Improvement of 1,6-hexaaldehyde purity

A technology of adipaldehyde and purity, applied to improve 1, can solve the problems of reduced yield, waste, perishable, low yield of 1,6-adipaldehyde, etc.

Inactive Publication Date: 2006-05-31
CHINA PETROCHEMICAL CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, low temperature (less than 15°C) storage is required. When using the prior art to separate and purify 1,6-hexanedialdehyde, 1,6-hexanedialdehyde is also very easy to deteriorate, resulting in is

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0023] This example illustrates the method provided by the invention.

[0024] Place the three-necked flask in a water bath. Adjust the temperature of the water bath to 70°C. Add 235.4 g of sodium periodate to the flask, then add 450 ml of water at 70° C., and stir until the sodium periodate powder is completely dissolved. Mix the obtained sodium periodate solution with 920 grams of silica gel particles, and stir under the condition of controlling the temperature at 70-80°C until the silica gel changes from the viscous state when it was first added to a solid fluid state, and then stop stirring to obtain catalyst C1 .

[0025] Add 115.4 grams of catalyst C1 in a three-necked flask, add 250 milliliters of dichloromethane, and mix 170 milliliters of dichloromethane and 11.6 grams (calculated on the basis of 23.54 grams of sodium periodate, sodium periodate and cyclohexane The weight ratio of diol is 2.03) the dichloromethane solution of the cyclohexanediol that cyclohexanedio...

example 2

[0031] This example illustrates the method provided by the invention.

[0032] Prepare the concentrated solution of 1,6-hexanedial by the method of example 1, the difference is only, the pressure of vacuum distillation is 15mmHg (1993.4 Pa), and the temperature is 5 ℃, obtains the concentrated solution containing 1,6-hexanedial 10.12 g, the content of 1,6-hexanedial in the concentrate is 95% by weight, and the yield of 1,6-hexanedial is 82.9% by weight.

example 3

[0034] This example illustrates the method provided by the invention.

[0035]Add 115.4 grams of catalyst C1 in a three-necked flask, add 200 milliliters of dichloroethane, and mix 150 milliliters of dichloroethane and 21.4 grams of cyclohexanediol under stirring at 42°C to obtain the dichloromethane of cyclohexanediol Solution, after the dropwise addition, reacted for another 2 hours, filtered the mixture of catalyst and liquid reaction product obtained, washed the catalyst with 25 milliliters of dichloroethane, washed 3 times in total, mixed the obtained liquid reaction product and washing liquid, and mixed the obtained liquid reaction product and the washing solution at 22 ° C. Carry out underpressure distillation, the pressure of underpressure distillation is 150mmHg (19934 handkerchiefs), obtains the concentrated solution 19.5 grams that contains 1,6-hexanedial, in the concentrated solution, the content of 1,6-hexanedial is 93% by weight, 1 , The yield of 6-hexanedial was...

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PUM

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Abstract

A method for improving 1,6-biformyl purity is carried out by distilling solution containing 1,6-biformyl and organic solvent below normal pressure and under atmosphere of indifferent gas. It has higher purity and more output.

Description

technical field [0001] The present invention relates to a method for separating and purifying compounds containing more than one -CHO group, more precisely, relates to a method for improving the purity of 1,6-hexanedialdehyde. Background technique [0002] 1,6-Hexanedial (1,6-hexanedial) is a new type of green chemical product, which is harmless to the human body. Especially in the field of disinfection and sterilization, it has achieved good results due to its green and non-residue characteristics. Among them, in terms of plant sterilization, it has a unique effect in curing many diseases such as yellow wilt, root rot, and rice blast. Sterilization of oilfield injection water is the advantage of 1,6-hexanedialdehyde, which can effectively kill many protein pathogens such as ferrophytes and saprophytes. Applied to disinfection and sterilization of medical equipment, food equipment, poultry and livestock houses, etc., it can quickly and efficiently kill most bacteria, bacter...

Claims

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Application Information

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IPC IPC(8): C07C47/127C07C45/82
Inventor 李琼肖作兵毛海舫蔡宝国熊远凡王路
Owner CHINA PETROCHEMICAL CORP
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