Method for preparing allyldimethyl dehydroabietyl ammonium chloride

A technology for allyl dimethyl dehydroabietyl and dimethyl dehydroabietin amine, which is applied in the field of preparing cationic surfactants containing dehydroabietin amine structure, and can solve the problem of affecting product application performance, decreasing reaction activity, etc. problem, to achieve the effect of excellent antistatic performance, low preparation cost and high content

Inactive Publication Date: 2012-11-14
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The invention of a method for preparing allyl dimethyl dehydroabietyl ammonium chloride is mainly to solve the problem of preparing allyl dimethyl by direct reaction of allyl chloride and N,N-dimethyl dehydroabietyl ammonium chloride. Allyl chloride self-polymerization and allyl chloride and the generated allyl dimethyl dehydroabietyl

Method used

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  • Method for preparing allyldimethyl dehydroabietyl ammonium chloride
  • Method for preparing allyldimethyl dehydroabietyl ammonium chloride
  • Method for preparing allyldimethyl dehydroabietyl ammonium chloride

Examples

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Effect test

Embodiment 1

[0020] 100 grams of dehydroabietic amines are dissolved with 400 grams of composite solvents composed of ethanol and acetonitrile in a mass ratio of 0.01: 7 to form a homogeneous solution, then add 600 grams of formic acid aqueous solution with a mass percentage concentration of 30%, and stir to form The solution of abietamine formate; Add 50 grams of methylation reagents consisting of formaldehyde and paraformaldehyde in a mass ratio of 1.0:5.0 to the solution containing dehydroabietamine formate, and react at 40°C After 60 hours, the mixed material containing N,N-dimethyl dehydroabietamine formate was obtained; the mixed material containing N,N-dimethyl dehydroabietamine formate was neutralized, extracted with toluene, saturated salt Water washing, water washing and liquid separation, normal pressure or reduced pressure distillation to recover toluene and vacuum fractionation to obtain N,N-dimethyl dehydroabietic amine and compound inhibitor according to the mass ratio of 0.1...

Embodiment 2

[0022] 100 grams of dehydroabietic amines are dissolved with 800 grams of ethanol and acetonitrile in a composite solvent of 0.1: 10 by mass ratio to form a homogeneous solution, then add 900 grams of formic acid aqueous solution with a mass percentage concentration of 50%, and stir to form a compound solvent containing dehydrogenated The solution of abietamine formate; Add 100 grams of methylation reagents consisting of formaldehyde and paraformaldehyde in a mass ratio of 7:15 to the solution containing dehydroabietamine formate, and react at 70°C In 36 hours, the mixed material containing N,N-dimethyl dehydroabietamine formate was obtained; the mixed material containing N,N-dimethyl dehydroabietamine formate was neutralized, extracted with toluene, saturated salt Water washing, water washing and liquid separation, normal pressure or reduced pressure distillation to recover toluene and vacuum fractionation to obtain N,N-dimethyl dehydroabietine amine and compound inhibitor acc...

Embodiment 3

[0024]100 grams of dehydroabietic amines are dissolved with 1200 grams of composite solvents composed of ethanol and acetonitrile in a mass ratio of 3: 13 to form a homogeneous solution, then add 900 grams of formic acid aqueous solution with a mass percentage concentration of 70%, and stir to form The solution of abietamine formate; Add 150 grams of methylation reagents consisting of formaldehyde and paraformaldehyde in a mass ratio of 5.0:3 to the solution containing dehydroabietamine formate, and react at 60°C In 48 hours, the mixed material containing N,N-dimethyl dehydroabietamine formate was obtained; the mixed material containing N,N-dimethyl dehydroabietamine formate was neutralized, extracted with toluene, saturated salt Water washing, water washing and liquid separation, normal pressure or reduced pressure distillation to recover toluene and vacuum fractionation to obtain N,N-dimethyl dehydroabietine amine and composite inhibitor in mass ratio 0.1:0.01 and then use ab...

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Abstract

The invention relates to a method for preparing allyldimethyl dehydroabietyl ammonium chloride. The allyldimethyl dehydroabietyl ammonium chloride is a cationic surfactant containing unsaturated active C=C double bond and dehydroabietylamine structure. The method comprises the following steps: dissolving dehydroabietylamine in an ethanol-acetonitrile composite solvent, and reacting with formic acid and formaldehyde to obtain N,N-dimethyldehydroabietylamine; in the presence of a composite polymerization inhibitor composed of 2,2,6,6-tetramethylpiperidin-1-yl)oxyl (TEMP), p-hydroxyanisole and hydroquinone in a mass ratio of (0.01-10):(0.01-100):(0.01-10), reacting allyl chloride and the N,N-dimethyldehydroabietylamine at 10-90 DEG C for 5-120 hours to obtain crude allyldimethyl dehydroabietyl ammonium chloride; and finally, recrystallizing by using a composite solvent composed of chloroform, ethyl acetate, aether, dioxane and tetrahydrofuran in a mass ratio of (0.01-10):(0.001-12):(0.1-10):(0.001-16):(0.001-18), and carrying out vacuum drying to obtain the allyldimethyl dehydroabietyl ammonium chloride product of which the mass percentage is greater than 90%.

Description

technical field [0001] The method for preparing allyl dimethyl dehydroabietyl ammonium chloride involved in the present invention is a novel method for preparing cationic surfactants containing dehydroabietamine structure in the field of forestry chemical industry in surfactant chemistry . Background technique [0002] Rosin is a substance obtained from the fractionation of pine resin, which is the secretion of pine trees, and it is also a renewable natural resource. As a chemical raw material, rosin has the characteristics of abundant sources and low price. The main component of rosin is a resin acid with a three-membered phenanthrene ring structure composed of abietic acid, long-leaved abietic acid and neoabietic acid. Because there are not only carboxyl groups but also unsaturated carbon-carbon double bonds in the structures of these resin acids, they can be converted into rosin derivatives such as abietamine, dehydroabietamine, and abietol through chemical modification...

Claims

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Application Information

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IPC IPC(8): C07C211/63C07C209/08
Inventor 蔡照胜朱雪梅商士斌裴立军徐大雄张怀红赵玲玲郁桂云
Owner YANCHENG INST OF TECH
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