Continuous preparation method for bisphenol A-di(diphenyl phosphate)

A technology of diphenyl phosphate and bisphenol, which is applied in the field of continuous preparation of bisphenol A-bis(diphenyl phosphate), can solve the problem that the product quality and yield are difficult to meet the process requirements, increase equipment investment and maintenance Costs, inability to achieve product quality and other issues, to achieve the effect of solving the difficulty of solid feeding, solving the problem of air tightness of the device, and improving product yield and quality

Active Publication Date: 2017-03-15
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the production cannot be continuous, the reaction conditions are unstable, the reaction time is long, and large-scale production needs to invest a lot of equipment, instruments, and personnel, and the quality of batch products cannot be stabilized, and the investment scale is huge.
In addition, further expand the product scale according to market demand. If large-scale equipment (listed in more than 10,000L kettles) is used, the output of a single reactor can be increased. The quality and yield are more difficult to meet the process requirements, and the larger the reactor, the greater the risk of its operation
In order to ensure the product quality yield and increase the output, the existing process often uses multiple reactors and multiple sets of devices, which greatly increases the investment and maintenance costs of the equipment.

Method used

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  • Continuous preparation method for bisphenol A-di(diphenyl phosphate)
  • Continuous preparation method for bisphenol A-di(diphenyl phosphate)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The preparation of embodiment 1 BDP, its technological process is as figure 1 As shown, the specific steps are as follows:

[0031] 1. Continuous multi-stage cross-linking reaction process:

[0032] Put 2000Kg / h of phosphorus oxychloride into the premixing tank, recover 2500Kg / h of phosphorus oxychloride, and 15Kg / h of magnesium chloride, and then heat the mixed phosphorus oxychloride to 90-100°C by pump pressurization , at the same time, bisphenol A1500kg / h is continuously fed in proportion, and the cross-linking reaction is carried out in the first-stage cross-linking reactor: the reaction material passes through the bottom of the tank, pressurized by a pump, and goes to the gas-liquid separator tower and condenser to realize gas-liquid separation and condensation. Phosphorus oxychloride returned to the kettle. The reaction temperature in the kettle is 95-100°C, and the reaction material is transferred to the subsequent reactor for heat preservation by using the poten...

Embodiment 2

[0047] Substantially the same as Example 1, but remove the capping reaction and add magnesium chloride 10Kg / h, and the residence time of each reactor material is 3 hours. Other things remain unchanged, the final finished product is 4266.5kg / h, and the product yield is 96.80%. Product color 35, TPP content 0.86%, main content N 1 84.7% (HPLC).

Embodiment 3

[0049] It is basically the same as Example 1, but the amount of phosphorus oxychloride is changed to 5500kg / h, the amount of phenol in the continuous capping reaction process is changed to 2380kg, and 10Kg of added magnesium chloride is removed. Other things remain unchanged, the final finished product is 4288.49kg / h, and the product yield is 97.3%. Product color 35, TPP content 0.78%, main content N 1 87.4% (HPLC).

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Abstract

The invention discloses a continuous preparation method for bisphenol A-di(diphenyl phosphate). The continuous preparation method for the bisphenol A-di(diphenyl phosphate) comprises a multistage crosslinking reaction process, a continuous phosphorus oxychloride recycling process, a continuous multistage end capping reaction and phenol recycling process, a continuous crude product refining process, and a continuous solvent recycling and filtering process. The BDP is prepared by the continuous processes, the production cost is reduced, the labor intensity of operators is greatly reduced, the labor efficiency is improved, and the product yield is greatly improved, so the lot production quality is stable, and the production is safe and environment-friendly. The yield is improved by 1-1.5%, the color number is improved below 50, and the TPP is controlled to be 1%, and is reduced by 50% compared by an original intermittence device. The high-end customer requirement is satisfied, and the quality index fluctuation of each product is small.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a continuous preparation method of 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-bis(diphenyl phosphate) is a colorless or light yellow liquid, insoluble in water, and miscible with dichloromethane, toluene, methanol and methyl ethyl ketone. Density (25°C) 1.26g / ㎝ 3 , the viscosity (40°C) is about 2200mpa.s, and the temperatures for TGA weight loss of 5%, 10% and 50% are 371°C, 397°C and 444°C, respectively. [0005] It is a halogen-free flame retardant widely used in PC / ABS, PPO / HIPS and other polymers. [0006] At present, regarding the method of preparing bisphenol A-bis(diphenyl phosphate) flame retardant, the commonly used...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/12
CPCC07F9/12
Inventor 吕云兴金译平陶光撑王福兵许晓敏
Owner ZHEJIANG WANSHENG
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