Preparation method and application of p-phenylacetophenone

A technology of phenylacetophenone and biphenyl, which is applied in the field of preparation of p-phenylacetophenone, can solve the problems of not being able to meet market demand, increase production cost expenditure, environmental impact, etc., achieve large specific surface area, reduce Production cost, the effect of reducing industrial production cost

Active Publication Date: 2022-01-18
PAPANNA BEIJING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Biphenol is an important fine chemical intermediate for the synthesis of bifenazate. At present, there are two main industrial production methods of biphenol: 1. Sulfonated alkali fusion method, but this method will produce a large amount of waste acid water, which is very important for factory wastewater treatment The system generates a lot of pressure, which increases the production cost
2. Purify the by-products from the phenol production process, but the yield is low and cannot meet the existing market demand
However, this method will produce a large amount of aluminum trichloride wastewater, and alkaline hydrolysis will produce a large amount of waste acid water and waste solids, which will have a serious impact on the environment.

Method used

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  • Preparation method and application of p-phenylacetophenone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The preparation of embodiment 1 H type molecular sieve catalyst

[0040] Concrete preparation steps are as follows:

[0041] Dissolve 100g of silica sol in 200g of distilled water, dissolve 2.84g of sodium aluminate and 2.32g of strong sodium oxide in 80g of distilled water to form an alkaline sodium aluminate solution. At a temperature of 25-30°C, add the aqueous silica sol solution dropwise to the alkaline sodium aluminate solution, keep stirring for 5.0-6.0h, then add it to the crystallization autoclave, and crystallize at 200°C for 50h. Then filter under reduced pressure, and the refined high-purity crystals are calcined at 400-450° C. for 3.0-4.0 hours to obtain ordinary Na-ZSM-5 zeolite.

[0042] Then, under the condition of 100-120°C, put Na-ZSM-5 zeolite in ammonium nitrate solution (2mol / L) and stir for 5.0h to obtain preliminary H-ZSM-5 zeolite, and add 30% sulfuric acid solution after filtration , stirred at 50°C for 2.0h, filtered, calcined at 250-300°C fo...

Embodiment 2

[0044]The synthesis of embodiment 2 p-phenylacetophenone

[0045] Proceed as follows:

[0046] Add 315g DMSO in 1000ml autoclave, add biphenyl (1.0mol, 157.36g), acetic acid (1.3mol, 79.66g), H-type molecular sieve catalyst 9.44g (6% of biphenyl mass).

[0047] Raise the temperature to 180°C, pressurize to 0.6MPa, stir and react for 5.0h, lower the temperature and pressure, take samples for analysis, and the reaction is complete.

[0048] The dehydration catalyst was removed by filtration, DMSO and acetic acid were removed by vacuum distillation, 315 g of dichloroethane and 50 g of water were added, the mixture was stirred and left to separate layers, and the organic phase was spin-dried to obtain 193.78 g of the product with a purity of 96.50% and a yield of 95.41%.

Embodiment 3

[0050] Proceed as follows:

[0051] Add 315g DMSO in 1000ml autoclave, add biphenyl (1.0mol, 157.36g), acetic acid (1.5mol, 91.92g), H-type molecular sieve catalyst 12.59g (8% of biphenyl mass).

[0052] Raise the temperature to 180°C, pressurize to 0.6MPa, stir and react for 5.0h, lower the temperature and pressure, take samples for analysis, and the reaction is complete.

[0053] The dehydration catalyst was removed by filtration, DMSO and acetic acid were distilled off under reduced pressure, 315 g of dichloroethane and 50 g of water were added, stirred and left to separate, and the organic phase was spin-dried to obtain 193.89 g of the product with a purity of 95.42% and a yield of 94.39%.

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Abstract

The invention belongs to the technical field of diphenol preparation, and particularly relates to a preparation method and application of p-phenylacetophenone. The invention provides a preparation method of p-phenylacetophenone, wherein the method comprises the following step: in an organic solvent, dehydrating biphenyl and acetic acid under the action of an H-type molecular sieve catalyst under the conditions of high temperature and high pressure to generate p-phenylacetophenone. According to the invention, an H-type molecular sieve catalyst is introduced into a p-phenylacetophenone generation process for the first time, the purpose of producing p-phenylacetophenone by using cheaper acetic acid as a raw material is achieved by utilizing the structural characteristics of the H-type molecular sieve catalyst, and the production cost of p-phenylacetophenone is greatly reduced; the production process has few reaction steps, and the product purity and yield are obviously improved; and the process solves the problem that a large amount of aluminum trichloride wastewater is generated in the existing p-phenylacetophenone generation process.

Description

technical field [0001] The invention belongs to the technical field of biphenol preparation, and in particular relates to a preparation method and application of p-phenylacetophenone. Background technique [0002] Bifenazate (bifenazate, chemical name 3-(4-methoxybiphenyl-3-yl) isopropyl carbazate) is a new type of selective foliar spray acaricide. Its mechanism of action is the inhibitory effect on the gamma-aminobutyric acid (GABA) receptor of the central nervous system of mites. It is effective against all life stages of mites, and has a long duration of effect. It is also effective against herbivorous mites such as spider mites and panonychia, and has a contact effect. It can be used to prevent and control spider mites and panonychia in crops such as apples, strawberries, peaches, grapes, and stone fruits. At the same time, it is harmless to beneficial insects, has low toxicity, and is environmentally friendly. [0003] Biphenol is an important fine chemical intermedia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/784C07C45/45B01J29/40B01J35/10C07C39/15C07C37/01
CPCC07C45/455B01J29/40B01J35/1004C07C37/01C07C37/64C07C67/42C07C2529/40B01J2229/37B01J2229/40C07C2527/054C07C2531/02C07C49/784C07C39/15C07C39/235C07C69/16Y02P20/584
Inventor 邢文龙孙飞
Owner PAPANNA BEIJING TECH
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