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Synthesis method of neopentyl glycol dibenzoate

A technology of neopentyl glycol dibenzoate and a synthesis method, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem of low utilization rate of raw materials and difficult synthesis of neopentyl glycol. , the problem of high production cost, to reduce the color number of products, improve the efficiency of esterification reaction, and shorten the production cycle.

Pending Publication Date: 2021-09-17
武汉亿科德精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of this, it is necessary to provide a synthetic method of neopentyl glycol dibenzoate, in order to solve the technical problems that the synthesis of neopentyl glycol is difficult, the raw material utilization rate is low, and the production cost is high in the prior art

Method used

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preparation example Construction

[0011] The invention provides a kind of synthetic method of neopentyl glycol dibenzoate, comprising the following steps:

[0012] S1, the solid neopentyl glycol is dissolved in water or liquefied by introducing water vapor to obtain a neopentyl glycol solution;

[0013] S2. Mix neopentyl glycol solution, catalyst and benzoic acid, pass nitrogen gas, and evaporate water, then raise the temperature to 160-255°C, and perform esterification reaction for 5-10 hours. After the esterification reaction, decolorize, neutralize And, washed with water, dehydrated, filtered, cooled to obtain neopentyl glycol dibenzoate.

[0014] In the present invention, use water as solvent, dissolve or liquefy solid neopentyl glycol by heating method, then add benzoic acid to dissolve, do not use organic solvent, can reduce product cost, be environmentally friendly, have less potential safety hazards, improve benzoic acid reaction Efficiency, increased reaction speed.

[0015] In the present invention...

Embodiment 1

[0026] Put 104.15g of neopentyl glycol and 72g of water in the reactor, heat and stir to make the neopentyl glycol dissolve completely, continue to add 219.82g of benzoic acid, catalyst (0.81g of stannous oxalate, 0.81g of basic zirconium carbonate); pass into nitrogen , keep warm at 110-120°C for about 6 hours to evaporate water; raise the temperature to 180-185°C to start the first step of esterification reaction, keep warm for 3 hours, after the end, continue to heat up to 250-255°C, keep warm for 3 hours; the reaction is complete Finally, stop heating, transfer the material to the water washing kettle, keep feeding nitrogen, and when the temperature of the material is reduced to about 80-85°C, add hydrogen peroxide, and keep it at 100-105°C for 1 hour; wait for the temperature of the material to drop to about 80-85°C , slowly add lye to adjust the pH of the system to above 9, and keep the system temperature at 90°C, stir for 30 minutes, let it stand for 30 minutes, extract ...

Embodiment 2

[0028] Put 104.15g of neopentyl glycol and 108g of water in the reactor, heat and stir to make the neopentyl glycol dissolve completely, continue to add 244.24g of benzoic acid, catalyst (magnesium silicate 2.8g, basic zirconium carbonate 0.7g); feed nitrogen , keep warm at 110-120°C for about 6 hours to evaporate water, raise the temperature to 170-175°C to start the first step of esterification reaction, keep warm for 3 hours, after the end, continue to heat up to 220-225°C, keep warm for 4 hours; the reaction is complete Finally, stop heating, transfer the material to the water washing kettle, keep feeding nitrogen, and when the temperature of the material is reduced to about 70-75°C, add hydrogen peroxide, and keep it at 110-115°C for 1 hour; wait for the temperature of the material to drop to about 80-85°C , slowly add lye to adjust the pH of the system to above 9, and keep the system temperature at 90°C, stir for 45 minutes, let it stand for 45 minutes, extract the aqueou...

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Abstract

The invention discloses a synthesis method of neopentyl glycol dibenzoate, which comprises the following steps: adding water into solid neopentyl glycol for dissolving or introducing water vapor for liquefying to obtain a neopentyl glycol solution; mixing the neopentyl glycol solution, a catalyst and benzoic acid, introducing nitrogen, evaporating water, then raising the temperature to 160-255 DEG C, carrying out esterification reaction for 5-10 hours, and after the esterification reaction is finished, carrying out decoloration, neutralization, water washing, dehydration, filtration and cooling to obtain neopentyl glycol dibenzoate. Water is added as a medium, and a two-step esterification method is used, so that the color number of a product can be reduced, and the esterification reaction efficiency is improved; the method is simple in process, short in production period, high in product yield, small in color number, energy-saving, environment-friendly and easy to realize industrialization.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a synthetic method of neopentyl glycol dibenzoate. Background technique [0002] Neopentyl glycol dibenzoate is a crystalline solid powder which is insoluble in water but soluble in many solvents such as alcohols, ketones, esters, aliphatic hydrocarbons, aromatic hydrocarbons and chlorinated hydrocarbons. This product is compatible with polyvinyl chloride, polyvinyl butyrate, polymethyl methacrylate, cellulose acetate butyrate, ethyl cellulose and nitrocellulose, the compatible capacity reaches 50% of the resin content, and can Used in rubber and polyurethane products, as a plasticizer for these resins, it has excellent heat resistance and light resistance. This product is an environmentally friendly additive, which can be regarded as non-toxic and can be widely used in consumer products such as cosmetics. [0003] The synthesis of ester can be divided into esterifica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/78B01J21/14B01J27/236B01J31/04B01J31/38
CPCC07C67/08B01J31/04B01J27/236B01J21/14B01J31/38B01J2231/49B01J35/19C07C69/78Y02P20/584
Inventor 彭檬李本强胡永红
Owner 武汉亿科德精细化工有限公司
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