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A kind of preparation method of acryloyl morpholine

A technology for acryloyl morpholine and morpholine, which is applied in the field of preparing acryloyl morpholine by a single-container method, can solve the problems of serious skin contact or inhalation hazards, difficult separation, hidden safety hazards, etc., and achieves low cost, simple operation, and side reactions. less effect

Active Publication Date: 2018-01-05
TIANJIN JIURI NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] However, this method uses highly toxic dimethyl sulfate, which is seriously harmful in skin contact or inhalation, and has great potential safety hazards in the industrial production process.
[0011] Another method is US2683703, US4959364, CN 1345302, He Kaiyu, etc., and the method disclosed in the Proceedings of the 25th Annual Meeting of Gansu Chemical Society, etc., is also a method commonly used in China now, through acrylic acid to generate acryloyl chloride, and the obtained acryloyl chloride The two-step method of reacting with morpholine to generate acryloylmorpholine has the advantage of simple process flow, but the disadvantage is that the method has many by-products, low yield and difficult separation

Method used

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  • A kind of preparation method of acryloyl morpholine
  • A kind of preparation method of acryloyl morpholine
  • A kind of preparation method of acryloyl morpholine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: Preparation of acryloylmorpholine

[0035] In a four-necked flask equipped with a spherical condenser and a stirrer, add 1g p-hydroxyanisole, 21.6g (0.3mol) acrylic acid and 17.7g (0.13mol) phosphorus trichloride, and add 50ml dichloromethane as a solvent , Lower the temperature to 0°C, add 57.4g (0.66mol) of morpholine (previously dissolved in 30ml of dichloromethane) into the reaction solution, slowly add dropwise, control the reaction temperature at 0~5°C, and finish the dropwise addition in 3.5 hours. Incubate the reaction for 1 hour, filter, and spin-dry the solvent to obtain 38 g of crude product, with a GC analysis content of 91%, and vacuum distillation to obtain 34 g with a yield of 81% and a GC content of 99%.

Embodiment 2

[0036] Example 2: Preparation of acryloylmorpholine

[0037] In a four-necked flask equipped with a spherical condenser and stirrer, add 1g phenothiazine, 21.6g (0.3mol) acrylic acid and 17.7g (0.13mol) phosphorus trichloride, and add 50ml of dichloromethane as a solvent to cool down To 0°C, add 57.4g (0.66mol) morpholine (dissolved in 30ml of dichloromethane in advance) to the reaction solution dropwise, slowly add dropwise, control the reaction temperature at 0~5°C, the dropwise addition is over in 3.5 hours, and the reaction is kept warm After 1h, filter and spin-dry the solvent to obtain 37.8g of crude product, GC analysis content is 90%, vacuum distillation obtains 33.2g, yield is 79%, GC content is 99%.

Embodiment 3

[0038] Example 3: Preparation of acryloylmorpholine

[0039] In a four-necked flask equipped with a spherical condenser and stirrer, add 1g p-hydroxyanisole, 21.6g (0.3mol) acrylic acid and 8.3g (0.06mol) phosphorus trichloride, and add 50ml of dichloromethane as a solvent , Lower the temperature to 0°C, add 57.4g (0.66mol) of morpholine (previously dissolved in 30ml of dichloromethane) into the reaction solution, slowly add dropwise, control the reaction temperature at 0~5°C, and finish the dropwise addition in 3.5 hours. Incubate the reaction for 1 hour, filter, and spin-dry the solvent to obtain 38 g of crude product, with a GC analysis content of 92%, and vacuum distillation to obtain 33.6 g, with a yield of 80% and a GC content of 99%.

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Abstract

The invention provides a method for preparing acryloyl morpholine according to a single-container method, and aims to overcome the detects of low yield, high reaction complexity, cumbersome operation and the like. The method provided by the invention has the advantages that the reaction steps are less, and thus the operation is simple; the side reactions are less, and thus the yield is high and the purification is easy; the requirement on reaction equipment of reaction processes is low; corrosion of the reaction equipment is avoided; the environment is protected as generation of the acidic gas hydrogen chloride is avoided; the cost is low; the suitability for industrialized production is high; the superiority to the prior art is considerable.

Description

Technical field [0001] The content of the present invention relates to a preparation method of acryloyl morpholine, in particular to a method for preparing acryloyl morpholine by a single container method. Background technique [0002] N-acryloyl morpholine is a functional monomer and reactive diluent with excellent performance. Due to its double bond and morpholine group, it has relatively active chemical properties (high sensitivity) and does not produce any pungent odor (extremely odorous). Low), and has the characteristics of low viscosity, fast curing, and strong dilution ability. The UV and EB curable resin modified with N-acryloylmorpholine has very low moisture absorption, and has good acid, alkali and solvent resistance. Products modified with N-acryloylmorpholine as raw materials are used in oilfield additives, ink additives, papermaking additives and adhesives. Acrylmorpholine can also be used as a new type of water-soluble polymer monomer or as a comonomer modified ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/185
CPCC07D295/185
Inventor 张齐武瑞毛桂红罗想赵国锋
Owner TIANJIN JIURI NEW MATERIALS CO LTD