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Citric acid mixed ester production method

A production method and citric acid technology, applied in the field of plasticizers, can solve the problems of high synthesis temperature of octyl citrate, influence on market application of citrate ester, and high product color number, and achieve environmental friendliness, strong adaptability, and low catalyst cost. Effect

Pending Publication Date: 2021-01-12
山东朗晖石油化学股份有限公司
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Problems solved by technology

[0002] Citric acid ester is an environmentally friendly plasticizer. With the inclusion of o-phthalic plasticizers in the excellent control catalog, the use is limited. As a substitute plasticizer, the market will continue to expand, with There is a huge market space, but the common butyl citrate in the market currently has the problem of easy precipitation and oil leakage, and the problem of high color number of the product due to the high synthesis temperature of octyl citrate has affected the market application of citrate

Method used

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  • Citric acid mixed ester production method

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Embodiment 1

[0027] The production method of citric acid mixed ester comprises the following steps:

[0028] 1) Esterification process

[0029] The role of the esterification process is to complete the main reaction of the device and is a key process to control the conversion rate of raw materials. Add citric acid, butanol, octanol and catalyst to the reaction kettle, use concentrated sulfuric acid as the catalyst, carry out esterification according to the molar ratio of citric acid:alcohol (butanol+octanol) of 1:4.5, and the alcohol is excessive. The melting temperature is controlled within 145°C.

[0030] 2) Neutralization and washing process

[0031] Use lye to neutralize and remove sulfuric acid and incompletely esterified citric acid mono- and di-esters in the crude ester.

[0032] 3) Stripping process

[0033] The neutralized crude ester contains water, a small amount of low boiling matter and a certain amount of alcohol. In this process, the nitrogen protection vacuum stripping ...

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Abstract

The present invention relates to the technical field of plasticizers, and discloses a citric acid mixed ester production method, which comprises the steps of: an esterification process; a neutralizingand washing process; a steam stripping process; and a filtration process. According to the citric acid mixed ester production method, concentrated sulfuric acid is adopted as a catalyst, the catalystactivity is high, the reaction temperature is low, the reaction speed is high, the catalyst cost is low, the esterification synthesis temperature is controlled within 145 DEG C, it is ensured that the color number of the produced mixed citrate product is within 45, the market use requirement is met, and by adjusting the added butanol according to the market requirement, tetrabutyl citrate, dibutyl-octyl citrate, monobutyl dioctyl citrate and trioctyl citrate in different proportions can be obtained according to the octanol proportion, it is ensured that the produced citric acid mixed ester does not have the phenomena of precipitation and oil seepage in the using process, meanwhile, the using requirements of production of different customers are met, an intermittent esterification processis adopted, the operation elasticity is high, the strain capacity is high, and market requirements can be met.

Description

technical field [0001] The invention relates to the technical field of plasticizers, in particular to a production method of citric acid mixed esters. Background technique [0002] Citric acid ester is an environmentally friendly plasticizer. With the inclusion of o-phthalic plasticizers in the excellent control catalog, the use is limited. As a substitute plasticizer, the market will continue to expand, with There is a huge market space, but the common butyl citrate in the market currently has the problem of easy precipitation and oil leakage, and the problem of high color number of the product due to the high synthesis temperature of octyl citrate has affected the market application of citrate. [0003] The production method adopts a brand-new production technology, uses concentrated sulfuric acid as a catalyst, and adopts low-temperature synthesis technology to produce citric acid mixed esters. Contents of the invention [0004] (1) Solved technical problems [0005] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C67/60C07C67/48C07C67/56C07C69/704
CPCC07C67/08C07C67/60C07C67/48C07C67/56C07C69/704
Inventor 李乐钦刘延华张旭王美霞
Owner 山东朗晖石油化学股份有限公司
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