CN104084090A - Method for preparing surfactant by taking rosin as raw material - Google Patents

Abstract

The invention discloses a method for preparing a surfactant by taking rosin as a raw material, belonging to the technical field of rosin deep processing. The method comprises the following steps: firstly, reacting the rosin, ethanol and zinc oxide in a reaction kettle; then, adding fumaric acid and hydroquinone and reacting; next, adjusting the pH value to be within the range of 6 to 8, and adding epoxy chloropropane and dimethylamine and reacting; and finally, carrying out mixing and refluxing on the product obtained by the reaction and ethanol to obtain the surfactant. According to the method, the surfactant is prepared by directly taking the rosin which is low in cost as the raw material, and meanwhile, adopting corresponding preparation steps and preparation conditions, and according to the preparation method, the cost is low; the surfactant product is high in comprehensive performance.

Description

Method taking rosin as preparing surfactant

Technical field

The invention belongs to rosin deep process technology field, relate in particular to a kind of method taking rosin as preparing surfactant.

Background technology

Rosin is a kind of natural reproducible resource, due to its aboundresources, and low price and being paid close attention to widely, its deep processed product is widely used in each department of daily life.Because the luxuriant and rich with fragrance structure of the ring of three in rosin molecular structure has good oleophylic performance, after being connected with hydrophilic radical, can be used as good surfactant, and because the hydrophobic performance of rosin is stronger, rosin connects the compound obtaining after hydrophilic group and there is very strong some surface active property, so can be used for making surfactant.Its preparation method is generally that purchase rosin deep processed product dehydrogenated rosin or disproportionated rosin are that raw material is made surfactant.But because the price of rosin deep processed product dehydrogenated rosin or disproportionated rosin is high, cause its overall production cost also very high, be unfavorable for the development of enterprise.

Summary of the invention

The technical problem that the present invention solves is to provide a kind of directly method taking rosin as preparing surfactant, and the cost of the rosin-based surfactant that the method makes is low.

In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:

A method taking rosin as preparing surfactant, the method comprises the following steps:

A. under stirring condition, by the rosin of 30 weight portion～35 weight portions, the zinc oxide of the ethanol of 45 weight portion～50 weight portions and 0.1 weight portion～1 weight portion is put into reactor, first mixes at 100 DEG C～120 DEG C, then be warming up to 130 DEG C～140 DEG C, react 1 hour～2 hours; Then be warming up to again 180 DEG C～210 DEG C, react 4 hours～6 hours;

After B.A step, continue, under stirring condition, in described reactor, to add the fumaric acid of 60 weight portion～65 weight portions and the hydroquinones of 0.02 weight portion～0.03 weight portion, be then cooled to 90 DEG C～105 DEG C, insulation reaction 0.5 hour～1 hour;

After C.B step, continue under stirring condition, in described reactor, add NaOH, make the pH value of reaction mass in 6～8 scope, then add the epoxychloropropane of 100 weight portion～110 weight portions and the dimethylamine of 20 weight portion～30 weight portions, be cooled to 50 DEG C～65 DEG C, insulation reaction 2 hours～4 hours, discharging, obtains intermediate product;

After D.C step, the intermediate product obtaining is mixed with the ethanol of 80 weight portion～90 weight portions, at 55 DEG C～65 DEG C, reflux 5 hours～6 hours, obtain this surfactant.

Owing to adopting technique scheme, the beneficial effect that the present invention obtains is:

The present invention taking low-cost rosin as raw material, adopts corresponding preparation process and preparation condition to make surfactant by directly simultaneously, makes this preparation method's cost low, the good combination property of its surfactant product.

Detailed description of the invention

Below in conjunction with specific embodiment, the invention will be further described, and protection scope of the present invention is not only confined to following examples.

Embodiment 1

This method taking rosin as preparing surfactant comprises the following steps:

A. under stirring condition, by 30kg rosin, 45kg ethanol and 0.1kg zinc oxide are put into reactor, first mix at 100 DEG C, are then warming up to 130 DEG C, react 1 hour; Then be warming up to again 180 DEG C, react 4 hours;

After B.A step, continue, under stirring condition, in described reactor, to add 60kg fumaric acid and 0.02kg hydroquinones, be then cooled to 90 DEG C, insulation reaction 0.5 hour;

After C.B step, continue, under stirring condition, in described reactor, to add NaOH, the pH value that makes reaction mass is 6, then adds 100kg epoxychloropropane and 20kg dimethylamine, is cooled to 50 DEG C, insulation reaction 2 hours, and discharging, obtains intermediate product;

After D.C step, the intermediate product obtaining is mixed with 80kg ethanol, at 55 DEG C, reflux 5 hours, obtain this surfactant.

The critical micelle concentration of the surfactant that the present embodiment makes is 0.2mmol/L; Emulsifiability is 41min; Frothing capacity is 285mm.

Embodiment 2

This method taking rosin as preparing surfactant comprises the following steps:

A. under stirring condition, by 35kg rosin, 50kg ethanol and 1kg zinc oxide are put into reactor, first mix at 120 DEG C, are then warming up to 140 DEG C, react 2 hours; Then be warming up to again 210 DEG C, react 6 hours;

After B.A step, continue, under stirring condition, in described reactor, to add 65kg fumaric acid and 0.03kg hydroquinones, be then cooled to 105 DEG C, insulation reaction 1 hour;

After C.B step, continue, under stirring condition, in described reactor, to add NaOH, the pH value that makes reaction mass is 8, then adds 110kg epoxychloropropane and 30kg dimethylamine, is cooled to 65 DEG C, insulation reaction 4 hours, and discharging, obtains intermediate product;

After D.C step, the intermediate product obtaining is mixed with 90kg ethanol, at 65 DEG C, reflux 6 hours, obtain this surfactant.

The critical micelle concentration of the surfactant that the present embodiment makes is 0.3mmol/L; Emulsifiability is 44min; Frothing capacity is 290mm.

Embodiment 3

This method taking rosin as preparing surfactant comprises the following steps:

A. under stirring condition, by 32kg rosin, 48kg ethanol and 0.6kg zinc oxide are put into reactor, first mix at 110 DEG C, are then warming up to 135 DEG C, react 1.5 hours; Then be warming up to again 200 DEG C, react 5 hours;

After B.A step, continue, under stirring condition, in described reactor, to add 62kg fumaric acid and 0.025kg hydroquinones, be then cooled to 100 DEG C, insulation reaction 0.5 hour;

After C.B step, continue, under stirring condition, in described reactor, to add NaOH, the pH value that makes reaction mass is 7, then adds 105kg epoxychloropropane and 25kg dimethylamine, is cooled to 60 DEG C, insulation reaction 3 hours, and discharging, obtains intermediate product;

After D.C step, the intermediate product obtaining is mixed with 85kg ethanol, at 60 DEG C, reflux 5.5 hours, obtain this surfactant.

The critical micelle concentration of the surfactant that the present embodiment makes is 0.25mmol/L; Emulsifiability is 45min; Frothing capacity is 280mm.

Claims (1)

1. the method taking rosin as preparing surfactant, is characterized in that comprising the following steps:

A. under stirring condition, by the rosin of 30 weight portion～35 weight portions, the zinc oxide of the ethanol of 45 weight portion～50 weight portions and 0.1 weight portion～1 weight portion is put into reactor, first mixes at 100 DEG C～120 DEG C, then be warming up to 130 DEG C～140 DEG C, react 1 hour～2 hours; Then be warming up to again 180 DEG C～210 DEG C, react 4 hours～6 hours;

After B.A step, continue, under stirring condition, in described reactor, to add the fumaric acid of 60 weight portion～65 weight portions and the hydroquinones of 0.02 weight portion～0.03 weight portion, be then cooled to 90 DEG C～105 DEG C, insulation reaction 0.5 hour～1 hour;

After C.B step, continue under stirring condition, in described reactor, add NaOH, make the pH value of reaction mass in 6～8 scope, then add the epoxychloropropane of 100 weight portion～110 weight portions and the dimethylamine of 20 weight portion～30 weight portions, be cooled to 50 DEG C～65 DEG C, insulation reaction 2 hours～4 hours, discharging, obtains intermediate product;

After D.C step, the intermediate product obtaining is mixed with the ethanol of 80 weight portion～90 weight portions, at 55 DEG C～65 DEG C, reflux 5 hours～6 hours, obtain this surfactant.