System and method for synthesis of tri-n-butyl citrate through continuous esterification

A technology for tri-n-butyl ester and a synthesis method, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of limited output in a single workshop, difficulty in safe production, and many sets of equipment, and achieves enhanced Market competitiveness, improving the utilization rate of raw materials, and reducing the effect of the three wastes

Inactive Publication Date: 2015-10-07
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] 1. There are many sets of equipment, large floor area, and large building area. Due to the restriction of chemical design regulations, the output of a single workshop is limited, and it is difficult to realize a single production device (workshop) with a scale of 25,000 tons / year or more.
[0005] 2. Difficult to realize automatic control, large amount of labor, high labor intensity and poor working environment
[0006] 3. There are many production links and control points, relying on manual control is easy to cause operational errors, it is difficult to produce safely, and it is easy to cause waste of raw materials and energy, and it is difficult to guarantee the stability of product quality
[0007] 4. Too much investment, high production costs, reducing the market competitiveness of products

Method used

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  • System and method for synthesis of tri-n-butyl citrate through continuous esterification

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Example 1: A continuous esterification synthesis of tri-n-butyl citrate system, including dissolving tank 1, esterification tank 2, dehydration tower 3, condenser 4, oil-water separator 5, dissolving tank 1 is set to two, dissolving Tank 1 is connected to 4 esterification tanks 2 connected in series, esterification tank 2 is connected to dehydration tower 3, the top outlet of dehydration tower 3 is connected to condenser 4, condenser 4 is connected to oil-water separator 5, and oil-water separator 5 is connected to dehydration Near the upper end of the tower 3, the bottom of the dehydration tower 3 is connected to the first esterification kettle 2. The operation procedure includes the following steps:

[0030] a. Mix and dissolve citric acid, n-butanol and catalyst in the mixing and dissolving tank 1. The molar ratio of citric acid and n-butanol is generally 1:4, and the catalyst is added in an appropriate amount according to production needs;

[0031] b. Add the mixed liqui...

Embodiment 2

[0036] Example 2: Take a 50,000 tons / year TBC production device as an example.

[0037] Refer to the system of Example 1:

[0038] 1. Design the volume and heating area of ​​each esterification vessel, the diameter of the esterification dehydration tower and the height of the packing (or the number of trays), the size and form of the condenser, the specifications of the oil-water separator, etc., and consider the appropriate margin to build 50,000 tons / Year TBC continuous esterification unit.

[0039] 2. Configure a mixed solution of citric acid and n-butanol in a ratio of 1:4.5 (molar ratio) and add an appropriate amount of catalyst. Add the mixed solution (according to the corresponding acid content) into the No. 1 esterification kettle at a constant speed and heat it with steam.

[0040] 3. Turn on the standby butanol pump to add proper butanol to the first esterification kettle, and adjust the steam consumption of each esterification kettle, and control the temperature of each ke...

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Abstract

The invention provides a method for synthesis of tri-n-butyl citrate (TBC) through continuous esterification. The method comprises the following steps: adding a mixture of citric acid, n-butanol and a catalyst into a reaction system at a uniform speed, wherein the reaction system is composed of a plurality of esterification reaction vessels in series connection, the mixture is added into a first esterification vessel, reaction temperature successively rises from 112-160 DEG C, and a semi-finished product containing butanol in a certain proportion is discharged from a last esterification vessel; allowing the semi-finished product to enter an evaporator to remove residual butanol so as to obtain crude ester liquid; and carrying out conventional post-treatment with a plasticizer so as to obtain a TBC finished product. According to the invention, the continuous esterification is more applicable to automatic operation and large-scale production; land occupation is small, and investment is low; reaction is thorough, and the utilization rate of the raw materials is high; safety production and stable product quality are guaranteed; and comprehensive utilization is realized, energy is saved, and discharge of waste water, waste gas and waste industrial residues is reduced.

Description

Technical field [0001] The invention relates to a continuous production process of tri-n-butyl citrate, which is produced by a continuous esterification method, and belongs to the technical field of chemical synthesis engineering. Background technique [0002] Acetyl tri-n-butyl citrate (ATBC) and tri-n-butyl citrate (TBC) have the advantages of good compatibility with high molecular polymers, high plasticizing efficiency, non-toxicity, strong weather resistance, and easy biodegradability. It has attracted wide attention and has become an excellent substitute for phthalates and other petrochemical plasticizers that are highly reproductively toxic, suspected of causing cancer, not easily biodegradable, and have a large impact on the environment, especially for children's toys, food packaging and medical materials The application is the most common. [0003] The first chemical reaction in the synthesis of ATBC is the reaction of citric acid and n-butanol to form TBC. The traditiona...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/704
CPCC07C67/08C07C69/704
Inventor 周建安周永芳陈平曹立军邵平
Owner 江苏雷蒙新材料有限公司
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