CN112375046A - Recovery method of waste material after elimination and purification of N-acryloyl morpholine - Google Patents
Recovery method of waste material after elimination and purification of N-acryloyl morpholine Download PDFInfo
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- CN112375046A CN112375046A CN202011419351.8A CN202011419351A CN112375046A CN 112375046 A CN112375046 A CN 112375046A CN 202011419351 A CN202011419351 A CN 202011419351A CN 112375046 A CN112375046 A CN 112375046A
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- waste
- acryloyl morpholine
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- morpholine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D295/00—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms
- C07D295/16—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms acylated on ring nitrogen atoms
- C07D295/18—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms acylated on ring nitrogen atoms by radicals derived from carboxylic acids, or sulfur or nitrogen analogues thereof
- C07D295/182—Radicals derived from carboxylic acids
- C07D295/185—Radicals derived from carboxylic acids from aliphatic carboxylic acids
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for recovering waste materials after elimination and purification of N-acryloyl morpholine, which comprises the following steps: (1) adding acrylic anhydride into the waste, wherein the molar weight ratio of the acrylic anhydride to the morpholinyl propionyl morpholine in the waste is 1: 1, setting the reaction temperature to be 0-5 ℃ and setting the reaction time to be 4 hours; (2) after the reaction in the step (1) is finished, heating to 90 ℃, and distilling under the pressure of-0.08 mpa to-0.09 mpa to collect acrylic acid; (3) after the collection in the step (2) is finished, the temperature is kept, the pressure is reduced, the absolute pressure is set to be 100-200 pa in the pressure environment, and the N-acryloyl morpholine is collected by distillation. (4) And (4) after the collection in the step (3) is finished, discharging the treatment liquid, and cooling to room temperature to obtain solid waste residues. The invention aims at that most morpholinyl propionyl morpholine in the waste material after the elimination and purification of N-acryloyl morpholine is subjected to substitution reaction by using acrylic anhydride, and then the N-acryloyl morpholine generated in the substitution reaction is collected by adopting a distillation method.
Description
Technical Field
The invention relates to the technical field of chemical synthesis, in particular to a method for recovering waste materials after elimination and purification of N-acryloyl morpholine.
Background
In the process of synthesizing N-acryloyl morpholine, after the N-acryloyl morpholine is prepared and purified by a thermal cracking method, a part of waste materials still remain, and the waste materials comprise N-acryloyl morpholine, morpholinyl propionyl morpholine, a catalyst, a polymerization inhibitor, N-acryloyl morpholine polymer and the like. The waste material accounts for about 18% of the mass ratio of the reaction raw materials, wherein the morpholinyl propionyl morpholine accounts for about 10% of the mass ratio. Therefore, the method for preparing the N-acryloyl morpholine has low yield and high cost, and cannot be applied to industrial production, so that the method for recovering the purified N-acryloyl morpholine by eliminating the waste materials is needed.
Disclosure of Invention
The invention provides a method for recovering waste materials after elimination and purification of N-acryloyl morpholine.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for recovering waste materials after elimination and purification of N-acryloyl morpholine is based on the following chemical reaction principle:
the method comprises the following steps:
(1) adding acrylic anhydride into the waste, wherein the molar weight ratio of the acrylic anhydride to the morpholinyl propionyl morpholine in the waste is 1: 1, setting the reaction temperature to be 0-5 ℃ and setting the reaction time to be 4 hours;
(2) after the reaction in the step (1) is finished, heating to 90 ℃, and distilling under the pressure of-0.08 mpa to-0.09 mpa to collect acrylic acid;
(3) after the collection in the step (2) is finished, keeping the temperature, continuously reducing the pressure, setting the absolute pressure in a pressure environment to be 100-200 pa, and distilling to collect the N-acryloyl morpholine.
As a preferable configuration of the present invention, in the step (3), the absolute pressure of the vacuum distillation apparatus is 150 pa.
As a preferred arrangement of the present invention, further comprising step (4): after the collection in the step (3) is finished, discharging the treatment liquid, and cooling to room temperature to obtain solid waste residue
Compared with the prior art, the invention has the following beneficial effects: the invention aims at that most morpholinyl propionyl morpholine in the waste material after the elimination and purification of N-acryloyl morpholine is subjected to substitution reaction by using acrylic anhydride, and then the N-acryloyl morpholine generated in the substitution reaction is collected by adopting a distillation method.
Detailed Description
The technical scheme of the invention is described in detail by combining with the examples, wherein the N-acryloyl morpholine waste is obtained after N-acryloyl morpholine is produced by a thermal cracking method.
Example 1
(1) Adding acrylic anhydride into 300g of waste, wherein the molar weight ratio of the acrylic anhydride to the morpholinyl propionyl morpholine in the waste is 1: 1, setting the reaction temperature to be 0-5 ℃ and setting the reaction time to be 4 hours;
(2) after the reaction in the step (1) is finished, heating to 90 ℃, distilling under the pressure of-0.08 mpa to collect acrylic acid, weighing and recording;
(3) after the collection in the step (2) is finished, keeping the temperature, continuously reducing the pressure, setting the absolute pressure in a pressure environment to be 100pa, distilling and collecting the N-acryloyl morpholine, weighing and recording.
(4) And (4) immediately discharging the treatment liquid after the collection in the step (3), cooling to room temperature to obtain solid waste residues, and conveying the solid waste residues to qualified hazardous waste treatment companies for treatment.
Example 2
(1) Adding acrylic anhydride into 300g of waste, wherein the molar weight ratio of the acrylic anhydride to the morpholinyl propionyl morpholine in the waste is 1: 1, setting the reaction temperature to be 0-5 ℃ and setting the reaction time to be 4 hours;
(2) after the reaction in the step (1) is finished, heating to 90 ℃, distilling under the pressure of-0.085 mpa to collect acrylic acid, weighing and recording;
(3) after the collection in the step (2) is finished, keeping the temperature, continuously reducing the pressure, setting the absolute pressure in a pressure environment to be 150pa, distilling and collecting the N-acryloyl morpholine, weighing and recording.
(4) And (4) immediately discharging the treatment liquid after the collection in the step (3), cooling to room temperature to obtain solid waste residues, and conveying the solid waste residues to qualified hazardous waste treatment companies for treatment.
Example 3
(1) Adding acrylic anhydride into 300g of waste, wherein the molar weight ratio of the acrylic anhydride to the morpholinyl propionyl morpholine in the waste is 1: 1, setting the reaction temperature to be 0-5 ℃ and setting the reaction time to be 4 hours;
(2) after the reaction in the step (1) is finished, heating to 90 ℃, distilling under the pressure of-0.09 mpa to collect acrylic acid, weighing and recording;
(3) after the collection in the step (2) is finished, keeping the temperature, continuously reducing the pressure, setting the absolute pressure in a pressure environment to be 200pa, distilling and collecting the N-acryloyl morpholine, weighing and recording.
(4) And (4) immediately discharging the treatment liquid after the collection in the step (3), cooling to room temperature to obtain solid waste residues, and conveying the solid waste residues to qualified hazardous waste treatment companies for treatment.
The results of the treatment of the N-acryloylmorpholine waste in the above examples are shown in Table 1.
TABLE 1
As can be seen from Table 1, the recovery rate of N-acryloyl morpholine is highest under the environment of 150pa of absolute pressure.
The invention aims at that most morpholinyl propionyl morpholine in the waste material after the elimination and purification of N-acryloyl morpholine is subjected to substitution reaction by using acrylic anhydride, and then the N-acryloyl morpholine generated in the substitution reaction is collected by adopting a distillation method.
Furthermore, those skilled in the art will appreciate that while some embodiments described herein include some features included in other embodiments, rather than other features, combinations of features of different embodiments are meant to be within the scope of the invention and form different embodiments. For example, in the claims above, any of the claimed embodiments may be used in any combination. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Claims (3)
1. A method for recovering waste materials after elimination and purification of N-acryloyl morpholine is based on the following chemical reaction principle:
the method is characterized by comprising the following steps:
(1) adding acrylic anhydride into the waste, wherein the molar weight ratio of the acrylic anhydride to the morpholinyl propionyl morpholine in the waste is 1: 1, setting the reaction temperature to be 0-5 ℃ and setting the reaction time to be 4 hours;
(2) after the reaction in the step (1) is finished, heating to 90 ℃, and distilling under the pressure of-0.08 mpa to-0.09 mpa to collect acrylic acid;
(3) after the collection in the step (2) is finished, the temperature is kept, the pressure is reduced, the absolute pressure is set to be 100-200 pa in the pressure environment, and the N-acryloyl morpholine is collected by distillation.
2. The method for recycling and treating N-acryloyl morpholine waste material as claimed in claim 1, wherein in step (3), the absolute pressure of the vacuum distillation device is 150 pa.
3. The method for recycling and treating N-acryloyl morpholine waste material as claimed in claim 1, further comprising step (4): and (4) after the collection in the step (3) is finished, discharging the treatment liquid, and cooling to room temperature to obtain solid waste residues.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011419351.8A CN112375046A (en) | 2020-12-06 | 2020-12-06 | Recovery method of waste material after elimination and purification of N-acryloyl morpholine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011419351.8A CN112375046A (en) | 2020-12-06 | 2020-12-06 | Recovery method of waste material after elimination and purification of N-acryloyl morpholine |
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| CN112375046A true CN112375046A (en) | 2021-02-19 |
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| CN202011419351.8A Pending CN112375046A (en) | 2020-12-06 | 2020-12-06 | Recovery method of waste material after elimination and purification of N-acryloyl morpholine |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006182676A (en) * | 2004-12-27 | 2006-07-13 | Nippon Shokubai Co Ltd | Method for producing amide compound |
| CN108164477A (en) * | 2016-12-07 | 2018-06-15 | 深圳市有为化学技术有限公司 | The preparation method of single or multiple degree of functionality acid/acrylic amide type compound |
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2020
- 2020-12-06 CN CN202011419351.8A patent/CN112375046A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006182676A (en) * | 2004-12-27 | 2006-07-13 | Nippon Shokubai Co Ltd | Method for producing amide compound |
| CN108164477A (en) * | 2016-12-07 | 2018-06-15 | 深圳市有为化学技术有限公司 | The preparation method of single or multiple degree of functionality acid/acrylic amide type compound |
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Application publication date: 20210219 |
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