Preparation method for resin curing agent N-acetoacetyl morpholine

A technology of acetoacetylmorpholine and resin curing, applied in organic chemistry and other directions, to achieve the effects of high product purity, simple separation and purification process, and short reaction time

Inactive Publication Date: 2014-05-28
南通惠康国际企业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although N-acetoacetylmorpholine has been used for a long time, the domestic literature on the synthesis of N-acetoacetylmorpholine has not been reported. Therefore, the preparation method of N-acetoacetylmorpholine has important industrial application value.

Method used

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  • Preparation method for resin curing agent N-acetoacetyl morpholine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] In a 250mL four-necked flask, add 50g of solvent, 17.4g of morpholine, 0.4g of polymerization inhibitor, and 17.7g of diketene, install a reflux condenser and a thermometer, start the stirrer, control the temperature at 85-100°C, and the reaction time is 6 -10h, after the reaction is over, distill off most of the solvent under normal pressure, and distill the remaining organic phase under reduced pressure, first distill off the remaining solvent and unreacted raw materials, and then collect the fraction at 114-116°C / 1.65kPa , to obtain the N-acetoacetylmorpholine product, and the product yield is 93.51%.

Embodiment 2

[0015] In a 250mL four-necked flask, add 50g of solvent, 17.4g of morpholine, 0.5g of inhibitor, and 21g of diketene, install a reflux condenser, a thermometer, start the stirrer, control the temperature at 85-100°C, and the reaction time is 6- After 12 hours, after the reaction, most of the solvent was distilled off under normal pressure, and the remaining organic phase was distilled off under reduced pressure. First, the remaining solvent and unreacted raw materials were distilled off, and then the fraction at 114-116°C / 1.65kPa was collected. The N-acetoacetylmorpholine product was obtained, and the product yield was 93.92%.

Embodiment 3

[0017] In a 250mL four-neck flask, add 50g of solvent, 17.4g of morpholine, 0.7g of polymerization inhibitor, and 21g of diketene, install a reflux condenser and a thermometer, start the stirrer, control the temperature at 85-100°C, and the reaction time is 6- After 12 hours, after the reaction, most of the solvent was distilled off under normal pressure, and the remaining organic phase was distilled off under reduced pressure. First, the remaining solvent and unreacted raw materials were distilled off, and then the fraction at 114-116°C / 1.65kPa was collected. The N-acetoacetylmorpholine product was obtained, and the product yield was 93.12%.

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Abstract

The invention discloses a preparation method for a resin curing agent N-acetoacetyl morpholine. The N-acetoacetyl morpholine is prepared by using diketene and morpholine as raw materials under the condition with a solvent and a polymerization inhibitor. According to the method, diketene and morpholine are used to synthesize N-acetyl acetyl morpholine, the processes of separation and purification are simple, the reaction time is short, the yield of the product can reach more than 93%, the purity of the product is high, energy consumption is low, environmental pollution is little, the cost is low, and the method is a relatively ideal process for realizing industrialized production.

Description

technical field [0001] The invention relates to a method for preparing a resin curing agent N-acetoacetylmorpholine. Background technique [0002] N-Acetoacetylmorpholine. It can be used as a curing agent for unsaturated polyester resins and acrylic resins. Polyalcohol resins are usually cured by using methyl ethyl ketone peroxide as a curing agent and organic cobalt as an accelerator. However, when the amount of cobalt increases in the boiling test, or yellowing occurs during use, it will affect the appearance. However, when N-acetoacetylmorpholine is used as a curing agent, the amount of cobalt is greatly reduced, and it does not affect the curing of the resin and does not change color. The finished product is close to colorless and transparent. Using this normal temperature curing resin can improve the artificial marble and The appearance quality of the bathtub. Its molecular formula is C 8 h 13 NO 3 , molecular weight: 171.19, molecular structure formula: [0003]...

Claims

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Application Information

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IPC IPC(8): C07D295/185
CPCC07D295/185
Inventor 王树清王歆然杜承贤祁云
Owner 南通惠康国际企业有限公司
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