtain a qualified monomer BDP706.44 g with a content of 91.25%.

Embodiment 3

[0033] The content of 99.3% POCl 3 750.4g, SO 4 2- / WO 3 -ZrO 2 Put 0.2g of catalyst into the reaction bottle, raise the temperature to about 80°C, and put 225 g of 99% bisphenol A in sealed batches (about 4h), the pressure is 0.04MPa, after feeding, raise the temperature to 90-95°C for 3.5h, the reaction is over Distill excess POCl 3 , then add 360 g of 99% phenol dropwise (add 130°C after melting), drop it for about 3 hours, keep it warm at 150°C for 3.5 hours, until no hydrogen chloride is released, after the heat preservation is over, remove the hydrogen chloride in a vacuum, and the excess phenol gets qualified monomer BDP640.75 g with a content of 89.45%.

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PUM

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Abstract

The invention discloses a preparation method of a bisphenol-A-bis(diphenyl phosphate) flame retardant. Firstly, bisphenol A reacts with excessive phosphoryl chloride, then, excessive phosphoryl chloride is removed, an obtained product reacts with phenol, and the bisphenol-A-bis(diphenyl phosphate) flame retardant is obtained. The bisphenol-A-bis(diphenyl phosphate) flame retardant is synthesized by a solid super acidic catalyst, so that the reaction time is greatly shortened, the reaction yield is increased, the product needs no acid washing and alkali washing processes, post-treatment steps are simplified, basically no wastewater is discharged, and compared with a Lewis acid catalyst, the solid super acidic catalyst reduces emission of 2.1 tons of wastewater for 1 ton of product.

Description

technical field [0001] The invention relates to a preparation method of flame retardant bisphenol A-bis(diphenyl phosphate). Background technique [0002] The molecular formula of bisphenol A-bis(diphenyl phosphate) (BDP for short) is C 39 h 34 o 8 P 2 , the molecular weight is 692, and its structural formula is as follows: [0003] , [0004] Bisphenol A bisdiphenyl phosphate (BDP) is an important class of phosphorus-based flame retardants. Compared with traditional non-polymeric flame retardants, it has good flame retardancy and good compatibility with polymer substrates. , Migration resistance, volatility resistance, long-lasting flame retardant effect. BDP is mainly used in the field of engineering plastics, suitable for the production of flame-retardant PC / ABS alloy, flame-retardant HIPS / PPO alloy and flame-retardant PC. It can compete with brominated flame retardants on flame retardant PC / ABS alloys. It can be used to manufacture flame-retardant PC / ABS and PC...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/12
Inventor 杜辉于春红刘晨晨吴金泉
Owner NANTONG JIANGSHAN AGROCHEM & CHEM LIMITED LIABILITY
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