Supercharge Your Innovation With Domain-Expert AI Agents!

Integrated process of synthesizing acetyl tributyl citrate by using activated carbon immobilized p-toluenesulfonic acid catalyst

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

Inactive Publication Date: 2015-07-01
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
View PDF2 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to propose a kind of integrated process of synthesizing acetyl tributyl citrate under the action of solid acid catalysis, has overcome the complex process that existing acetyl tributyl citrate preparation method exists, the production cycle is long, the product Disadvantages such as large loss, many "three wastes" and environmental pollution, the tributyl citrate produced according to the method of the present invention does not need to be separated and washed, but directly carries out acylation reaction after dealcoholization, and the catalyst used is simple to prepare, Easy separation and recovery, and mild reaction conditions, good product quality

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] An integrated method for the synthesis of acetyl tributyl citrate by activated carbon immobilized p-toluenesulfonic acid catalyst, comprising the following steps:

[0032] (1) Catalyst (TsOH / C) preparation

[0033] Weigh 1 kg of activated carbon for sugar liquid decolorization, soak it in 10 kg of p-toluenesulfonic acid solution with a mass concentration of 25%, stir it at room temperature for 20 hours, filter it after loading, and dry it at 90°C to constant weight to obtain the activated carbon. For the toluenesulfonic acid catalyst (TsOH / C), the mass ratio of p-toluenesulfonic acid in the catalyst calculated by the weight gain method is 35%.

[0034] (2) Preparation of tributyl citrate

[0035] Add 21.0kg (0.1kmol) of citric acid monohydrate, 31.9kg (0.43kmol) of n-butanol and 0.168kg of the above catalyst TsOH / C (monowater 0.8% of the mass of citric acid), stirred and reacted at 120°C for 4.0h, synthesized TBC, measured the acid value according to GB 1668-81, the e...

Embodiment 2

[0039] An integrated method for the synthesis of acetyl tributyl citrate by activated carbon immobilized p-toluenesulfonic acid catalyst, comprising the following steps:

[0040] (1) Catalyst (TsOH / C) preparation

[0041] Weigh 1 kg of activated carbon for decolorization of sugar liquid and soak it in 25 kg of p-toluenesulfonic acid solution with a mass concentration of 27%, stir and immobilize it at room temperature for 30 hours, filter it after immobilization, and dry it at 110°C to constant weight to obtain activated carbon immobilized p-toluene For the sulfonic acid catalyst (TsOH / C), the mass ratio of p-toluenesulfonic acid in the catalyst is calculated by the weight gain method to be 45%.

[0042] (2) Preparation of tributyl citrate

[0043] Add 21.0kg (0.1kmol) of citric acid monohydrate, 37.1kg (0.5kmol) of n-butanol and 0.105kg of the above catalyst TsOH / C (monowater 0.5% of the mass of citric acid), stirred and reacted at 140°C for 3.0h, synthesized TBC, measured t...

Embodiment 3

[0047] An integrated method for the synthesis of acetyl tributyl citrate by activated carbon immobilized p-toluenesulfonic acid catalyst, comprising the following steps:

[0048] (1) Catalyst (TsOH / C) preparation

[0049] Weigh 1 kg of activated carbon for sugar liquid decolorization and soak it in 40 kg of p-toluenesulfonic acid solution with a mass concentration of 30%, stir and immobilize it at room temperature for 40 hours, filter it after immobilization, and dry it at 100°C to constant weight to obtain activated carbon immobilized p-toluene For the sulfonic acid catalyst (TsOH / C), the mass ratio of p-toluenesulfonic acid in the catalyst is calculated by the weight gain method to be 55%.

[0050] (2) Preparation of tributyl citrate

[0051] Add 19.2kg (0.1kmol) of anhydrous citric acid, 33.4kg (0.45kmol) of n-butanol and 0.288kg (anhydrous 1.5% of the mass of citric acid), stirred and reacted at 110°C for 6.0h, synthesized TBC, measured the acid value according to GB 1668-...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
acid valueaaaaaaaaaa
purityaaaaaaaaaa
coloraaaaaaaaaa
Login to View More

Abstract

The invention relates to an integrated synthetic process of synthesizing acetyl tributyl citrate by using an activated carbon immobilized p-toluenesulfonic acid catalyst. The synthetic process comprises the step of preparing the activated carbon immobilized p-toluenesulfonic acid catalyst. The step of catalytically synthesizing acetyl tributyl citrate comprises the step of adding acetic anhydride into a dealcoholized tributyl citrate coarse product to react to obtain an acetyl tributyl citrate finished product. The integrated synthetic process provided by the invention overcomes the defects that the existing acetyl tributyl citrate preparation method is complex in process, long in production period, great in product loss and more in three wastes, pollutes environment and the like. The acetyl tributyl citrate produced by the method provided by the invention needs not to be separated and washed but is directly acylated after being dealcoholized. The used catalyst is simple to prepare and easy to separate and recover, and the reaction condition is mild and the product quality is good.

Description

technical field [0001] The present invention relates to a synthesis method of plasticizer acetyl tributyl citrate (ATBC), in particular to an integrated synthesis process for synthesizing acetyl tributyl citrate with an activated carbon immobilized p-toluenesulfonic acid catalyst, which belongs to chemical synthesis and craft fields. Background technique [0002] Traditional plasticizers, phthalates, may cause cancer, and foreign countries have legislated to restrict their use. Acetyl tributyl citrate (ATBC), as a new "green" plasticizer, has been approved by the US Food and Drug Administration (FDA). ATBC has the advantages of non-toxic, odorless, anti-mildew, good plasticizing effect, cold resistance, light resistance, water resistance, and low volatility. It is widely used in food packaging, medical products, children's toys and other fields, and has become a substitute for phthalates. The product of choice for plasticizers. [0003] At present, there is a huge gap in ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/67B01J31/02
CPCY02P20/10
Inventor 姚正军杜咪咪周金堂刘沛江王占红姚芮徐丹李琳姚田甜
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More