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Continuous production process for tributyl citrate

A technology of tributyl citrate and production process, which is applied in the field of chemical engineering, can solve the problems of discontinuous process, reduced production efficiency, large amount of waste water, etc., and achieves the effects of meeting environmental protection requirements, speeding up reaction speed, and small amount of waste water discharge

Active Publication Date: 2011-11-23
NANJING COLLEGE OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] ①Although sulfuric acid is cheap and has high catalytic activity, it has many disadvantages: long production cycle and low conversion rate; and due to the dehydration, esterification and oxidation of sulfuric acid, there are many by-products, which have a negative impact on the purification and recovery of reaction products. It is difficult; in addition, sulfuric acid also seriously corrodes equipment and increases production costs
[0007] ②The post-treatment of the traditional process mainly includes the steps of neutralization, water washing, vacuum dealcoholization, decolorization and pressure filtration, etc., which belongs to intermittent operation, the process is discontinuous, and the labor intensity is relatively high; alkali neutralization, water washing, and removal of sulfuric acid as a catalyst, As a result, the process is complicated, the amount of waste water is large, the separation efficiency is low, and the product is lost; the energy consumption of vacuum distillation dealcoholization is relatively high, and it must go through multi-stage dealcoholization to meet the requirements. The operation is complicated, the separation efficiency is low, the process is long, and the three wastes are generated more Many; equipment investment is large, production scale is small, reducing production efficiency
In general, the finer the catalyst particles, the faster the reaction rate, but the separation of small particle size catalysts is more difficult
Traditional separation methods such as gravity sedimentation, centrifugal separation, flotation, filter cake filtration, and depth filtration cannot effectively separate it from the liquid phase product, resulting in serious loss of catalyst and affecting the purity of the product

Method used

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  • Continuous production process for tributyl citrate
  • Continuous production process for tributyl citrate
  • Continuous production process for tributyl citrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1. Esterification process

[0038] Put citric acid and n-butanol into the reactor according to the molar ratio of 1:4.5, add 1.5% (mass percentage of citric acid) solid superacid catalyst 50 nm, close the feeding port, open the jacket heating steam valve, and control the steam <0.6 MPa (gauge pressure). Pay attention to the water outlet, strictly control the pressure in the kettle (gauge pressure) < 0.015 MPa, so as not to cause material flushing, control the maximum temperature of the reaction to less than 120°C, and take a sample for testing after 2 hours of reaction, and then take a sample every half an hour. When the acid value of the solution reaches less than 0.02 mg KOH / g, it can be considered that the esterification is completed, the jacket heating steam valve is closed, the reflux valve is closed, and the stirring is stopped. Open the reactor condenser to cool down.

[0039] 2. Membrane neutralization and water washing process

[0040] After the reaction is ...

Embodiment 2

[0046] 1. Esterification process

[0047] Put citric acid and n-butanol into the reaction kettle according to the molar ratio of 1:4, add 1% (mass percentage of citric acid) molecular sieve catalyst 10 nm, close the feeding port, open the jacket heating steam valve, and control the steam < 0.6 MPa (gauge pressure). Pay attention to the water outlet, strictly control the pressure in the kettle (gauge pressure) < 0.015 MPa, so as not to cause material flushing, control the maximum temperature of the reaction to less than 100 ° C, react for 3 hours, take samples for testing, and then take samples every half an hour, when the crude ester liquid When the acid value reaches less than 0.02mgKOH / g, it can be considered that the esterification is completed, the jacket heating steam valve is closed, the reflux valve is closed, and the stirring is stopped. Open the reactor condenser to cool down.

[0048] 2. Membrane neutralization and water washing process

[0049] After the reaction...

Embodiment 3

[0055] 1. Esterification process

[0056] Put citric acid and n-butanol into the reactor according to the molar ratio of 1:6, add 3% (mass percentage of citric acid) heteropolyacid catalyst 100 nm, close the feeding port, open the jacket heating steam valve, and control the steam <0.6 MPa (gauge pressure). Pay attention to the water outlet, strictly control the pressure in the kettle (gauge pressure) < 0.015 MPa, so as not to cause material flushing, control the maximum temperature of the reaction to less than 140 ° C, react for 4 hours, take samples for testing, and then take samples every half an hour, when the crude ester liquid When the acid value reaches less than 0.02mgKOH / g, it can be considered that the esterification is completed, the jacket heating steam valve is closed, the reflux valve is closed, and the stirring is stopped. Open the reactor condenser to cool down.

[0057] 2. Membrane neutralization and water washing process

[0058] After the reaction is compl...

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Abstract

The invention relates to a continuous production process for tributyl citrate, in particular to a continuous production process for refining the tributyl citrate by a membrane separation technology, and belongs to the technical field of chemical engineering. In esterification, a solid acid catalyst with the granularity of 10 to 100nm is adopted and has high activity and high reaction speed. The traditional neutralization washing, catalyst separation and reduced pressure dealcholization process is improved by the membrane separation technology, the whole technological process is continuously and automatically operated, the production efficiency is high, the product quality is stable. The catalyst separation process and the esterification process are coupled in the same system, and the problem that a fine suspended catalyst is seriously lost in the separating and recycling process is solved. By membrane separation, the energy consumption is low and the recovery efficiency of butanol is high. The equipment investment is small, and the process is suitable for large-scale production.

Description

technical field [0001] The invention relates to a continuous production process of tributyl citrate, in particular to a continuous production process for refining tributyl citrate by membrane separation technology, and belongs to the technical field of chemical engineering. Background technique [0002] Tributyl citrate (TBC for short) is a new type of "green" environmentally friendly plastic plasticizer. It has the advantages of non-toxic, tasteless, good compatibility, high plasticizing efficiency, easy biodegradation and low volatility. , Excellent light resistance and water resistance, and has anti-mildew properties in resins, and can replace traditional phthalate-based plasticizers. Therefore, TBC is widely used in food and medical equipment packaging, cosmetics, daily necessities, toys, personal hygiene products and other fields, and it is also an important chemical intermediate. [0003] The traditional TBC production process is generally synthesized by esterificati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/704C07C67/08B01D17/022B01D61/36
Inventor 李冬燕于清跃许宁
Owner NANJING COLLEGE OF CHEM TECH
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