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Vitamin C catalyzing and synthesizing method with solid phase bifunctional catalyst

A dual-function catalyst, vitamin technology, applied in chemical recovery, organic chemistry and other directions, can solve the problems of complicated operation, high energy consumption, large pollution, etc., and achieve the effect of reducing operation steps, reducing raw material consumption, and reducing production costs.

Active Publication Date: 2012-07-04
溧阳常大技术转移中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Thereby overcoming the problems of high energy consumption, heavy pollution and complicated operation in the prior art

Method used

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  • Vitamin C catalyzing and synthesizing method with solid phase bifunctional catalyst
  • Vitamin C catalyzing and synthesizing method with solid phase bifunctional catalyst
  • Vitamin C catalyzing and synthesizing method with solid phase bifunctional catalyst

Examples

Experimental program
Comparison scheme
Effect test

example (1

[0025] In the 500mL three-necked flask, add 64g 2-KLG (0.3mol, 91%), 112g n-butanol (1.5mol), 160g chlorobenzene and SJ-1 catalyst as shown in structural formula 1 (wherein R1, R2 are all methyl) 9.6 g. In the first stage of the reaction, the temperature was controlled at 65°C and stirred for 2.5 hours. In the second stage of the reaction, the appropriate vacuum degree was controlled, and the water and n-butanol in the reaction system were rectified under reduced pressure while reacting at 75° C., and the operation was maintained for 5.5 hours. The reaction mixture was cooled to room temperature and then filtered to obtain a brown solid mixture. The resulting solid mixture was dissolved with deionized water, beaten, and suction filtered. The filter residue is mainly a catalyst, which can be recycled after being washed three times with 75ml of water and four times with 100ml of n-butanol; the filtrate is VC solution, which is decolorized by adding activated carbon, concentrat...

example (2

[0027]Add 64g 2-KLG (0.3mol, 91%), 135g n-butanol (1.8mol), 160g chlorobenzene in the 500mL there-necked flask, use the SJ-2 catalyst shown in structural formula 1 instead (wherein R1, R2 are all methyl, R3 is C 3 h 6 Hydrocarbyl) 9.6g, heated to 65°C and stirred for 3.0h. Then control the appropriate degree of vacuum, and rectify under reduced pressure the water and n-butanol in the reaction system while reacting at 75° C., and maintain such an operation for 6.5 hours. The rest are the same as example (1). 44.8g VC was obtained, the content was 99.95%, and the yield was 84.8%.

example (3

[0029] Add 64g 2-KLG (0.3mol, 91%), 67g n-butanol (0.9mol), and 160g chlorobenzene into a 500mL three-necked flask, and use 9.6g of SJ-3 catalyst as shown in structural formula 1 instead, heat up to 65°C and stir for 3.5 h. Then control the appropriate degree of vacuum, and rectify under reduced pressure the water and n-butanol in the reaction system while reacting at 75° C., and maintain such an operation for 6.5 hours. The rest are the same as example (1). 43.7g VC was obtained, the content was 99.96%, and the yield was 82.8%.

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Abstract

The invention relates to a vitamin C catalyzing and synthesizing method with solid phase bifunctional catalyst, which comprises the following steps of: (1) adding 2-KLG, low carbon alcohol, solid acid and alkali bifunctional catalyst into inert solvent, stirring for temperature reaction, reacting for 1.5 to 3.5 h at 55 to 85 DEG C at the first stage, and reacting for 2.5 to 8.5 h at 45 to 100 DEGC at the second stage, wherein the mole ratio of 2-KLG to low carbon alcohol is 1:3-7, the low carbon alcohol is the alcohol with 1 to 8 carbon atoms, the inert solvent is halogenated hydrocarbon, ether or dutrex, and the weight of the catalyst is 5 to 25% of that of 2-KLG; (2) finishing reaction after stirring for a certain period of time in a temperature controlling mode, distilling low carbon alcohol and water from the reaction system after decompression, cooling the reactant mixture to room temperature, filtering to obtain brown solid mixture; and (3) dissolving solid mixture with deionized water, pulping, filtering to obtain VC solution, adding active carbon to remove color, reducing pressure and condensing, freezing for crystallization, filtering and drying in vacuum to obtain the purificatory VC finished products. The invention simplifies operation steps, reduces waste water discharge in production course.

Description

technical field [0001] The invention relates to the technical field of vitamin C (Vitamin C, hereinafter referred to as VC) production. Specifically, the production of VC is prepared by esterification and lactonization using guronic acid as a starting material under the action of an acid-base dual-function catalyst. craft. Background technique [0002] Vitamin C is an essential vitamin that has many biological and pharmaceutical functions. In the food industry, VC is widely used as a vitamin supplement and antioxidant in many foods. In medicine, VC has the functions of preventing bleeding, detoxification, enhancing the body's resistance to diseases, and reducing the incidence of cancer. It has a huge market demand in the pharmaceutical and food industries. [0003] The method for the industrial synthesis of VC is based on the catalytic conversion of 2-keto-L-gulonic acid (hereinafter referred to as 2-KLG). According to the different properties of raw materials or catalyst...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/62
CPCY02P20/584
Inventor 单玉华张元元王桂敏蒋志国汪友谊李明时
Owner 溧阳常大技术转移中心有限公司
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