Method for preparing dichlorohydrin through glycerinum chlorination under catalysis of HY type molecular sieve

A technology of molecular sieve catalyzing glycerol and dichloropropanol, applied in the direction of introducing halogen preparation, organic chemistry, etc., can solve the problems of difficult separation, difficult recovery of organic acids, large catalyst consumption, etc., and achieves easy operation, easy recovery and reuse, low cost effect

Inactive Publication Date: 2014-11-19
JIANGSU UNIV
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  • Abstract
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Problems solved by technology

[0004] At present, the research on the preparation of dichloropropanol by the chlorination of glycerin mainly uses organic acids as catalysts, but the characteristics of organic acids are not easy to recover and separate, which make the catalyst consumption is relatively large, so the development of catalysts that can be recycled is the focus of this process research

Method used

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  • Method for preparing dichlorohydrin through glycerinum chlorination under catalysis of HY type molecular sieve
  • Method for preparing dichlorohydrin through glycerinum chlorination under catalysis of HY type molecular sieve
  • Method for preparing dichlorohydrin through glycerinum chlorination under catalysis of HY type molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 1.5g HY type molecular sieve (purchased from Shanghai Youxin Molecular Sieve Co., Ltd., SiO 2 / Al 2 o 3 =5) Activate at 400°C for 2 hours, then add it into a 100mL four-neck flask containing 50g of glycerin, and stir to disperse evenly. When the system reaches 110°C, the flow rate of 60mL min into the system -1 HCl gas, reacted for 12h, and the tail gas was condensed and then absorbed by NaOH solution to remove HCl.

[0018] The molecular sieves in the above steps were changed to HY-type molecular sieves with silicon-aluminum ratios of 7 and 11 respectively, and the influence of molecular sieves with different silicon-aluminum ratios on the chlorination reaction of glycerin was studied. The experimental results are shown in Table 1:

[0019] Table 1 Effect of molecular sieves with different ratios of silicon to aluminum on the chlorination of glycerin

[0020]

[0021] Note: 2-MCPD is 2-chloro-1,3-propanediol, 3-MCPD is 3-chloro-1,2-propanediol, 1,3-DCP is 1,3-di...

Embodiment 2

[0024] 0.1g HY type molecular sieve (purchased from Shanghai Youxin Molecular Sieve Co., Ltd., SiO 2 / Al 2 o 3 =5) Activate at 400°C for 2 hours, then add it into a 100mL four-neck flask containing 50g of glycerin, and stir to disperse evenly. When the system reaches 110°C, the flow rate of 60mL min into the system -1 HCl gas, reacted for 12h, and the tail gas was condensed and then absorbed by NaOH solution to remove HCl.

[0025] Change the amount of molecular sieve in the above steps to 1g, 1.5g and 2.5g, and study the influence of catalyst amount on the experiment, the results are shown in Table 2:

[0026] Table 2 Effect of catalyst dosage on the chlorination reaction of glycerol

[0027]

[0028] Note: 2-MCPD is 2-chloro-1,3-propanediol, 3-MCPD is 3-chloro-1,2-propanediol, 1,3-DCP is 1,3-dichloro-2-propanol, 2, 3-DCP is 2,3-dichloro-1-propanol.

[0029] It can be seen from Table 2 that with the increase of the amount of catalyst, the reaction rate increases, but...

Embodiment 3

[0031] 1.5g HY type molecular sieve (purchased from Shanghai Youxin Molecular Sieve Co., Ltd., SiO 2 / Al 2 o 3 =5) Activate at 400°C for 2 hours, then add it into a 100mL four-neck flask containing 50g of glycerin, and stir to disperse evenly. When the system reaches 110°C, the flow rate of 60mL min into the system -1 HCl gas, reacted for 12h, and the tail gas was condensed and then absorbed by NaOH solution to remove HCl.

[0032] The reaction temperature in the above steps was changed to 90°C and 130°C to study the effect of the reaction temperature on the chlorination reaction of glycerol. The experimental results are shown in Table 3:

[0033] Table 3 Effect of reaction temperature on the chlorination reaction of glycerol

[0034]

[0035] Note: 2-MCPD is 2-chloro-1,3-propanediol, 3-MCPD is 3-chloro-1,2-propanediol, 1,3-DCP is 1,3-dichloro-2-propanol, 2, 3-DCP is 2,3-dichloro-1-propanol.

[0036] With the increase of reaction temperature, the rate of glycerin chlo...

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Abstract

The invention provides a method for preparing dichlorohydrin through glycerinum chlorination under catalysis of an HY type molecular sieve. According to the method, dichlorohydrin is prepared by taking a biodiesel byproduct glycerinum as a raw material, a normal hydrogen chloride gas as a chlorinating agent and the HY molecular sieve of different silicon-aluminum ratios as chlorination catalysts by using a gas-liquid two-phase method. The method for preparing dichlorohydrin is low in raw material cost, relatively gentle in reaction condition and small in amount of byproducts, the catalyst HY molecular sieve is high in catalysis activity and good in selectivity, appropriate reaction conditions are selected, and the yield of dichlorohydrin is greater than 87%. In addition, after the catalyst is repeatedly used for 5 times, the yield of dichlorohydrin is still greater than 80%, and the circulation effect is relatively good. By adopting the method, a novel way is provided for industrial production of dichlorohydrin through glycerinum chlorination.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a method for synthesizing dichloropropanol. Background technique [0002] The catalytic conversion of renewable resources and chemicals has received much attention, with studies showing that bulk chemicals from fossil sources, such as sugars and other compounds from plants, can be produced from renewable resources in biorefineries. Biodiesel, as a green fuel, can already be produced from vegetable oil. However, in the process of producing biodiesel, the main problem is that a considerable amount of glycerol will be produced as a by-product. For this reason, many researchers have devoted themselves to the research on the conversion of glycerol to high-value chemicals, a typical example of which is the preparation of dichloropropanol by chlorination of glycerol. [0003] Dichloropropanol is a raw material for the synthesis of various chemical products such as dichloroacetone, cell...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/36C07C29/62
CPCC07C29/62C07C31/36
Inventor 侯祥祥殷恒波王爱丽
Owner JIANGSU UNIV
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