CN112047854B - Preparation method of N-vinyl alkyl amide - Google Patents
Preparation method of N-vinyl alkyl amide Download PDFInfo
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- CN112047854B CN112047854B CN202011123377.8A CN202011123377A CN112047854B CN 112047854 B CN112047854 B CN 112047854B CN 202011123377 A CN202011123377 A CN 202011123377A CN 112047854 B CN112047854 B CN 112047854B
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- C07—ORGANIC CHEMISTRY
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- C07C231/00—Preparation of carboxylic acid amides
- C07C231/12—Preparation of carboxylic acid amides by reactions not involving the formation of carboxamide groups
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- C07C233/01—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms
- C07C233/02—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having nitrogen atoms of carboxamide groups bound to hydrogen atoms or to carbon atoms of unsubstituted hydrocarbon radicals
- C07C233/03—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having nitrogen atoms of carboxamide groups bound to hydrogen atoms or to carbon atoms of unsubstituted hydrocarbon radicals with carbon atoms of carboxamide groups bound to hydrogen atoms
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- C07C233/16—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having the nitrogen atom of at least one of the carboxamide groups bound to a carbon atom of a hydrocarbon radical substituted by singly-bound oxygen atoms
- C07C233/17—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having the nitrogen atom of at least one of the carboxamide groups bound to a carbon atom of a hydrocarbon radical substituted by singly-bound oxygen atoms with the substituted hydrocarbon radical bound to the nitrogen atom of the carboxamide group by an acyclic carbon atom
- C07C233/18—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having the nitrogen atom of at least one of the carboxamide groups bound to a carbon atom of a hydrocarbon radical substituted by singly-bound oxygen atoms with the substituted hydrocarbon radical bound to the nitrogen atom of the carboxamide group by an acyclic carbon atom having the carbon atom of the carboxamide group bound to a hydrogen atom or to a carbon atom of an acyclic saturated carbon skeleton
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- B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
- B01J2231/40—Substitution reactions at carbon centres, e.g. C-C or C-X, i.e. carbon-hetero atom, cross-coupling, C-H activation or ring-opening reactions
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Abstract
The invention relates to the technical field of vinyl compound production, in particular to a preparation method of N-vinyl alkylamide. The preparation method comprises the following steps: A) reacting acetaldehyde with alkylamide under the action of a composite alkaline catalyst to obtain N-hydroxyethyl alkylamide, and carrying out esterification reaction on the obtained N-hydroxyethyl alkylamide and acid anhydride to obtain an ester compound; the composite alkaline catalyst comprises inorganic alkali and amine compounds; B) and (3) carrying out medium-temperature cracking on the ester compound, and then carrying out reduced pressure rectification to obtain the N-vinyl alkylamide. The inventor finds that the inorganic base and the amine compound are used as the catalyst simultaneously, so that the dosage of the basic catalyst required by the reaction of the N-hydroxyethyl alkylamide and the anhydride can be obviously reduced, the temperature required by the subsequent cracking reaction is reduced, the reaction system is mild, the energy consumption is saved, and the yield and the purity of the reaction product can be obviously improved.
Description
Technical Field
The invention relates to the technical field of vinyl compound production, in particular to a preparation method of N-vinyl alkylamide.
Background
N-vinyl alkylamides are important functional vinyl compounds, the polymerization products of which can form polyvinylamines by hydrolysis. As a water-soluble polymer with amino directly connected to a hydrocarbon skeleton, polyvinylamine has the highest unit cationic charge density and is widely applied to paper-making chemicals and water treatment markets at present. Meanwhile, the polymer is a perfect substitute for polyethyleneimine, polyvinylpyrrolidone and the like in the field of biological medicines due to low cytotoxicity.
N-vinyl alkylamides are preferred monomers for the synthesis of polyvinylamines, since vinylamine monomers are not stable. At present, the synthesis technology of N-vinyl alkyl amide is mastered by two chemical families of basf and Mitsubishi all over the world, and in view of the fact that China is used as the largest global papermaking and water treatment market, a new synthesis route of N-vinyl alkyl amide monomers needs to be developed, and the problem of monomer sources of polyvinylamine products is solved.
N-vinyl methyl amide was synthesized by the following process, employed by Pasteur: hydrogen cyanide is used to react with acetaldehyde, followed by formamidation to form cyanoethylformamide, which is then cleaved to provide NVF. The reaction process requires the use of hydrogen cyanide, which is highly toxic and explosive. The mitsubishi chemical adopts the following process to synthesize the N-vinyl methyl amide: acetaldehyde reacts with formamide to produce hydroxyethyl formamide, then reacts with methanol to produce methoxyethyl formamide, and finally, NVF is obtained through pyrolysis. The process has low yield and purity of the obtained product due to the problem of cracking efficiency.
In order to overcome the defects of the prior art, a plurality of attempts are made at home and abroad to synthesize the N-vinyl alkylamide. U.S. Pittsburgh university in patent CN1678565 discloses a method for preparing N-vinylformamide by reacting hydroxyethyl formamide with an anhydride to form an ester, followed by pyrolysis. The reaction of the hydroxyethyl formamide and the acid anhydride in the reaction system needs to use alkali close to the stoichiometric amount of the hydroxyethyl formamide as a catalyst, which brings difficulty for the separation and purification of subsequent products. Meanwhile, the subsequent cracking reaction usually needs higher temperature (>150 ℃) to generate N-vinylformamide, which is a heat-sensitive substance, and the treatment under high temperature condition can sharply reduce the reaction yield.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method for preparing N-vinyl alkylamide, which has high product yield and purity, and is environmentally friendly.
The invention provides a preparation method of N-vinyl alkyl amide, which comprises the following steps:
A) reacting acetaldehyde with alkylamide under the action of a composite alkaline catalyst to obtain N-hydroxyethyl alkylamide, and carrying out esterification reaction on the obtained N-hydroxyethyl alkylamide and acid anhydride to obtain an ester compound;
the composite alkaline catalyst comprises inorganic alkali and amine compounds;
B) and (3) carrying out medium-temperature cracking on the ester compound, and then carrying out reduced pressure rectification to obtain the N-vinyl alkylamide.
Preferably, the inorganic base comprises one or more of sodium hydroxide, potassium hydroxide, anhydrous potassium carbonate, anhydrous sodium carbonate, sodium phosphate and potassium phosphate.
Preferably, the amine compound includes aliphatic amine or aromatic amine;
the aliphatic amine comprises methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, ethylenediamine, propylenediamine or pentylenediamine;
the aromatic amine comprises benzylamine, aniline, p-toluidine, p-chloroaniline, p-nitroaniline or diphenylamine;
in the composite alkaline catalyst, the mass content of the amine compound is 20-30%.
Preferably, the alkylamide is selected from formamide, acetamide or propionamide.
Preferably, the reaction of acetaldehyde and alkylamide under the action of the composite basic catalyst specifically comprises:
mixing the alkylamide with the composite alkaline catalyst, deoxidizing, cooling to the reaction temperature, and then dripping acetaldehyde for reaction.
Preferably, the reaction temperature of the acetaldehyde and the alkylamide is 0-30 ℃, and the reaction time is 2-5 h;
the reaction of acetaldehyde and alkylamide is carried out under the condition of protective gas; the protective gas is nitrogen.
Preferably, the molar ratio of acetaldehyde to alkylamide is 3-4.5: 1.
preferably, the acid anhydride comprises acetic anhydride, propionic anhydride, succinic anhydride, maleic anhydride, benzoic anhydride, or phthalic anhydride;
the molar ratio of the acid anhydride to the alkylamide is 1.2-2: 1.
preferably, the temperature of the esterification reaction is 20-60 ℃, and the time of the esterification reaction is 5-20 h;
the esterification reaction is carried out under the condition of protective gas; the protective gas is nitrogen.
Preferably, the temperature of the medium-temperature cracking is 40-100 ℃, and the time of the medium-temperature cracking is 2-8 h;
the pressure of the reduced pressure distillation is less than 500 Pa.
The invention provides a preparation method of N-vinyl alkyl amide, which comprises the following steps: A) reacting acetaldehyde with alkylamide under the action of a composite alkaline catalyst to obtain N-hydroxyethyl alkylamide, and carrying out esterification reaction on the obtained N-hydroxyethyl alkylamide and acid anhydride to obtain an ester compound; the composite alkaline catalyst comprises inorganic alkali and amine compounds; B) and (3) carrying out medium-temperature cracking on the ester compound, and then carrying out reduced pressure rectification to obtain the N-vinyl alkylamide. The inventor finds that the inorganic base and the amine compound are used as the catalyst simultaneously, so that the dosage of the basic catalyst required by the reaction of the N-hydroxyethyl alkylamide and the anhydride can be obviously reduced, the temperature required by the subsequent cracking reaction is reduced, the reaction system is mild, the energy consumption is saved, and the yield and the purity of the reaction product can be obviously improved. Meanwhile, the preparation method of the N-vinyl alkyl amide provided by the invention does not need hydrogen cyanide with high toxicity and explosion risk, and is environment-friendly.
Experimental results show that the yield of the N-vinyl formamide prepared by the preparation method of the N-vinyl alkyl amide provided by the invention is more than 71%, and the purity is more than 95%.
Drawings
FIG. 1 shows the NMR spectrum of N-vinylformamide prepared in example 1 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of N-vinyl alkyl amide, which comprises the following steps:
A) reacting acetaldehyde with alkylamide under the action of a composite alkaline catalyst to obtain N-hydroxyethyl alkylamide, and carrying out esterification reaction on the obtained N-hydroxyethyl alkylamide and acid anhydride to obtain an ester compound;
the composite alkaline catalyst comprises inorganic alkali and amine compounds;
B) and (3) carrying out medium-temperature cracking on the ester compound, and then carrying out reduced pressure rectification to obtain the N-vinyl alkylamide.
According to the invention, acetaldehyde and alkylamide are reacted under the action of the composite alkaline catalyst to obtain N-hydroxyethyl alkylamide.
In certain embodiments of the present invention, the complex basic catalyst comprises an inorganic base and an amine compound. In certain embodiments of the invention, the inorganic base comprises one or more of sodium hydroxide, potassium hydroxide, anhydrous potassium carbonate, anhydrous sodium carbonate, sodium phosphate, and potassium phosphate. In certain embodiments of the present invention, the amine compound comprises an aliphatic amine or an aromatic amine. In certain embodiments of the invention, the aliphatic amine comprises methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, ethylenediamine, propylenediamine or pentylenediamine. In certain embodiments of the invention, the aromatic amine comprises benzylamine, aniline, p-toluidine, p-chloroaniline, p-nitroaniline, or diphenylamine.
In some embodiments of the present invention, the content of the amine compound in the composite basic catalyst is 20% to 30% by mass. In certain embodiments, the mass content of the amine compound in the composite basic catalyst is 22%, 27% or 25%.
In certain embodiments of the invention, the alkylamide is selected from formamide, acetamide, or propionamide.
In some embodiments of the present invention, reacting acetaldehyde with alkylamide under the action of the composite basic catalyst specifically comprises:
mixing the alkylamide with the composite alkaline catalyst, deoxidizing, cooling to the reaction temperature, and then dripping acetaldehyde for reaction.
The invention has no special limit on the time of the deoxidization and can realize an oxygen-free environment. In certain embodiments of the present invention, the oxygen removal may be accomplished by passing nitrogen gas.
In certain embodiments of the invention, after oxygen removal, the temperature is reduced to 10 ℃ or 15 ℃.
In some embodiments of the invention, the dropping rate of the acetaldehyde is 100-400 mL/h.
The invention further carries out reaction after cooling, thereby ensuring the reduction of the occurrence degree of side reaction and ensuring the yield of the main product.
In some embodiments of the invention, the reaction temperature is 0-30 ℃, and the reaction time is 2-5 h. In certain embodiments, the temperature of the reaction is 5 to 15 ℃. In certain embodiments, the temperature of the reaction is 10 ℃ or 15 ℃. In some embodiments, the reaction time is 2.5-3.5 hours. In certain embodiments, the reaction time is 3 hours or 3.5 hours. In certain embodiments of the invention, the reaction is carried out under protective gas conditions. In certain embodiments, the shielding gas is nitrogen.
In certain embodiments of the present invention, the acetaldehyde to alkylamide molar ratio is 3 to 4.5: 1. in certain embodiments, the acetaldehyde to alkylamide molar ratio is 3.2 to 4.2: 1. in certain embodiments, the acetaldehyde to alkylamide molar ratio is 3.4: 1 or 4: 1.
after obtaining the N-hydroxyethyl alkylamide, continuously carrying out esterification reaction on the N-hydroxyethyl alkylamide and the acid anhydride under the action of the composite alkaline catalyst to obtain the ester compound.
In certain embodiments of the invention, the anhydride comprises acetic anhydride, propionic anhydride, succinic anhydride, maleic anhydride, benzoic anhydride, or phthalic anhydride.
In certain embodiments of the present invention, the molar ratio of the anhydride to the alkylamide is 1.2-2: 1. in certain embodiments, the molar ratio of the anhydride to the alkylamide is 1.5 to 1.8: 1. in certain embodiments, the molar ratio of the anhydride to the alkylamide is 1.5: 1.
in some embodiments of the present invention, the esterification reaction of the N-hydroxyethyl alkylamide with the acid anhydride under the action of the composite basic catalyst specifically includes:
after the reaction between acetaldehyde and alkylamide is completed, acid anhydride is added to perform esterification reaction.
The acid anhydride is directly added into the product after the reaction of the acetaldehyde and the alkylamide is finished, and the esterification reaction can be carried out under the action of the prior composite alkaline catalyst without additionally adding the composite alkaline catalyst.
In certain embodiments of the present invention, the mass ratio of the composite basic catalyst to the alkylamide is 1-3: 50-100, in some embodiments, the mass ratio of the composite basic catalyst to the alkylamide is 1.28-2.28: 50 to 100. In certain embodiments, the mass ratio of the composite basic catalyst to the alkylamide is 1.8: 90. 1.5: 59 or 2.0: 73. the amount of the composite alkaline catalyst added in the step A) not only ensures the generation of the N-hydroxyethyl alkylamide, but also ensures the generation of the ester compound.
In some embodiments of the present invention, the temperature of the esterification reaction is 20 to 60 ℃, and the time of the esterification reaction is 5 to 20 hours. In certain embodiments, the temperature of the esterification reaction is 30 to 50 ℃. In certain embodiments, the temperature of the esterification reaction is 35 ℃, 40 ℃, or 30 ℃. In certain embodiments, the esterification reaction time is 8 to 12 hours. In certain embodiments, the esterification reaction time is 10h, 12h, or 15 h. In certain embodiments of the present invention, the esterification reaction is carried out under protective gas conditions. In certain embodiments, the shielding gas is nitrogen.
In certain embodiments of the invention, the mesophilic cleavage can be carried out directly after the esterification reaction without any post-treatment steps.
After an ester compound is obtained, the ester compound is subjected to medium-temperature cracking and then is subjected to reduced pressure rectification to obtain the N-vinyl alkyl amide.
In some embodiments of the present invention, the medium-temperature cracking temperature is 40-100 ℃, and the medium-temperature cracking time is 2-8 h. In some embodiments, the medium temperature cracking temperature is 50-70 ℃. In certain embodiments, the temperature of the mesophilic cleavage is 60 ℃. In some embodiments, the medium-temperature cracking time is 3-4 h, 3.5h, 3h or 4 h.
In certain embodiments of the invention, the pressure of the reduced pressure distillation is less than 500 Pa. In certain embodiments, the pressure of the reduced pressure distillation is no greater than 200 Pa. In some embodiments, the pressure of the reduced pressure distillation is 100-150 Pa, 100-200 Pa or 100-300 Pa.
The source of the above-mentioned raw materials is not particularly limited in the present invention, and may be generally commercially available.
The invention provides a preparation method of N-vinyl alkyl amide, which comprises the following steps: A) reacting acetaldehyde with alkylamide under the action of a composite alkaline catalyst to obtain N-hydroxyethyl alkylamide, and carrying out esterification reaction on the obtained N-hydroxyethyl alkylamide and acid anhydride to obtain an ester compound; the composite alkaline catalyst comprises inorganic alkali and amine compounds; B) and (3) carrying out medium-temperature cracking on the ester compound, and then carrying out reduced pressure rectification to obtain the N-vinyl alkylamide. The inventor finds that the inorganic base and the amine compound are used as the catalyst simultaneously, so that the dosage of the basic catalyst required by the reaction of the N-hydroxyethyl alkylamide and the anhydride can be obviously reduced, the temperature required by the subsequent cracking reaction is reduced, the reaction system is mild, the energy consumption is saved, and the yield and the purity of the reaction product can be obviously improved. Meanwhile, the preparation method of the N-vinyl alkyl amide provided by the invention does not need hydrogen cyanide with high toxicity and explosion risk, and is environment-friendly.
Experimental results show that the yield of the N-vinyl formamide prepared by the preparation method of the N-vinyl alkyl amide provided by the invention is more than 71%, and the purity is more than 95%.
In order to further illustrate the present invention, the following examples are provided to describe the preparation method of N-vinyl alkyl amide of the present invention in detail, but should not be construed as limiting the scope of the present invention.
The starting materials used in the following examples are all generally commercially available.
Example 1
45g (1.0mol) of formamide is taken, 0.9g of composite basic catalyst (0.7 g of potassium carbonate and 0.2g of triethylamine) is added, nitrogen is introduced, oxygen is removed, then the temperature is reduced to 10 ℃, 150g (3.4mol) of acetaldehyde is dropwise added, and the reaction is carried out for 3 hours at 10 ℃ to obtain the hydroxyethyl formamide. And then adding 153g (1.5mol) of acetic anhydride, continuously reacting in a closed reaction bottle for 10 hours at the reaction temperature of 35 ℃ under the protection of nitrogen to obtain an ester compound, cracking the ester compound for 3.5 hours at the temperature of 60 ℃ to obtain a mixture containing N-vinylformamide, and carrying out reduced pressure rectification under the pressure of 100-150 Pa to obtain the N-vinylformamide. The detection proves that the yield of the N-vinyl formamide is 75.8 percent, and the purity is 96.2 percent. The nuclear magnetic resonance spectrum of the obtained product N-vinylformamide is shown in figure 1. FIG. 1 shows the NMR spectrum of N-vinylformamide prepared in example 1 of the present invention. As can be seen from FIG. 1, the resonance peak at 4.5ppm should be assigned to the characteristic peak of the hydrogen atom of the vinyl group bonded to the N atom in the N-vinylformamide structure; the resonance peak at 6.5-7.0ppm should be assigned as the proton peak attached to the N atom; and the characteristic peak at 7.5-8.0ppm should be assigned as the proton peak connected to the carbonyl carbon in the amide structure. The presence of the above characteristic peaks clearly demonstrates the successful preparation of N-vinylformamide.
Example 2
59g (1.0mol) of acetamide is taken, 1.5g of composite alkaline catalyst (1.1 g of potassium phosphate and 0.4g of p-toluidine) is added, nitrogen is introduced, oxygen is removed, then the temperature is reduced to 15 ℃, 176g (4.0mol) of acetaldehyde is added dropwise, and the reaction is carried out for 3.5h at 15 ℃ to obtain the hydroxyethyl acetamide. And then adding 150g (1.5mol) of succinic anhydride, continuously reacting in a closed reaction bottle for 12 hours at the reaction temperature of 40 ℃ under the protection of nitrogen to obtain an ester compound, cracking the ester compound for 3 hours at the temperature of 75 ℃ to obtain a mixture containing N-vinyl acetamide, and carrying out reduced pressure rectification under the pressure of 100-200 Pa to obtain the N-vinyl acetamide. The yield of the obtained product N-vinyl acetamide is 82.2%, and the purity is 95.7%.
Example 3
Taking 73g (1.0mol) of propionamide, adding 2.0g of composite alkaline catalyst (wherein 1.5g of potassium carbonate and 0.5g of diphenylamine), introducing nitrogen, removing oxygen, cooling to 10 ℃, then dropwise adding 150g (3.4mol) of acetaldehyde, and reacting for 3 hours at 10 ℃ to obtain the hydroxyethyl propionamide. And then adding 200g (1.5mol) of acetic anhydride, continuously reacting in a closed reaction bottle for 15h under the protection of nitrogen at the reaction temperature of 30 ℃ to obtain an ester compound, cracking the ester compound for 4h at the temperature of 60 ℃ to obtain a mixture containing N-vinyl propionamide, and performing reduced pressure rectification under the pressure of 100-300 Pa to obtain the N-vinyl propionamide. The yield of the obtained product N-vinylpropionamide was 71.2% and the purity was 95.1%.
Comparative example 1
45g (1.0mol) of formamide is taken, 0.9g of potassium carbonate is added, nitrogen is introduced to remove oxygen, then the temperature is reduced to 10 ℃, 150g (3.4mol) of acetaldehyde is dripped to react for 3 hours at 10 ℃, and the hydroxyethyl formamide is obtained. Then adding 153g (1.5mol) of acetic anhydride, continuously reacting in a closed reaction bottle for 10 hours at the reaction temperature of 35 ℃ under the protection of nitrogen to obtain an ester compound, cracking the ester compound for 4 hours at the temperature of 60 ℃ to obtain a mixture containing N-vinylformamide, and performing reduced pressure rectification under the pressure of 150-300 Pa to obtain the N-vinylformamide. The yield of the obtained product N-vinylformamide is 35.2%, and the purity is 68.7%.
Comparative example 2
59g (1.0mol) of acetamide is taken, 1.5g of p-toluidine is added, nitrogen is introduced for deoxidization, then the temperature is reduced to 15 ℃, 176g (4.0mol) of acetaldehyde is dripped, and the reaction is carried out for 3.5 hours at 15 ℃ to obtain the hydroxyethyl acetamide. And then adding 150g (1.5mol) of succinic anhydride, continuously reacting in a closed reaction bottle for 12h at the reaction temperature of 40 ℃ under the protection of nitrogen to obtain an ester compound, cracking the ester compound for 6h at the temperature of 75 ℃ to obtain a mixture containing N-vinyl acetamide, and carrying out reduced pressure rectification under the pressure of 200-350 Pa to obtain the N-vinyl acetamide. The yield of the obtained product N-vinyl acetamide is 38.9%, and the purity is 71.5%.
Experimental results show that the yield of the N-vinyl formamide prepared by the preparation method of the N-vinyl alkyl amide provided by the invention is more than 71%, and the purity is more than 95%.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A process for the preparation of an N-vinyl alkylamide comprising the steps of:
A) reacting acetaldehyde with alkylamide under the action of a composite alkaline catalyst to obtain N-hydroxyethyl alkylamide, and carrying out esterification reaction on the obtained N-hydroxyethyl alkylamide and acid anhydride to obtain an ester compound; the alkyl amide is selected from formamide, acetamide or propionamide;
the composite basic catalyst is potassium carbonate and triethylamine; or the composite alkaline catalyst is potassium carbonate and p-toluidine; or the composite alkaline catalyst is potassium carbonate and diphenylamine;
B) carrying out medium temperature cracking on the ester compound, and then carrying out reduced pressure rectification to obtain N-vinyl alkylamide; the temperature of the medium-temperature cracking is 40-100 ℃.
2. The production method according to claim 1,
in the composite alkaline catalyst, the mass content of the amine compound is 20-30%.
3. The preparation method according to claim 1, wherein the reaction of acetaldehyde with alkylamide under the action of the composite basic catalyst specifically comprises:
mixing the alkylamide with the composite alkaline catalyst, deoxidizing, cooling to the reaction temperature, and then dripping acetaldehyde for reaction.
4. The preparation method according to claim 1, wherein the reaction temperature of acetaldehyde and alkyl amide is 0-30 ℃, and the reaction time is 2-5 h;
the reaction of acetaldehyde and alkylamide is carried out under the condition of protective gas; the protective gas is nitrogen.
5. The method according to claim 1, wherein the molar ratio of acetaldehyde to alkylamide is 3 to 4.5: 1.
6. the production method according to claim 1, wherein the acid anhydride comprises acetic anhydride, propionic anhydride, succinic anhydride, maleic anhydride, benzoic anhydride, or phthalic anhydride;
the molar ratio of the acid anhydride to the alkylamide is 1.2-2: 1.
7. the preparation method according to claim 1, wherein the temperature of the esterification reaction is 20 to 60 ℃, and the time of the esterification reaction is 5 to 20 hours;
the esterification reaction is carried out under the condition of protective gas; the protective gas is nitrogen.
8. The preparation method according to claim 1, wherein the medium-temperature cracking time is 2-8 h;
the pressure of the reduced pressure distillation is less than 500 Pa.
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