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Preparation method of electronic grade 1, 3-propanesultone

A technology of propane sultone and electronic grade, which is applied in the field of preparation of electronic grade 1,3-propane sultone, can solve the problems of high cost, unqualified product quality, inability to prepare stable electronic grade, etc., and achieve quality stable effect

Inactive Publication Date: 2014-12-03
武汉松石科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For the control of 1.3-PS moisture and acid value, the traditional preparation of 1.3-PS is through rectification control to meet the requirements of electronic grade 1.3-PS products, but it cannot be well and stably controlled, and its quality is unstable
Rectification can obviously increase the content of the product, but in most cases, the water can only be stably controlled at 300ppm, and the acid value can only be stably controlled at 500ppm. Electronic grade 1.3-PS products produced by this method Quality often falls short
[0006] In addition, simply using molecular sieves to dehydrate 1,3-PS can solve the problem of 1,3-PS moisture, but the amount of use is large, the cost is high, and other impurities will be introduced, especially Na+, which seriously exceeds the standard, making the product The quality of the
[0007] In summary, the existing methods of rectification and molecular sieve cannot prepare stable electronic grade 1,3-PS

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] a) First, put 1000g of 1,3-propane sultone (acid value 500ppm, moisture 400ppm, sodium ion 50ppm) into a reactor equipped with 4A molecular sieves and let it stand at 35°C for 1 hour to obtain an acid value of 50ppm 1,3-propane sultone with 80ppm of water and 80ppm of sodium ion;

[0019] b) After filtering the liquid in the reactor, put 1,3-propane sultone into the reactor for vacuum distillation, the distillation temperature is 110-130°C, and the distillation pressure is -0.999MP;

[0020] c) Finally, the 1,3-propane sultone fraction is continuously passed through the glass column of 4A molecular sieve at a flow rate of 200L / h to obtain 520g of 1,3-propanesulfonate with an acid value of 35ppm, a water content of 50ppm, and a sodium ion content of 20ppm acid lactone.

Embodiment 2

[0022] a) First, put 1000kg of 1,3-propane sultone (acid value 450ppm, moisture 300ppm, sodium ion 40ppm) into a reactor equipped with 5A molecular sieves and let it stand at 40°C for 3 hours to obtain an acid value of 45ppm 1,3-propane sultone with a water content of 75ppm and a sodium ion content of 70ppm;

[0023] b) After filtering the liquid in the reactor, put 1,3-propane sultone into the reactor for vacuum distillation, the distillation temperature is 110-130°C, and the distillation pressure is -0.999MP;

[0024] c) Finally, the 1,3-propane sultone fraction is continuously passed through the glass column of 5A molecular sieve at a flow rate of 300L / h to obtain 600kg of 1,3-propanesulfonate with an acid value of 30ppm, a water content of 25ppm, and a sodium ion content of 15ppm acid lactone.

Embodiment 3

[0026] a) First put 1000kg of 1,3-propane sultone (acid value 500ppm, moisture 350ppm, sodium ion 45ppm) into a reactor equipped with molecular sieves and let stand at 35°C for 5 hours to obtain an acid value of 30ppm. 1,3-propane sultone with 65ppm of water and 68ppm of sodium ion;

[0027] b) After filtering the liquid in the reactor, put 1,3-propane sultone into the reactor for vacuum distillation, the distillation temperature is 110-130°C, and the distillation pressure is -0.999MP;

[0028] c) Finally, the 1,3-propane sultone fraction is continuously passed through the glass column of molecular sieve at a flow rate of 500L / h to obtain 620kg of 1,3-propanesulfonic acid with an acid value of 15ppm, a water content of 25ppm and a sodium ion of 15ppm Lactone.

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Abstract

The invention discloses a preparation method of electronic grade 1, 3-propanesultone. The preparation method comprises the following steps: a) firstly, putting 1, 3-propanesultone into a reaction kettle provided with a molecular sieve, and standing for 1-10 hours at 30-40 DEG C to obtain 1, 3-propanesultone with the acid value of 0-50ppm and the water mass content of 0-100ppm; b) after filtering, carrying out reduced-pressure distillation, wherein the distillation temperature is 110-130 DEG C and the distillation pressure is (-0.5)-(-0.1)MP; and c) finally, continuously passing through a glass column of the molecular sieve to obtain the 1, 3-propanesultone with the acid value of 0-50ppm, the water content of 0-100ppm and the content of sodium ions of 0-20ppm. The preparation method disclosed by the invention is simple and convenient to operate and low in cost, and the indexes of the prepared electronic grade 1, 3-propanesultone are qualified. The prepared electronic grade 1, 3-propanesultone is stable in quality.

Description

technical field [0001] The invention relates to a preparation method of 1,3-propane sultone, in particular to a preparation method of electronic grade 1,3-propane sultone. Background technique [0002] 1.3-Propane sultone (hereinafter referred to as "1.3-PS") is an important intermediate. 1,3-Propane sultone is a white crystal at room temperature with a melting point of 30-33°C. It is widely used in surface treatment, electronic plating, biochemistry, emulsion polymerization, wastewater treatment, photosensitive materials, lithium batteries, surfactants, etc. [0003] In recent years, due to the continuous advancement of science and technology, a large number of applications of 3G products, and the country's requirements for energy conservation and environmental protection, the application of lithium batteries has become more and more widely used. People's demand for lithium batteries has increased significantly. The role of 1.3-PS in lithium batteries can be improved. The ...

Claims

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Application Information

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IPC IPC(8): C07D327/04
CPCC07D327/04
Inventor 宋朝阳杨磊周烈平石国林刘淑君王娟潘菲
Owner 武汉松石科技股份有限公司
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