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Technology for synthesizing ATBC (acetyl tributyl citrate) under catalysis of composite solid acid

A technology of acetyl tributyl citrate and tributyl citrate, which is applied in the synthesis field of plasticizer acetyl tributyl citrate (ATBC), can solve the problem of many "three wastes", large product loss, long production cycle, etc. problems, to achieve the effect of less "three wastes", less equipment corrosion, and high product quality

Active Publication Date: 2015-07-29
江苏雷蒙新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to research and develop a kind of composite solid acid catalyst, the TBC synthesized under the action of this kind of catalyst is not separated and washed with water, only need dealcoholization can directly carry out acylation reaction, synthesize acetyl tributyl citrate The process overcomes the shortcomings of the existing preparation method of acetyl tributyl citrate, such as complex process, long production cycle, large product loss, many "three wastes" and environmental pollution. The catalyst is simple to prepare, easy to separate and recycle, and does not need It can be recycled and reused many times

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) Catalyst preparation

[0026] Weigh SnO 2 and SiO 2 500g each, Al 2 o 3， 3kg, add 200g of water and stir evenly, the catalyst is calcined in a muffle furnace at a temperature of 650°C for 2.5 hours to obtain a solid acid catalyst, the catalyst contains SnO 2 : SiO 2 1:1, (SnO 2 —SiO 2 ):Al 2 o 3 It is 1:3.

[0027] 2) Preparation of tributyl citrate

[0028] Add 19.2kg (0.1kmol) of anhydrous citric acid, 29.7kg (0.4kmol) of n-butanol and 4.32kg of the above catalyst (theoretical citrate mass 1.2% of 1.2%), stirred and reacted at 130°C~160°C for 3.0h~6.0h, synthesized TBC, measured the acid value according to GB 1668-81, the esterification rate was ≥ 99.0%, and the product was dealcoholized to obtain crude TBC.

[0029] 3) Preparation of acetyl tributyl citrate Add 12.1kg (0.12kmol) of acetic anhydride to the crude TBC (35.7kg) prepared in step 1), react at 70℃~80℃ for 0.5h~1.5h, synthesize ATBC, and then Filter the catalyst, add water to the filtrate (t...

Embodiment 2

[0030] Embodiment 2: With reference to Example 1, the catalyst preparation parameters are unchanged, and the parameter settings in the preparation of tributyl citrate and the preparation of acetyl tributyl citrate are changed:

[0031] 2) Preparation of tributyl citrate

[0032] Add anhydrous citric acid 19.2kg (0.1kmol), n-butanol 37.1kg (0.5kmol) and catalyst 5.76kg (theoretical citric acid ester mass 1.6%), stirred and reacted at 130°C~160°C for 3.0h~6.0h, synthesized TBC, measured the acid value according to GB 1668-81, the esterification rate was ≥99.0%, and the product was dealcoholized to obtain crude TBC.

[0033] 3) Preparation of acetyl tributyl citrate

[0034] Add 15.3kg (0.15kmol) of acetic anhydride to the obtained TBC crude product (35.5kg), react at 70°C~80°C for 0.5h~1.5h to synthesize ATBC, then filter the catalyst, add water to the filtrate (the amount of water added is equal to or slightly greater than the amount required for complete hydrolysis of unrea...

Embodiment 3

[0035] Embodiment 3: With reference to Example 1, the catalyst preparation parameters are unchanged, and the parameter settings in the preparation of tributyl citrate and the preparation of acetyl tributyl citrate are changed:

[0036] 2) Preparation of tributyl citrate

[0037] Add anhydrous citric acid 19.2kg (0.1kmol), n-butanol 29.7kg (0.4kmol) and catalyst 7.2kg (theoretical citric acid ester mass 2.0% of 2.0%), stirred and reacted at 130℃~160℃ for 3.0h~6.0h, synthesized TBC, measured the acid value according to GB 1668-81, the esterification rate was ≥ 99.0%, and the product was dealcoholized to obtain crude TBC.

[0038] 3) Preparation of acetyl tributyl citrate

[0039] Add 12.1kg (0.12kmol) of acetic anhydride to the obtained TBC crude product (35.8kg), react at 70°C~80°C for 0.5h~1.5h to synthesize ATBC, then filter the catalyst, add water to the filtrate (the amount of water added is equal to or slightly greater than the amount required for the complete hydrolysi...

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Abstract

A technology for synthesizing ATBC (acetyl tributyl citrate) under catalysis of composite solid acid comprises steps as follows: citri acid anhydrous and n-butyl alcohol are added to a reactor, a catalyst is added, the mixture reacts for 3-6 hours at the temperature of 120 DEG C-160 DEG C, and TBC (tributyl citrate) is synthesized and dealcoholized; acetic anhydride is added to dealcoholized TBC and reacts for 1-2 hours at the temperature of 60 DEG C-100 DEG C, the catalyst is obtained through filtering after a reaction liquid is cooled, water is added to filtrate, acetic anhydride is hydrolyzed, acetic acid is recovered through deacidification, and an ATBC finished product is prepared through aftertreatment. Defects of a complicated technology, long production period, high product loss, numerous three wastes, environmental pollution and the like of an existing preparation method of ATBC are overcome; the catalyst is simple to prepare and easy to separate and recover and can be recycled without treatment.

Description

technical field [0001] The invention belongs to the field of chemical synthesis and technology, and relates to a method for synthesizing plasticizer acetyl tributyl citrate (ATBC). Background technique [0002] Traditional plasticizers, phthalates, may cause cancer, and foreign countries have legislated to restrict their use. Acetyl tributyl citrate (ATBC), as a "green" environmental plasticizer, has been approved by the US Food and Drug Administration (FDA). With the advantages of water resistance and low volatility, it is widely used in food packaging, medical products, children's toys and other fields, and has become the first choice to replace phthalate plasticizers. [0003] At present, there is a huge vacancy in the ATBC domestic market. The traditional method of ATBC synthesis is a homogeneous system with concentrated sulfuric acid as a catalyst. The separation of raw materials and products requires a large amount of lye to neutralize and wash with water, the post-t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/67
CPCC07C67/08C07C69/67C07C69/704
Inventor 曹立军周永芳陈平周建安
Owner 江苏雷蒙新材料有限公司
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