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Novel solvent-free method for preparing AKD by taking tri-n-propylamine as raw material

A technology of tri-n-propylamine, alkyl ketene dimer, applied in the direction of adding water repellent, organic chemistry, etc., can solve the problem of high viscosity

Inactive Publication Date: 2020-05-12
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In view of the fact that the viscosity of the reaction system is too high due to the solvent-free preparation of alkyl ketene dimer by using triethylamine as raw material, the present invention adopts tri-n-propylamine as raw material for preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Weigh 145mL of tri-n-propylamine and 151g of stearyl chloride, add tri-n-propylamine into the reaction kettle, stir and preheat to 60°C; then gradually drop stearyl chloride into the reaction kettle, and control the feed rate below 5g / min , control the reaction temperature to 60° C. and continue to stir, and continue to react for another 3 hours when the feeding is completed.

[0017] After the reaction, add 25g of hydrochloric acid with a mass concentration of 37%, react for 10min, and take the oil layer after standing for stratification; add 300mL of 60°C hot water, stir fully, continue for 20min, stand for stratification, and obtain AKD; then dry, that is For AKD products. Afterwards, the purity of AKD was 91.32%, which was detected by a UV-visible spectrophotometer.

Embodiment 2

[0019] Weigh 100mL of triethylamine and 151g of stearyl chloride, add triethylamine into the reactor, stir and preheat to 60°C; then gradually drop stearyl chloride into the reactor, and control the feed rate below 5g / min , control the reaction temperature to 60° C. and keep stirring, and continue the reaction for 5 hours after the feed is completed.

[0020] After the reaction, add 25g of hydrochloric acid with a mass concentration of 37%, react for 20min, and take the oil layer after standing for stratification; add 300mL of hot water at 60°C, stir fully, continue for 20min, and let stand for stratification to obtain AKD; then dry it, that is For AKD products. Then it was tested with a UV-Vis spectrophotometer, and the purity of AKD was 90.20%.

Embodiment 3

[0022] Weigh 95mL of tri-n-propylamine, 44mL of toluene and 151g of stearyl chloride, add tri-n-propylamine and toluene into the reactor, stir and preheat to 60°C; Below 5g / min, control the reaction temperature to 60°C and keep stirring, and continue the reaction for another 2hr after the feeding is completed.

[0023] After the reaction, add 300mL of hot water at 60°C, stir thoroughly for 20 minutes, and let stand to separate layers to obtain AKD; then dry it to obtain the AKD product. Then it was detected by a UV-Vis spectrophotometer, and the purity of AKD was 89.56%.

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PUM

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Abstract

According to the invention, triethylamine is replaced by tri-n-propylamine, and AKD is synthesized by carrying out a reaction on the tri-n-propylamine and stearoyl chloride through a solvent-free method, so that the viscosity of the reaction system can be reduced, and the purity and the yield of the AKD are effectively improved; and the feasibility of using tri-n-propylamine as a reactant tertiaryamine is proved. The invention relates to a solvent-free method for preparing alkyl ketene dimer AKD.

Description

technical field [0001] The invention relates to a synthesis technology of alkyl ketene dimer AKD. It is mainly suitable for the synthesis method of tertiary amine and fatty acid chloride, especially for the preparation of AKD by the solvent-free method. Background technique [0002] As the most commonly used neutral sizing agent in the paper industry, AKD is in increasing demand. Traditional AKD production methods generally use benzene and toluene as solvents. With the improvement of people's awareness of environmental protection, people have put forward higher requirements for the quality of products they are in contact with daily. The inspection standards for organic residues in products are getting higher and higher. Paper is The toluene content of our commonly used items is relatively strict. Some large paper companies in many developed countries have limited the maximum content of toluene in AKD, and some companies even stipulate that AKD emulsions containing toluene s...

Claims

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Application Information

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IPC IPC(8): C07D305/12D21H21/16
CPCC07D305/12D21H21/16
Inventor 卢素敏朱峰
Owner TIANJIN POLYTECHNIC UNIV
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