Synthesizing method for preparing N-acryloyl morpholine

A technique for the synthesis of acryloylmorpholine and its synthesis method, which is applied in the field of synthesis of high-purity N-acryloylmorpholine, which can solve the problems of difficulty in obtaining raw materials, easy thermal polymerization of acryloylmorpholine, and difficult control of thermal cracking reactions, etc. Achieve the effect of less side reactions, low cost and easy control

Active Publication Date: 2010-11-03
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The raw materials of this method are difficult to obtain, and the thermal cracking reaction is not easy to control, and acryloylmorpholine is prone to thermal polymerization

Method used

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  • Synthesizing method for preparing N-acryloyl morpholine
  • Synthesizing method for preparing N-acryloyl morpholine
  • Synthesizing method for preparing N-acryloyl morpholine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 134 grams of acrylic acid to a 500ml reactor equipped with paddle stirring and a constant temperature water bath, start stirring, control the stirring speed at 80 rpm, raise the temperature to 30-35°C, and then use a constant pressure funnel to drop it within 0.5-1 hour. Add 86 grams of phosphorus trichloride (mass content 95%), the temperature will rise slowly during the dropping process, and the dropping rate is controlled so that the temperature during the dropping process does not exceed 45°C. After the dropwise addition, keep at 40-45°C for 3 hours. Separate the supernatant, then carry out rectification with a rectification tower, and the intermediate product acryloyl chloride is directly collected in a carbon tetrachloride constant pressure funnel equipped with 200 grams of solvent for subsequent use.

[0030] Add 121 grams of morpholine and 90 grams of solid powder of sodium carbonate, an acid-binding agent, into a 1L reaction kettle with a low-temperature wa...

Embodiment 2

[0032] Intermediate product solvated acryloyl chloride is prepared with embodiment 1

[0033] Add 121 grams of morpholine and 125 grams of acid-binding agent tripropylamine into a 1L reaction kettle with a low-temperature water bath in sequence, and the reaction kettle is emptied and equipped with a tail gas absorption device. Start the agitator, control the stirring speed at 100 rev / min, cool down to 0°C, then add the solvated acryloyl chloride dropwise through the constant pressure funnel, the dropwise addition is completed in 3 to 3.5 hours, and keep for another 3 hours; the temperature is controlled throughout the reaction process Between 0 and 5°C, then filter the supernatant. The supernatant after filtering is added to rectifying in the rectification under vacuum tower that 0.5 gram composite polymerization inhibitor (parahydroxyanisole 25%; Hydroquinone 25%; Cuprous chloride 50%) is housed, finally 124.7 g of N-acryloylmorpholine product with color number No. 20 (plati...

Embodiment 3

[0035] Add 335 grams of acrylic acid to a 1L reaction kettle equipped with paddle stirring and a constant temperature water bath, start stirring, control the stirring speed at 80 rpm, raise the temperature to 30-35°C, and then use a constant pressure funnel to drop it within 0.5-1 hour Add 215 grams of phosphorus trichloride (mass content 95%), the temperature will rise slowly during the dropping process, and the dropping rate is controlled so that the temperature during the dropping process does not exceed 45°C. After the dropwise addition, keep at 40-45°C for 3 hours. Separate the supernatant, and then carry out rectification with a rectification tower, and the intermediate product acryloyl chloride is directly collected in a trichloromethane constant pressure funnel equipped with 450 grams of solvent for subsequent use.

[0036] Add 302 grams of morpholine and 350 grams of acid-binding agent sodium bicarbonate solid powder into a 2L reactor with a low-temperature water bath...

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Abstract

The invention relates to a method for synthesizing high-purity N-acryloyl-morpholine, comprising the steps of: dropwise mixing acrylic acid and phosphorus trichloride within 0.5-1 hours, and allowing reaction at 40-45DEG C for 3-4 hours under stirring speed of 80-100rpm to obtain acryloyl chloride; and dropwise mixing morpholine, an acid-binding agent and a solvent within 3-4 hours to obtain a mixed liquid, allowing reaction at 0-5DEG C for 3 hours under stirring speed of 80-100rpm, collecting supernatant, and distilling in the presence of a compound polymerization inhibitor under reduced pressure to obtain an N-acryloyl-morpholine product with purity over 99%, wherein the molar ratio of phosphorus trichloride and acrylic acid is 1:(3-3.5), the molar ratio of acryloyl chloride and morpholine is 1:(1-1.5), the addition amount of the acid-binding agent is 50-150 wt% of morpholine, the solvent addition amount is 100-200 wt% of morpholine, and the addition amount of the compound polymerization inhibitor is 0.1-1 wt% of morpholine.

Description

technical field [0001] The invention relates to a synthesis method for preparing high-purity N-acryloylmorpholine by using phosphorus trichloride and acrylic acid as raw materials. Background technique [0002] N-acryloylmorpholine is an excellent additive and modifier for synthetic resins, used as a reactive diluent for UV-curable resins, and an effective modifier for acrylate resins and gelatin. The polyacryloylmorpholine polymerization product based on it is used in the fields of oilfield additives, ink additives, papermaking additives and adhesives. Since acryloylmorpholine is non-toxic and has good biocompatibility as a monomer, it has broad application prospects in the fields of water treatment and medicine. [0003] The early synthesis technology of acryloylmorpholine was reported to be obtained by pyrolysis of alkyl-substituted propionylmorpholine. Japanese patent JP111000375 has reported that by morpholino propionyl morpholine route (4-morpholino propionyl morphol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/185
Inventor 张吉波田振生王勋章刘宇郑志强周亚婷刘长清盛光宫立波宋妍
Owner BC P INC CHINA NAT PETROLEUM CORP
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