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Preparation method of 1, 4-bis(4-phenoxy benzoyl) benzene and polyether ketone ketone

A technology of phenoxybenzoyl and phenoxybenzaldehyde, which is applied in the preparation of polyether ketone ketone and 1,4-bisphenyl, can solve the problems of waste of raw materials, increased procedures, and increased costs, and achieves The preparation method is effective, the content of impurities is reduced, and the effect of high product purity

Pending Publication Date: 2021-07-23
SHENZHEN WOTE ADVANCED MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, in the prior art, diphenyl ether and terephthaloyl chloride are used as raw materials to prepare 1,4 bis(4-phenoxybenzoyl)benzene, which will produce some xanthyl alcohol side reaction impurities
If there are impurities such as xanthanol in 1,4 bis(4-phenoxybenzoyl)benzene, when preparing polyether ketone ketone (PEKK), structures such as xanthan alcohol will be formed in polyether ketone ketone (PEKK) The end group of the polymer is unstable at high temperature and will break to form a small molecular benzene ring substance, which will further undergo side reactions such as crosslinking and grafting with the polymer, which will affect the thermal stability of the material.
Moreover, the xanthene alcohol side reaction impurities are very difficult to remove, and the removal steps are complicated and cannot be completely removed
[0004] The method for preparing 1,4 bis(4-phenoxybenzoyl)benzene by the prior art, or the preparation of 1,4 bis(4-phenoxybenzoyl)benzene has more side reactions of xanthyl alcohols Impurities that affect the thermal stability of synthetic polyetherketoneketone (PEKK)
Either increase the removal steps of xanthene alcohol side reaction impurities, resulting in an increase in the process and an increase in cost
In addition, a large amount of waste of raw materials will be caused due to the use of excessive diphenyl ether

Method used

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  • Preparation method of 1, 4-bis(4-phenoxy benzoyl) benzene and polyether ketone ketone
  • Preparation method of 1, 4-bis(4-phenoxy benzoyl) benzene and polyether ketone ketone
  • Preparation method of 1, 4-bis(4-phenoxy benzoyl) benzene and polyether ketone ketone

Examples

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preparation example Construction

[0038] The embodiment of the present invention provides a preparation method of 1,4 bis(4-phenoxybenzoyl)benzene, comprising the following steps:

[0039] S10, providing the reactant mixture comprising 4-phenoxybenzaldehyde shown in formula (2), terephthaloyl chloride shown in formula (3) and Lewis acid catalyst in solvent, carry out Friedel-Crafts acylation Reaction, to obtain the mixture that comprises the compound described in following formula (1), and

[0040] S20, performing oxidation reaction and deacidification reaction sequentially on the mixture containing the compound described in the following formula (1), so as to obtain a mixture containing 1,4 bis(4-phenoxybenzoyl)benzene.

[0041] The preparation method of traditional 1,4 bis(4-phenoxybenzoyl)benzene is to prepare 1,4 bis(4-phenoxybenzoyl)benzene with diphenyl ether and terephthaloyl chloride as raw materials , in the presence of a catalyst, terephthaloyl chloride can easily attack diphenyl ether to form xanth...

Embodiment 1

[0088] 1. Add 45g of anhydrous AlCl to a 500ml three-necked bottle equipped with magnetic stirring and gas conduit 3 , 4.5gCuCl, 300ml0-DCB, 16mlDPE, start stirring, heat to 25°C, continue to feed a mixed gas of CO and HCl (1:1), and react for 6h.

[0089] 2. Switch the incoming gas to nitrogen, add 10.15g of TPC to the three-necked flask, and continue the reaction for 10h.

[0090] 3. The gas is switched to oxygen to carry out the oxidation reaction, the heating temperature is raised to 35°C, and the reaction is continued for 1 hour.

[0091] 4. The gas is switched to nitrogen, and the heating temperature is increased to 125° C. for decarboxylation reaction, and the reaction is continued for 1 hour.

[0092] 5. After the reaction is completed, slowly add 200ml of ice methanol to quench, filter, and wash with methanol and deionized water repeatedly until there is no organic residue and the filtrate is neutral. Finally, the product was dried in a vacuum oven at 150° C. to a c...

Embodiment 2

[0094] The preparation method of Example 2 is basically the same as that of Example 1, except that the molar ratio of CO and HCl in the mixed gas of CO and HCl is 1:3.

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Abstract

The invention relates to a preparation method of 1, 4-bis(4-phenoxy benzoyl) benzene and a preparation method for preparing polyether ketone ketone from the 1, 4-bis (4-phenoxy benzoyl) benzene. The preparation method of the 1, 4-bis (4-phenoxybenzoyl) benzene comprises the following steps: providing a reactant mixture containing 4-phenoxybenzaldehyde, terephthaloyl chloride and a Lewis acid catalyst in a solvent, and carrying out a Friedel-Crafts acylation reaction to obtain a mixture containing a compound as shown in the following formula (1); and sequentially carrying out an oxidation reaction and a decarboxylation reaction on the mixture containing the compound as shown in the formula (1) to obtain a mixture containing 1, 4-bis (4-phenoxy benzoyl) benzene.

Description

technical field [0001] The present invention relates to the technical field of organic synthesis, in particular to a method for preparing 1,4 bis(4-phenoxybenzoyl)benzene, and the 1,4 bis(4-phenoxybenzoyl) Benzene started the preparation method of polyether ketone ketone. Background technique [0002] 1,4 bis(4-phenoxybenzoyl)benzene is an intermediate used in many organic synthesis, and can also be used as a raw material for the synthesis of polyether ketone ketone (PEKK). In the prior art, 1,4 bis(4-phenoxybenzoyl)benzene is mostly synthesized with excess diphenyl ether and terephthaloyl chloride under the condition of Lewis acid as a catalyst, such as document US4816,556, In document WO95 / 23821 and document CN201880031935.2, when preparing 1,4 bis(4-phenoxybenzoyl)benzene, the molar ratio of diphenyl ether to terephthaloyl chloride exceeds 2. [0003] However, in the prior art, diphenyl ether and terephthaloyl chloride are used as raw materials to prepare 1,4 bis(4-phen...

Claims

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Application Information

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IPC IPC(8): C07C51/373C07C65/40C08G61/12
CPCC07C51/373C08G61/12C08G2261/3442C07C65/40
Inventor 陈章何征吴宪
Owner SHENZHEN WOTE ADVANCED MATERIALS
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