Preparation method of antistatic agent onium salt fluoride

A technology of antistatic agent and onium salt, applied in the field of preparation of antistatic agent onium fluoride salt, can solve the problems of affecting yield, large amount of deionized water, long time consumption, etc., and achieves high production efficiency and short time consumption , the effect of simple process

Inactive Publication Date: 2012-09-12
HUNAN HONGYUE CHEM MFG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing onium fluoride salts using tap water to solve the problems of long time consumption, large amount of deionized water, and dissolving after repeated washing. A part of onium fluoride salt affects the yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Mix 33.9 g of potassium perfluorobutane sulfonate and 33.9 g of tetrabutylphosphine bromide, dissolve in 100 mL of tap water at 70°C, stir for 30 minutes, let stand to separate layers, and decant to remove The water-containing material in the upper layer is obtained as the lower liquid phase insoluble in water; (2) at a temperature of 70 °C, add the same volume of tap water as the lower liquid phase to wash the lower liquid phase once; (3) after cooling, dissolve the lower liquid phase with methanol , add 10 g of strong-acid styrene-based cation exchange resin, stir for 10 minutes, filter, then add 10 g of strong-base acrylic anion-exchange resin, stir for 10 minutes, and filter; (4) Distill methanol to obtain the product onium fluoride Salt 54.8 g (yield 98.2%).

[0021] The melting point of the product onium fluoride salt was measured to be 73.4° C. by a differential thermal scanning analyzer (DSC). The quality comparison of the product washed once with tap water...

Embodiment 2

[0024] (1) Mix 33.9 g of potassium perfluorobutane sulfonate and 33.9 g of tetrabutylphosphine bromide, dissolve in 100 mL of tap water at 75°C, stir for 28 minutes, let stand to separate layers, and decant to remove (2) At a temperature of 75 °C, add tap water of the same volume as the lower layer to wash twice; (3) After cooling, dissolve the lower liquid phase with methanol, add 10 g strong-acid styrene-based cation-exchange resin, stirred for 12 minutes, filtered, then added 10 g of strong-base acrylic-based anion-exchange resin, stirred for 12 minutes, filtered; (4) distilled methanol to obtain 54.6 g of onium fluoride salt (Yield 97.8%).

[0025] The melting point of the product onium fluoride salt was measured to be 74.1 °C by differential scanning calorimeter (DSC). The quality comparison of the product washed once with tap water and the final product is as follows:

[0026] project Potassium ion / ppm Magnesium ion / ppm Calcium ion / ppm Chloride / ppm ...

Embodiment 3

[0028] (1) Mix 1.0 kg potassium perfluorobutane sulfonate with 1.0 kg tetrabutylphosphine bromide, dissolve in 1500 mL tap water at 68°C, stir for 35 minutes, let stand to separate layers, and decant to remove (2) At 68°C, add tap water of the same volume as the lower layer to wash once; (3) After cooling, dissolve the lower liquid phase with methanol and add 300 g strong-acid styrene-based cation-exchange resin, stirred for 15 minutes, filtered, then added 300 g of strong-base acrylic-based anion-exchange resin, stirred for 15 minutes, filtered; (4) distilled off methanol to obtain 1.63 kg of onium fluoride salt (Yield 98.8%).

[0029] The melting point of the product onium fluoride salt was 74.3 °C as measured by a differential scanning calorimeter (DSC). The quality comparison of the product washed once with tap water and the final product is as follows:

[0030] project Potassium ion / ppm Magnesium ion / ppm Calcium ion / ppm Chloride / ppm Bromide / ppm Sul...

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Abstract

The invention relates to a preparation method of antistatic agent onium salt fluoride, which comprises the following steps: (1) adopting tap water as a solvent and carrying out ion association reaction on perfluorobutane metal sulfonate and halogenated tetrabutyl onium salt at a temperature of 60-80 DEG C; standing and layering, and decantating an upper layer of water-containing material; obtaining a lower layer of liquid phase which is insoluble in water; (2) washing the lower layer of liquid phase by using tap water with the same volume as the lower layer of liquid phase at a temperature of 60-80 DEG C for 1-2 times; (3) adsorbing inorganic ions in the lower layer of liquid phase by using ion exchange resin; dissolving the lower layer of liquid phase by using methanol, adding strongly-acidic type styrene cation exchange resin of which the crosslinking degree is 25 percent, agitating and filtering; and then adding strongly-basic type crylic acid type anion exchange resin with strong water absorption, agitating and filtering; (4) steaming out methanol to obtain the onium salt fluoride of which foreign ions reach the standards. The preparation method has the advantages of simple process, energy conservation, emission reduction, high yield and the like.

Description

technical field [0001] The invention relates to a preparation method of an antistatic agent onium fluoride salt, in particular to a method of tetrabutylium perfluorobutylsulfonate. Background technique [0002] Common synthetic polymers are not good conductors. Due to the accumulation of static charges, dust and impurities tend to be easily adsorbed on their surfaces, causing other difficulties in their processing and application. In order to avoid this electrostatic effect, a small amount of antistatic agent is usually added to the polymer. Onium fluoride salt has been found to be an excellent antistatic agent, mainly used in PS and ABS materials, and also used in plastic products such as PE, PP, PVC, PC, PET, etc. The antistatic effect is remarkable and long-lasting. [0003] The method of preparing antistatic agent onium fluoride salt reported and used in domestic and foreign patent literature is mainly to use deionized water as solvent, make perfluorobutyl metal sulfona...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/06C07C303/32C07F9/54
Inventor 孙胜培欧阳杰苏凯洲王雄伟孙晓光颜小雄
Owner HUNAN HONGYUE CHEM MFG
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