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Preparation method of macromolecular bisphenol A tetraphenyl diphosphate

A technology of tetraphenyl bisphosphate and polymer is applied in the field of polymer compound preparation, which can solve the problems of reducing the thermal deformation temperature of flame-retardant substrates, low total product yield, and large plasticizing effect, so as to save processing energy. , The effect of good material fluidity and low volatility

Active Publication Date: 2010-03-17
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical solution of the present invention is to overcome the need to be equipped with heat preservation system and metering pump device when applying LDBP in the prior art, which is not conducive to environmental protection, has a large plasticizing effect, reduces the thermal deformation temperature of the flame-retardant substrate, and the product The shortcoming that the total yield is still low, provides a method for preparing SBDP, determines reasonable and feasible process conditions, and can meet the requirements of industrial production in terms of product quality, yield and environmental protection

Method used

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  • Preparation method of macromolecular bisphenol A tetraphenyl diphosphate
  • Preparation method of macromolecular bisphenol A tetraphenyl diphosphate
  • Preparation method of macromolecular bisphenol A tetraphenyl diphosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Step 1: Preparation of MPDCPO

[0034] 230g (1.5mol) POCl 3 and 0.2gAlCl 3 Add it into the reaction flask, stir, heat up to 70°C, start to add phenol dropwise, the dosage is 47g (0.5mol), POCl 3 / phenol=3 / 1 (molar ratio). After adding phenol dropwise, the reaction can take place. The phenol was added over 0.5 h at 70°C. After the phenol was added, the temperature began to rise, and the temperature of the material was raised to 100° C. within 45 minutes, and then the material was ordered to react at this temperature. The reaction was stopped when no more HCl was evolved. After the reaction was completed, excess POCl was distilled off under reduced pressure 3 , the residue is the product of the first step, which contains MPDCPO90%, and the yield (in terms of phenol) is 97%. If you want to prepare MPDCPO with higher purity, you can purify it with vacuum distillation.

[0035] Step 2: Preparation of HPC

[0036] 148g (0.7mol) MPDCPO (applied directly after the previ...

Embodiment 2

[0043] Step 1: Preparation of MPDCPO

[0044] With 153g (1.0mol) POCl3, 23.5g (0.25mol) phenol and 0.24gMgCl 2 Put it into the reactor at room temperature, then start to heat up, rise from room temperature to 70°C within the first 30 minutes (at this time, HCl will be released), stay for 10 minutes, then raise the temperature from 70°C to 120°C within 45 minutes, and then at this temperature Continue the reaction for 1 to 1.5 hours until the actual amount of HCl released is similar to the theoretical amount, that is, stop the reaction. After completion of the reaction, excess POCl was distilled off under reduced pressure 3 , the residue is the product of the first step, and the yield (in terms of phenol) is 98%.

[0045] Step 2: Preparation of HPC

[0046] 54.8g (0.26mol) MPDCPO, 59.3g (0.26mol) bisphenol A (MPDCPO / bisphenol A = 1.0 (molar ratio)) and 1.0gAlCl 3 Add it into the reactor, stir, heat up, and raise the temperature to 60°C within 25 minutes (that is, HCl is rel...

Embodiment 3

[0052] Step 1: Preparation of MPDCPO

[0053] 383g (2.5mol) POCl 3 and 0.7g ZnCl 2 Add it into the reaction bottle, stir, heat up to 70°C, start to add phenol dropwise, the dosage is 47g (0.5mol), add the phenol within 1.0h at 75°C, after adding the phenol, start to heat up, within 40min by 75°C was raised to 130°C, and then the materials were ordered to react at this temperature, and the reaction was completed when HCl was no longer released. Distill off excess POCl under reduced pressure 3 , the residue is the product of the first step, and the yield (in terms of phenol) is 98.5%.

[0054] Step 2: Preparation of HPC

[0055] MPDCPO97.8g (0.46mol), bisphenol A 116g (0.51mol) (MPDCPO / bisphenol A = 0.9 (molar ratio)) and AlCl 3 Add 1.0g into the reaction flask, stir, heat up, and raise the temperature to 50°C within 6 minutes; then raise the temperature to 65°C within 10 minutes, and react at 65°C for 20 minutes; then raise the temperature to 80°C within 10 minutes, and re...

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Abstract

The invention relates to a preparation method of macromolecular bisphenol A tetraphenyl diphosphate, belonging to the technical field of macromolecular compound preparation. The method contains four specific steps, the previous three steps are used to prepare raw SBDP and the final step is to wash raw SBDP. The method comprises the following specific steps: step 1 preparing phenoxyphosphinic dichloride (MPDCPO) with two functional groups; step 2 preparing macromolecular bisphenol A diphosphate phosphorylchloride (HPC); and step 3 capping the end of HPC; and step 4 washing the raw SBDP to obtain the finished product. The invention has the advantages that organic solvent is not needed in the preparation process and the yield is 5% higher than that of LBDP. SBDP is a solid high polymer, the charging of SBDP is convenient, the hydrolysis stability is high, the mobility is low, the volatility is low and the material has little influence on the heat stability of the base material; in addition, the softening and melting temperature of SBDP are low and SBDP is in melting state under the processing temperature of engineering plastics so that SBDP can be mixed evenly with the flame resistance base material; the fluidity of the material is good, thus saving the processing energy.

Description

technical field [0001] The invention belongs to the technical field of polymer compound preparation, and relates to a preparation method of polymer bisphenol A tetraphenyl bisphosphate. Background technique [0002] Due to human beings' increasing emphasis on environmental protection, due to the restrictions of the EU RoHS Directive and the Stockholm Convention, and due to the need to meet the requirements of international and new flame retardant standards in my country, halogen-free in the field of flame retardant has become a recognized development trend, and it is inevitable. Row. Therefore, the halogen-free bisphosphonate BDP listed at home and abroad in recent years has a large market and objective application prospects (currently mainly used in PC and PC / ABS), but BDP is liquid (LBDP) and has a low molecular weight, so there are the following Disadvantages: (1) Since it is in a liquid state, it needs to be equipped with an insulation system and a metering pump device f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/04
Inventor 金译平吕云兴陆凯凯
Owner ZHEJIANG WANSHENG