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Method for preparing ethoxyabietic amine by spraying process

A technology of rosin amine polyoxyethylene ether and spray method, which is applied in the field of chemical additives, can solve the problems of incomplete conversion of polymerization reactants, small polymerization reaction space, poor quality of finished products, etc., and achieve stable physical and chemical performance indicators and high reaction efficiency. The effect of shortening the time and complete response

Inactive Publication Date: 2008-02-13
吴金海
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, the conversion of the polymerization reactants of rosin amine and ethylene oxide is incomplete, the polymerization reaction space is small, the polymerization reaction is greatly affected by the material, and the product contains more free amines such as viscous primary and secondary amines, and the reaction is incomplete. , incomplete
And the reaction time is longer, and the quality of the finished product is poor
After the rosin amine polyoxyethylene ether prepared by the stirring method is compounded with other surfactants, a lot of flocs will be produced, and the compatibility stability is poor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The first step, inhale 580kg of disproportionated rosinamine in a 2000L spray reactor, when heated to 50°C, inhale 1.5kg of 70% (wt) phosphorous acid, heat up to 170°C while vacuuming, and control the pressure in the kettle to 0.3Mpa , close the vacuum valve, turn on the magnetic circulation pump, the material is sucked out of the kettle and then sprayed into the kettle, and the valve for ethylene oxide is opened, and the material and ethylene oxide are simultaneously sprayed out from the multi-group combination nozzles of the spray reactor. Spray reaction was carried out in the upper space of the kettle, and the reaction was circulated for 1.2 hours. The amount of ethylene oxide added was 120 kg. After the reaction was completed, it was kept for 30 minutes and cooled to 95 ° C;

[0016] Second step, vacuumize in above-mentioned spray reactor, while inhaling 50% (wt) potassium hydroxide 4kg, be warming up to 125 ℃, keep warm for more than 30 minutes, continuously replace...

Embodiment 2

[0018] The first step, inhale 580kg of disproportionated rosinamine in a 2000L spray reactor, when heated to 60°C, inhale 1.5kg of 70% (wt) phosphorous acid, heat up to 180°C while vacuuming, and control the pressure in the kettle to 0.2Mpa , close the vacuum valve, turn on the magnetic circulation pump, the material is sucked out from the kettle and then sprayed into the kettle, and the valve for ethylene oxide is opened, and the material and ethylene oxide are simultaneously sprayed out from the multi-group nozzles of the spray reactor , carry out the spray reaction in the upper space of the kettle, such a circular reaction for 0.8 hours, the addition of ethylene oxide is 240kg, the reaction is completed and kept for 35 minutes, and cooled to 100 ° C;

[0019] Second step, in the above-mentioned spray reactor, vacuumize while sucking 50% (wt) of potassium hydroxide 4kg, while heating up to 130°C, keep warm for more than 40 minutes, replace the air in the still with nitrogen f...

Embodiment 3

[0021] The first step, inhale 480kg of disproportionated rosinamine in a 2000L spray reactor, when heated to 55°C, 1.5kg of 70% (wt) phosphorous acid, heat up to 175°C while vacuuming, control the pressure in the kettle to 0.25Mpa, Close the vacuum valve, turn on the magnetic circulation pump, the material is sucked out of the kettle and then sprayed into the kettle, and the valve for ethylene oxide is opened, and the material and ethylene oxide are simultaneously sprayed out from the multi-group combination nozzles of the spray reactor. Spray reaction was carried out in the upper space of the kettle, and the reaction was circulated for 1.5 hours. The amount of ethylene oxide added was 360kg. After the reaction was completed, it was kept for 40 minutes and cooled to 90°C;

[0022] Second step, vacuumize in above-mentioned spray reaction kettle, while inhaling 50% (wt) potassium hydroxide 4kg, be warming up to 120 ℃, keep warm for more than 40 minutes, continuously replace the a...

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Abstract

The invention relates to a method for preparing rosin amine polyoxyethylene ether by spraying method. The reaction is divided into two steps: the first step is to inhale disproportionated rosin amine into a spray reactor, and when heated to 50-60°C, inhale phosphorous acid and pump while Raise the temperature to 170-180°C under vacuum, control the pressure in the kettle to 0.2-0.3Mpa, close the vacuum valve, turn on the magnetic circulation pump, the material is sucked out from the kettle and then sprayed into the kettle, and the valve of ethylene oxide is opened, the material and epoxy Ethane is sprayed out at the same time, such a circular reaction for 0.8-1.5 hours, heat preservation for 30-40 minutes, and cooling to 90-100 °C; the second step is to vacuumize the inside of the above-mentioned kettle, while inhaling potassium hydroxide, while raising the temperature to 120- 130°C, keep warm for more than 20 minutes, replace the air in the kettle with nitrogen, raise the temperature to 165-175°C, close the vacuum valve, turn on the magnetic circulation pump, and spray the material and the remaining ethylene oxide into the spray reactor at the same time, so that the cycle reaction is 1 -2 hours, keep warm for more than 40 minutes. The method of the invention has short reaction time, complete reaction and good compatibility with other surfactants.

Description

technical field [0001] The invention relates to a method for preparing rosin amine polyoxyethylene ether by spraying. It belongs to the technical field of chemical additives. Background technique [0002] Rosin amine polyoxyethylene ether is widely used in chemical production as emulsifier. At present, most of the preparation methods of rosin amine polyoxyethylene ether adopt stirring method: it is prepared by addition reaction of disproportionated rosin amine and ethylene oxide in a stirred reactor. Catalysts are basic catalysts and acidic catalysts. In this method, the conversion of the polymerization reaction product of rosin amine and ethylene oxide is incomplete, the polymerization reaction space is small, the polymerization reaction is greatly affected by the material, and the product contains more free amines such as viscous primary and secondary amines, and the reaction is incomplete. , Not thorough. And the reaction time is longer, and the finished product quali...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/26C08G65/333
Inventor 吴金海
Owner 吴金海
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