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Method for preparing trimethylolpropane-tri (1-aziridinyl) propionate

A technology of trimethylolpropane and aziridine group, which is applied in the field of preparation of trimethylolpropane-tris(1-aziridine) propionate, and can solve the problems of temporary protection and application without precision products.

Inactive Publication Date: 2016-12-07
NANCHANG HANGKONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Waterborne polyurethane dispersions have been widely used in leather, textiles, furniture, plastics, automobiles, etc. Temporary protection of the product is applied

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] (1) Mix 72 grams of acrylic acid and 32 grams of trimethylolpropane, then add 1.8-2.5 grams of cerium sulfate, 0.4 grams of hydroquinone, and 60 grams of toluene in sequence, and stir evenly;

[0015] (2) Heating to 50-55°C while stirring, then blowing in air for about 2 hours, then heating to 80-85°C and reflux reaction for about 4 hours, keeping stirring throughout the process;

[0016] (3) After cooling to 60 °C, add 45 ml of water, stir for 20 minutes, then let it stand for more than 15 minutes, and remove the lower liquid after layering;

[0017] (4) For the upper liquid, first wash with 15% (mass parts) sodium hydroxide solution for 2 to 3 times, then wash with saturated sodium chloride solution for 2 to 3 times, and finally wash with water for 2 to 3 times;

[0018] (5) After heating to about 60-65 ℃ for 30 minutes, add 0.1 g of hydroquinone, and rotary steam for 30 minutes to obtain a light yellow transparent liquid;

[0019] (6) Take 60 grams of light yellow t...

Embodiment 2

[0023] (1) Mix 360 grams of acrylic acid and 160 grams of trimethylolpropane, add 9.0-12.5 grams of cerium sulfate, 2.0 grams of hydroquinone, and 300 grams of toluene;

[0024] (2) After heating to 50-55 °C while stirring, air is introduced for about 2 hours; then heated to 80-85 °C for about 4 hours under reflux;

[0025] (3) After cooling to 60 °C, add 225 ml of water, stir for 20 minutes, then let stand for more than 15 minutes, and remove the lower liquid after layering;

[0026] (4) For the retained upper liquid, first wash with 15% (mass parts) sodium hydroxide solution for 2 to 3 times, then wash with saturated sodium chloride solution for 2 to 3 times, and finally wash with water for 2 to 3 times;

[0027] (5) After heating to about 60-65 ℃ for 30 minutes, add 0.5 g of hydroquinone, and rotary steam for 30 minutes to obtain a light yellow transparent liquid;

[0028] (6) Take 300 grams of light yellow transparent liquid and place it in an environment of 10°C (water b...

Embodiment 3

[0032] (1) Mix 180 grams of acrylic acid and 80 grams of trimethylolpropane, add 4.5-6.0 grams of cerium sulfate, 1.0 grams of hydroquinone, and 150 grams of toluene;

[0033] (2) After heating to 50-55 °C while stirring, air is introduced for about 2 hours; then heated to 80 °C and refluxed for about 4 hours;

[0034] (3) After cooling to 60 °C, add 112 ml of water, stir for 20 minutes, then let stand for more than 15 minutes, and remove the lower liquid after layering;

[0035] (4) For the retained upper liquid, first wash with 15% (mass parts) sodium hydroxide solution for 2 to 3 times, then wash with saturated sodium chloride solution for 2 to 3 times, and finally wash with water for 2 to 3 times;

[0036] (5) After heating to about 60-65 ℃ for 30 minutes, add 0.25 g of hydroquinone, and rotary steam for 30 minutes to obtain a light yellow transparent liquid;

[0037] (6) Put 100 grams of light yellow transparent liquid in an environment of 10°C (water bath or ice bath), ...

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PUM

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Abstract

The invention discloses a method for preparing trimethylolpropane-tri (1-aziridinyl) propionate. The method comprises the following steps: mixing trimethylolpropanewith acrylic acid, and adding cerium sulphate, hydroquinone and toluene; stirring, heating, subjecting to a refluxing reaction, adding water to stir and keeping stand, removing a lower-layer liquid after layering, keeping an upper-layer liquid, washing with a sodium hydroxide solution, washing with a saturated sodium chloride solution and finally washing with water; adding hydroquinone after heating, and obtaining a pale yellow transparent liquid by rotary evaporation, putting the pale yellow transparent liquid in a water bath,dropwise addingaziridineunder stirring, transferring to a brown bottle, and placing in the dark at room temperature to obtaintrimethylolpropane-tri (1-aziridinyl) propionate. The peel strength of apeelable protective film layer obtained from a cured aqueous polyurethane dispersion is 300 to 500 N / m.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a method for preparing trimethylolpropane-tris(1-aziridinyl) propionate, the organic compound is used for curing aqueous peelable polyurethane dispersion, and the cured film Layers are peelable. Background technique [0002] Polyurethane resins have excellent properties and are widely used in the fields of coatings and adhesives. Waterborne polyurethane resin has the advantages of environmental protection and energy saving and has become the development direction. Waterborne polyurethane resins are divided into three types: aqueous solution type, dispersion type and emulsion type. The waterborne polyurethane resins on the market are basically dispersion type and emulsion type. Waterborne polyurethane dispersions have been widely used in leather, textiles, furniture, plastics, automobiles, etc. Temporary protection of the product is applied. For example, polymethyl methacrylat...

Claims

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Application Information

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IPC IPC(8): C07D203/08C09D175/04C09D5/20C09D7/12
CPCC07D203/08C08K5/3412C09D5/20C09D7/63C09D175/04
Inventor 孟江燕傅念清王云英陈芳芳
Owner NANCHANG HANGKONG UNIVERSITY