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Method for producing citrate by using microchannel reactor

A technology of microchannel reactor and citric acid ester, which is applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc., can solve the problems of high energy consumption and heavy pollution, and achieve low energy consumption and low reaction volume The effect of small size and simple process

Active Publication Date: 2014-01-08
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional method of producing citrate has the disadvantages of high energy consumption and heavy pollution.

Method used

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  • Method for producing citrate by using microchannel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Microchannel Reactor 1, see figure 1 , comprising an inlet 2, a catalyst column 3 and an outlet 4 connected in sequence through a connecting pipe, the inlet 2 is connected with a solution tank 6 through a liquid inlet pipe, a solution pump 7 is arranged on the liquid inlet pipe, and a heating sleeve 5 is also included, and the heating Sleeve pipe 5 is sleeved on the catalyst column 3; The pipeline diameter of this microchannel reactor is 2.1mm, and the liquid inlet pipe length is 15cm, and the connecting pipe length between inlet 2 and catalyst column 3 is 25cm, and catalyst column 3 and The length of the connecting pipe between the outlets 4 is 20cm; the volume of the catalyst column is 3mL, and the column is filled with D001 strong acid resin.

[0025] Take 340 g of citric acid monohydrate and 480 g of n-butanol and heat and stir to form a homogeneous phase to obtain a mixed solution; pump the mixed solution into a microchannel reactor. The reaction fluid flowed thro...

Embodiment 2

[0027] Microchannel reactor 1 is basically the same as Example 1, and the difference is only: the pipeline diameter of this microchannel reactor is 2.1mm, and the length of the liquid inlet pipe is 10cm, and the connection between the inlet 2 and the catalyst column 3 The length of the tube is 20cm, and the length of the connecting tube between the catalyst column 3 and the outlet 4 is 30cm; the volume of the catalyst column is 2mL, and the column is filled with solid superacid S 2 o 8 2- / SnO 2 SiO 2 .

[0028] Take 340 g of citric acid monohydrate and 430 g of n-propanol and heat and stir to form a homogeneous phase to obtain a mixed solution; pump the mixed solution into a microchannel reactor. The reaction fluid flowed through the catalyst column at a rate of 0.1 mL / min, and the jacket heating temperature of the catalyst column was 110°C. The crude product is collected at the outlet; the esterification rate is calculated by measuring the acid value. The determination...

Embodiment 3

[0030] Microchannel reactor 1 is basically the same as embodiment 1, and the difference is only: the pipeline of this microchannel reactor is 0.5mm, and the length of the liquid inlet pipe is 30cm, and the connecting pipe between the inlet 2 and the catalyst column 3 The length is 10cm, the length of the connecting pipe between the catalyst column 3 and the outlet 4 is 10cm; the catalyst column is 1mL, and the column is filled with solid superacid S with a mass ratio of 1:1 2 o 8 2- / SnO 2 SiO 2 And D001 strong acid resin.

[0031] Take 1 mol of citric acid monohydrate and 3 mol of ethanol and heat and stir to form a homogeneous phase to obtain a mixed solution; pump the mixed solution into a microchannel reactor. The reaction fluid flowed through the catalyst column at 0.8 mL / min, and the jacket heating temperature of the catalyst column was 100°C. The crude product is collected at the outlet; the esterification rate is calculated by measuring the acid value. The determ...

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Abstract

The invention provides a method for producing citrate by using a microchannel reactor. The method comprises the following steps: dissolving citric acid in alcohol to obtain citric acid alcohol liquor; heating a catalyst column to a constant temperature; introducing the citric acid alcohol liquor to the microchannel reactor (1), wherein the citric acid alcohol liquor passes through the catalyst column at a constant flow rate; and collecting a catalyst column effluent to obtain the citrate. The method is simple in process, can continuously produce citrate, has high operating safety and high selectivity, and is small in reaction volume and short in time. The catalyst can be repeatedly used, and the equipment is hardly corroded. Meanwhile, as no water carrying agents are used, the esterification rate is over 96% by means of such characteristics of the microchannel reactor as efficient heat mass transfer capacity and easiness in direct amplification. The product has high quality and the energy consumption is low, so that the method is an environment-friendly and efficient method for synthesizing citrate.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a method for producing citrate by using a microchannel reactor. Background technique [0002] Plasticizer is the largest consumption of plastic additives, and its consumption accounts for more than 60% of the total consumption of plastic additives. At present, there are more than 500 kinds of plasticizers that have been commercialized, but the most consumed ones are phthalate plasticizers, especially di(2-ethyl)hexyl phthalate (DOP) and dibutyl phthalate (DBP), accounting for about 80% of the total consumption of plasticizers. In recent years, with people's attention to health and the in-depth research on phthalate plasticizers, it has been found that phthalate plasticizers pose a health threat to humans, and even have carcinogenic effects, especially on the development of infants and children The impact is greater. The United States, Japan, Sweden and other countries have en...

Claims

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Application Information

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IPC IPC(8): C07C69/704C07C67/08
CPCC07C67/08C07C69/704
Inventor 郭凯袁爱邦李昕唐拾贵欧阳平凯
Owner NANJING UNIV OF TECH
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