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One-step preparation method and application of propargyl alcohol ethoxylate

A technology of ethoxylate and propynyl alcohol, which is applied in the field of nickel plating brightener, can solve the problems that cannot be solved well, and achieve the effect of overcoming the deep color

Inactive Publication Date: 2019-01-11
WUHAN OXIRAN SPECIALTY CHEM CO +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Compared with the patents mentioned above, none of them can solve the problems of safety or green one-step synthesis that actually exist in the production process, and the traditional technology faces many limitations.

Method used

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  • One-step preparation method and application of propargyl alcohol ethoxylate
  • One-step preparation method and application of propargyl alcohol ethoxylate
  • One-step preparation method and application of propargyl alcohol ethoxylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 5mol of propynyl alcohol and 5g of tetramethylammonium hydroxide into a 1L stirred autoclave, and check the airtightness of the reactor. Carry out nitrogen replacement and vacuuming operations to ensure that the vacuuming time is greater than 30 minutes. The number of high-purity nitrogen replacement operations is 5 times, and the pressure is exhausted to 0-30KPa. Then, ethylene oxide is introduced into the reaction kettle, and the reaction temperature is controlled at 85 ° C ± 3°C and the reaction pressure is 0.3MPa~0.5MPa, until the total amount of ethylene oxide fed is 10mol, stop feeding ethylene oxide, and carry out post-treatment aging on the product to maintain the temperature of the reactor at 85°C±3°C, Until the pressure of the reactor no longer drops, it indicates that the aging reaction is completed. Decrease to 60°C and neutralize with glacial acetic acid.

[0035] The prepared propynyl alcohol ethoxylate was used as a brightener for nickel plating, and...

Embodiment 2

[0037]Add 5mol of propynyl alcohol and 5g of tetramethylammonium hydroxide and tetraethylammonium hydroxide mixture (mixture mass ratio is 1:3) in the autoclave with stirring of 1L, the airtightness inspection is carried out to reaction kettle, wait for After there is no pressure drop in the reactor within 1 hour, carry out nitrogen replacement and vacuuming operations at 50°C to ensure that the vacuuming time is greater than 30 minutes, and the number of high-purity nitrogen replacement operations is 5 times, and the pressure is discharged to 0-30KPa, and then to Feed ethylene oxide into the reaction kettle, control the reaction temperature at 85°C±3°C and the reaction pressure at 0.3MPa~0.5MPa, stop feeding ethylene oxide until the total amount of ethylene oxide fed is 10mol, Perform post-treatment aging on the product and maintain the temperature of the reactor at 85°C±3°C until the pressure of the reactor no longer drops, indicating that the aging reaction is completed. Lo...

Embodiment 3

[0040] Add 5mol of propynyl alcohol and 5g of tetraethylammonium hydroxide into a 1L stirred autoclave, and check the airtightness of the reactor. Carry out nitrogen replacement and vacuuming operations to ensure that the vacuuming time is greater than 30 minutes. The number of high-purity nitrogen replacement operations is 5 times, and the pressure is exhausted to 0-30KPa. Then, ethylene oxide is introduced into the reaction kettle, and the reaction temperature is controlled at 85 ° C ± 3°C and the reaction pressure is 0.3MPa~0.5MPa, until the total amount of ethylene oxide fed is 10mol, stop feeding ethylene oxide, and carry out post-treatment aging on the product to maintain the temperature of the reactor at 85°C±3°C, Until the pressure of the reactor no longer drops, it indicates that the aging reaction is completed. Lower to 60°C, neutralize with glacial acetic acid and remove from low boil.

[0041] The prepared propynyl alcohol ethoxylate was used as a brightener for n...

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Abstract

The invention discloses a one-step preparation method and application of propargyl alcohol ethoxylate. Propargyl alcohol ethoxylate is prepared from propargyl alcohol and ethylene oxide through synthesis. The method specifically comprises the steps of adding propargyl alcohol and a quaternary ammonium alkali catalyst into a reaction kettle, carrying out nitrogen displacement and vacuumizing for several times, introducing ethylene oxide, controlling the reaction temperature at 82-88 DEG C and the reaction pressure at 0.3MPa-0.5MPa, carrying out after-treatment ageing on the product, maintainingthe temperature of the reaction kettle until the pressure of the reaction kettle no longer decreases, cooling to 60 DEG C, then neutralizing by virtue of glacial acetic acid, and removing low-boiling-point substances. Propargyl alcohol ethoxylate prepared by virtue of the one-step preparation method has lots of advantages of high conversion rate and acetylene bond retention rate, light color andthe like, and an original required distillation purification manner can be replaced, so that the amount of waste is greatly reduced, and compared with preparation methods in the prior art, the one-step preparation method is relatively environment-friendly. By applying propargyl alcohol ethoxylate to an electronickelling process, an obtained plating layer is plump, and a skip plating phenomenon isbasically avoided.

Description

technical field [0001] The invention relates to the technical field of nickel-plating brighteners, in particular to a one-step preparation method and application of propynyl alcohol ethoxylates. Background technique [0002] Brighteners have been developed for decades and are used as one of the additive components of electroless plating and electroplating. It can make the coating uniform and improve the decoration of the plated parts. In terms of protection performance, it can improve the corrosion resistance of the product and increase the service life. In terms of functionality, it can improve the wear resistance and lubrication performance of the workpiece and other special functions. [0003] Brighteners are divided into macroscopic dispersion ability improvers (smoothing agents), microscopic dispersion ability improvers (leveling agents), wetting agents, modifiers (functional additives), masking agents, and auxiliary agents according to different functions. The funct...

Claims

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Application Information

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IPC IPC(8): C25D3/16
CPCC25D3/16
Inventor 任凡王亮王杰张静刘治田张旗耿聪付远波程宝
Owner WUHAN OXIRAN SPECIALTY CHEM CO
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