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Method for preparing 1,4-butane sultone by micro-channel reactor

A micro-channel reactor, sultone technology, applied in the direction of organic chemistry, etc., can solve the problems of poor temperature control effect of single-pot reaction, long mixing and contact time, easy to produce by-products, etc., to improve the molar yield and eliminate local Overheating phenomenon, molar yield improvement effect

Inactive Publication Date: 2019-07-02
ZHANGJIAGANG HICOMER CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Currently, the disclosed preparation methods of 1,4-butane sultone such as CN201610784116.8, CN201710182914.8, and CN201810314201.7 all belong to the traditional process, and all have the following disadvantages: 1. Using traditional batch operation, the production capacity per unit time Low, high energy consumption; 2. Large amplification effect, poor temperature control effect of single-pot reaction, long mixing contact time, slow separation, easy to produce by-products, low molar yield

Method used

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  • Method for preparing 1,4-butane sultone by micro-channel reactor
  • Method for preparing 1,4-butane sultone by micro-channel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. At room temperature, dissolve 132.3g of sodium sulfite in 529.4g of deionized water, stir and dissolve, and prepare an aqueous solution of sodium sulfite with a mass fraction of 20%.

[0026] 2. The heater is heated to 80°C, and the sodium sulfite aqueous solution and 150.6 g of chlorobutyl acetate are respectively pumped synchronously by the first micropump 3 and the second micropump 4 to the premixer 11 for mixing, and the flow rate of the sodium sulfite aqueous solution is 14.31 mL / min, the flow rate of chlorobutyl acetate is 1.36mL / min.

[0027] The mixed material in the premixer 11 enters the microchannel module 12 and reacts. The hydraulic diameter of the microchannel in the microchannel module 12 is 1.0mm, and the length of the microchannel is 100m. The residence time of the material in the microchannel module is 300s, the molar ratio of chlorobutyl acetate to sodium sulfite is 1:1.05.

[0028] 3. The reaction solution enters the reactor 5 from the discharge...

Embodiment 2

[0031] 1. At room temperature, dissolve 132.3g of sodium sulfite in 529.4g of deionized water, stir and dissolve, and prepare an aqueous solution of sodium sulfite with a mass fraction of 20%.

[0032] 2. The heater is heated to 120°C, and the sodium sulfite aqueous solution and 150.6g of chlorobutyl acetate are respectively pumped synchronously by the first micropump 3 and the second micropump 4 to the premixer 11 for mixing, and the flow rate of the sodium sulfite aqueous solution is 14.31mL / min, the flow rate of chlorobutyl acetate is 1.36mL / min.

[0033]The mixed material in the premixer 11 enters into the microchannel module 12 and reacts. The hydraulic diameter of the microchannel in the microchannel module 12 is 1.0mm, and the length of the microchannel is 100m. The material is in the microchannel of the microchannel module. The residence time is 300s, and the molar ratio of chlorobutyl acetate to sodium sulfite is 1:1.05.

[0034] 3. The reaction solution enters the ...

Embodiment 3

[0037] 1. At room temperature, dissolve 132.3g of sodium sulfite in 529.4g of deionized water, stir and dissolve, and prepare an aqueous solution of sodium sulfite with a mass fraction of 20%.

[0038] 2. The heater is heated to 145°C, and the sodium sulfite aqueous solution and 150.6g of chlorobutyl acetate are respectively pumped synchronously by the first micropump 3 and the second micropump 4 to the premixer 11 for mixing, and the flow rate of the sodium sulfite aqueous solution is 14.31mL / min, the flow rate of chlorobutyl acetate is 1.36mL / min.

[0039] The mixed material in the pre-mixer 11 enters the microchannel module 12 for reaction, the hydraulic diameter of the microchannel in the microchannel module 12 is 1.0mm, and the length of the microchannel is 100m, and the material is in the microchannel of the microchannel module The residence time is 300s, and the molar ratio of chlorobutyl acetate to sodium sulfite is 1:1.05.

[0040] 3. The reaction solution enters th...

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Abstract

The invention discloses a method for preparing 1,4-butane sultone by a microchannel reactor. A reaction device adopted by the method comprises the enhanced mass transfer type micro-channel reactor with a premixer and a micro-channel module, a first micro-pump and a second micro-pump are respectively connected with the premixer, the output end of the premixer is communicated with the feed end of the micro-channel module, the discharge end of the micro-channel module is connected to a reaction kettle, a discharge tube at the bottom of the reaction kettle is connected to a filter, and the filteris connected with a rectification kettle. An aqueous sodium sulfite solution and chlorobutyl acetate are respectively pumped into the premixer; a reaction solution enters the reaction kettle from thedischarge end of the micro-channel module, and undergoes reduced pressure dehydration, concentrated hydrochloric acid is added, and the obtained solution is refluxed and stirred; and the reaction solution in the reaction kettle is cooled, and then is filtered, and the obtained filtrate undergoes concentration, dehydration cyclization and rectification in the rectification kettle to obtain the finished 1,4-butane sultone. The method has the advantages of high reaction efficiency, good product quality, effective reduction of byproducts, and effective improvement of the molar yield.

Description

technical field [0001] The invention relates to the technical field of 1,4-butane sultone preparation. Background technique [0002] Microchannel reactor technology emerged in the 1990s. It can not only enhance mass transfer and heat transfer, but also meet continuous large-scale production, and has attracted widespread attention. Different from the simple dropwise addition of traditional reactors, the reaction method of microchannel reactors is the collision of reaction fluids, which has unique advantages in synthesis: reaction fluids can be mixed quickly, and the mixing time is shorter than the reaction time, forming a stable and uniform reaction environment without backmixing. [0003] Organic sulfonate is a new type of organic film-forming additive with better effect, mainly because its central sulfur atom has stronger electronegativity, and its reducibility at the graphite negative electrode interface is stronger than that of the corresponding carbonate, and its reduci...

Claims

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Application Information

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IPC IPC(8): C07D327/06
CPCC07D327/06
Inventor 赵建许国荣庞宝华周跃东刘国红
Owner ZHANGJIAGANG HICOMER CHEM CO LTD
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