CN109851531B - Preparation method of (N-methyl perfluoroalkyl sulfonamide) ethyl acrylate - Google Patents
Preparation method of (N-methyl perfluoroalkyl sulfonamide) ethyl acrylate Download PDFInfo
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Abstract
The invention relates to a preparation method of (N-methyl perfluoroalkyl sulfonamide) ethyl acrylate, which comprises the following steps: s1, reacting at a temperature lower than 4 ℃ by taking perfluoroalkyl sulfonyl fluoride and methylamine as raw materials and an inorganic saline solution as a solvent to obtain N-methyl perfluoroalkyl sulfonamide; s2, under the action of an alkaline catalyst, reacting the N-methyl perfluoroalkyl sulfonamide prepared by the S1 with ethylene carbonate to obtain N-hydroxyethyl-N-methyl perfluoroalkyl sulfonamide; s3, in the presence of hydroquinone, carrying out ester exchange reaction on the N-hydroxyethyl-N-methyl perfluoroalkyl sulfonamide prepared in the step S2 and methyl acrylate to obtain acrylic acid (N-methyl perfluoroalkyl sulfonamide) ethyl ester. Has the advantages that: the salt water solution is used as the solvent for preparing the N-methyl perfluoroalkyl sulfonamide, so that the technical bias that only a non-aqueous solvent can be used in the prior art is overcome, the COD content in the wastewater is greatly reduced, and the environment-friendly effect is achieved; high yield and purity.
Description
Technical Field
The invention relates to the field of preparation of unsaturated group-containing perfluorocarbon chain alkyl ester serving as a main raw material of three proofings of fabrics, in particular to a preparation method of (N-methyl perfluoroalkyl sulfonamide) ethyl acrylate.
Background
With the increasing of people's living water, the requirements for articles such as clothes and the like are higher and higher, the clothes are required to be light, breathable, waterproof, oil-proof and dustproof, so that a thin coating is required to be coated on the surface of a fabric, the fabric is endowed with the characteristics of lightness, breathability, oil-proof, waterproof, dustproof and the like, the daily necessities such as clothes, umbrellas and the like made of the fabric have the characteristics of breathability, oil-proof, waterproof, dustproof and three-proof of the fabric, the most main raw material for coating the fabric is fluorine ester, not all fluorine ester can be used, acrylic acid (N-methyl perfluorooctyl or hexyl or butyl sulfonamide) ethyl ester is commonly used, PFOS is generated in the degradation or production of the acrylic acid (N-methyl perfluorooctyl sulfonamide) ethyl ester is forbidden, and the fluorine ester used for three-proof of the fabric is acrylic acid (N-methyl perfluorohexyl or butyl sulfonamide) ethyl ester internationally allowed, the use of (N-methyl-perfluorooctylsulfonamide) ethyl acrylate is not permitted.
The (N-methylperfluoroalkylsulfonamido) acrylate is predominantly (N-methylperfluorooctyl or hexyl or butylsulfonamido) ethyl acrylate. It has excellent homopolymerization and copolymerization of other monomers, is one kind of fluoric polymerizable monomer with unique surface performance, and may be used widely in hydrophobic oil repellent, antifouling paint, leveling agent, dispersant, antiblocking agent, medical material and material with photoelectronic performance. The acrylic ester polymer has the characteristics of good film forming property and loose network structure, and the treated product has good air and moisture permeability, is soft and elastic, has good hand feeling and keeps the original style of the treated product.
In the prior art, the synthesis method of the acrylic acid (N-methyl perfluoroalkyl sulfonamide) ester comprises three steps: 1. Adding triethylamine and an organic solvent (non-aqueous solvent) into a reaction kettle, introducing methylamine gas below 5 ℃, slowly dropwise adding perfluoroalkyl sulfonyl fluoride to prepare perfluoroalkyl sulfonyl methylamine, washing with water to remove triethylamine salt of hydrofluoric acid, and drying; 2. reacting with ethylene carbonate under alkaline condition to generate N-methyl perfluoroalkyl amino ethanol; 3. the esterification reaction with acrylic acid in the presence of hydroquinone as a polymerization inhibitor to produce (N-methylperfluorosulfonamido) ethyl acrylate, the acrylic acid is in large excess in step 3 in order to obtain (N-methylperfluorosulfonamido) ethyl acrylate with high yield and without polymerization, and hydroquinone as a polymerization inhibitor is added. The preparation method has the disadvantages that the organic solvent is used in the step 1, the COD of the wastewater is high when the salt is removed by washing, the acrylic acid in the step 3 is excessive, the acrylic acid and the hydroquinone in the wastewater are not easy to recover during washing, the COD content of the wastewater is high, the method is not environment-friendly, and a new environment-friendly synthesis method needs to be found under the national high-pressure policy of environment protection, so that the product has a living space.
Disclosure of Invention
The invention provides a preparation method of (N-methyl perfluoroalkyl sulfonamide) ethyl acrylate, aiming at effectively overcoming the defects of solvent use, high COD (chemical oxygen demand) of wastewater and poor environmental protection in the existing preparation method.
The technical scheme for solving the technical problems is as follows: a preparation method of (N-methyl perfluoroalkyl sulfonamide) ethyl acrylate comprises the following steps:
s1, reacting at a temperature lower than 4 ℃ by taking perfluoroalkyl sulfonyl fluoride and methylamine as raw materials and an inorganic saline solution as a solvent to obtain N-methyl perfluoroalkyl sulfonamide;
s2, under the action of an alkaline catalyst, reacting the N-methyl perfluoroalkyl sulfonamide prepared by the S1 with ethylene carbonate to obtain N-hydroxyethyl-N-methyl perfluoroalkyl sulfonamide;
s3, in the presence of hydroquinone, carrying out ester exchange reaction on the N-hydroxyethyl-N-methyl perfluoroalkyl sulfonamide prepared in the step S2 and methyl acrylate to obtain acrylic acid (N-methyl perfluoroalkyl sulfonamide) ethyl ester.
On the basis of the technical scheme, the invention can further specifically select the following.
Further, the specific step of S1 is: adding methylamine water solution and inorganic salt water solution into a reaction kettle in a low-temperature environment below-8 ℃, stirring uniformly, starting to slowly dropwise add perfluoroalkyl sulfonyl fluoride to the bottom of the reaction solution through a bottom inserting tube at the temperature of-8 to-4 ℃, keeping the temperature of the reaction solution below 0 ℃ in the dropwise adding process, keeping the temperature below 0 ℃ after dropwise adding, fully reacting, floating the product on the liquid level, centrifuging, washing with water, and drying in vacuum to obtain the product.
Preferably, the concentration of the aqueous methylamine solution is 40 wt% and the concentration of the aqueous inorganic salt solution is 5 to 22 wt%.
Specifically, the perfluoroalkanesulfonyl fluoride in S1 is any one of perfluorobutanesulfonyl fluoride and perfluorohexylsulfonyl fluoride.
Further, the specific step of S2 is: adding an alkaline catalyst, heptane and N-methyl perfluoroalkyl sulfonamide obtained from S1 into a reaction container, keeping the temperature at 105 ℃ for refluxing, removing water by using a water separator, heating to 110 ℃ for refluxing when the water in the water separator is not increased any more, cooling to 98 ℃ when no heptane is evaporated out from the water separator, slowly dropwise adding ethylene carbonate, and keeping the temperature for full reaction after dropwise adding is finished to obtain the catalyst.
Further, the specific step of S3 is: after S2 full reaction is completed, adding hydroquinone, methyl acrylate and sodium methoxide into a reaction container, heating to 74-76 ℃ under the protection of inert gas, stirring and preserving heat for reaction, receiving methanol generated by the reaction by a water separator during the reaction, fully reacting until the mass of the methanol in the water separator is not increased any more, stopping the reaction, adjusting the reaction liquid to be neutral by acetic acid, and decompressing and steaming out the redundant methyl acrylate to obtain the (N-methyl perfluoroalkyl sulfonamide) ethyl acrylate.
Preferably, the molar ratio of perfluoroalkanesulfonyl fluoride to methylamine in S1 is 1: 2-2.5.
Specifically, the dosage ratio of the perfluoroalkyl sulfonyl fluoride in S1 to the inorganic salt water solution is 1mol:350-450 g; the solute of the inorganic salt water solution is any one or a mixture of sodium chloride, potassium chloride, sodium sulfate and potassium sulfate.
Most preferably, the reaction is maintained at a temperature of less than 0 ℃ in S1.
Preferably, the basic catalyst in S2 is sodium carbonate or potassium carbonate, and the molar ratio of the N-methyl perfluoroalkyl sulfonamide to the ethylene carbonate in S2 is 1: 1.05; N-hydroxyethyl-N-methyl perfluoroalkyl sulfonamide with methyl acrylate 1 in S3: 1.15-1.25.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention takes a saline solution as a solvent for preparing N-methyl perfluoroalkyl sulfonamide by reacting perfluoroalkyl sulfonyl chloride with methylamine, overcomes the technical prejudice that only a non-aqueous solvent can be used in the prior art (N-methyl perfluoroalkyl sulfonamide can not be obtained because perfluoroalkyl sulfonyl fluoride is easy to be hydrolyzed into perfluoroalkyl sulfonic acid under the condition of water), and finds that a large amount of perfluoroalkyl sulfonyl fluoride is hydrolyzed when the temperature is higher than 4 ℃, a small amount of perfluorobutyl sulfonyl fluoride is hydrolyzed between 0 and 4 ℃ but perfluorohexyl sulfonyl fluoride is not hydrolyzed, but almost all perfluorohexyl sulfonyl fluoride is not hydrolyzed when the temperature is lower than 0 ℃, and only perfluoroalkyl sulfonamide products are generated, so the invention can adopt water as the solvent to react at low temperature, the COD content in the final waste water is greatly reduced, and the environment is more friendly.
(2) If only water is used as a solvent at low temperature, perfluoroalkyl sulfonamide is easy to further react with perfluoroalkyl sulfonyl fluoride in methylamine water solution to generate N-methyl-bi-perfluoroalkyl sulfonamide, and the mixture of the N-methyl perfluoroalkyl sulfonamide and the N-methyl-bi-perfluoroalkyl sulfonamide is finally obtained, but the N-methyl-bi-perfluoroalkyl sulfonamide can not react with ethylene carbonate to generate sulfonamide containing hydroxyl, so that esterification reaction can not be carried out to generate acrylic acid (N-methyl perfluoroalkyl sulfonamide) ethyl ester, and the purity of the final product is not high, therefore, the invention takes saline solution as the solvent, leads the generated N-methyl perfluoroalkyl sulfonamide to float on the reaction liquid surface, thereby reducing the chance of re-reaction with the perfluoroalkyl sulfonyl fluoride and reducing the generation of byproducts, after the reaction is completed, only the solid (N-perfluoroalkyl sulfonamide which is insoluble in water) centrifugally thrown out is washed twice by deionized water, and the water phase after washing only contains water and sodium chloride, and then the water is distilled to remove water, and the sodium chloride is centrifugally separated, so that the method can be used in the reaction without polluting the environment.
(3) And when the perfluoroalkyl sulfonyl fluoride is dropwise added, bottom insertion and dropwise addition are adopted, so that the further reaction of the perfluoroalkyl sulfonyl fluoride and the generated N-methyl perfluoroalkyl sulfonamide can be reduced.
(4) Synthesizing fluorine ester by adopting ester exchange reaction, adopting reaction under the protection of argon, monitoring distillate by using gas chromatography, stopping the reaction when the methanol quality (the content of the gas chromatography and the quality of the distillate in a phase separator) is not increased any more, evaporating redundant methyl acrylate by using a pressure-changing and reducing device, and not needing water washing to obtain the product, wherein a small amount of hydroquinone added is used as a polymerization inhibitor, so that the possible subsequent self-polymerization of the generated (N-methyl perfluoroalkyl sulfonamide) ethyl acrylate can be prevented, the yield is higher, the product purity is higher, and the quality guarantee period of the product can be effectively prolonged; after the reaction is finished, hydroquinone does not need to be separated, the pH value is adjusted by acid, then the temperature is kept between 50 and 55 ℃, the salt is filtered and desalted, the filtered salt is collected to a certain amount, then the salt is washed by water and filtered to recover acrylic acid (N-methyl perfluoroalkyl sulfonamide) ethyl ester included in the salt, and the water phase is directly used in the production of the N-methyl perfluoroalkyl sulfonamide without generating three wastes.
Detailed Description
The principles and features of this invention are described below in conjunction with specific embodiments, which are set forth merely to illustrate the invention and are not intended to limit the scope of the invention.
For the sake of brevity, the methods or procedures used in the following examples are conventional methods or procedures known to those skilled in the art unless otherwise specified, and the drugs used are commercially available products unless otherwise specified.
Example 1
A preparation method of (N-methyl perfluorobutyl sulfonamide) ethyl acrylate comprises the following steps:
s1, a 1000mL four-neck flask reaction kettle with a dynamic stirring and thermometer is immersed in a water bath with the salt water temperature of-8 ℃, 108.5 g of 40% methylamine water solution (1.4mol) is accurately weighed, 340 g of water is added, 40.5 g of sodium chloride is added after uniform stirring, the stirring is continued until the sodium chloride is completely dissolved, 211.4 g (0.7mol) of perfluorobutane sulfonyl fluoride is dropwise added when the temperature of the kettle is reduced to-8 to-4 ℃, the kettle is inserted and slowly dropwise added to keep the temperature of the kettle below 0 ℃, the reaction is kept at the temperature for 4 hours after the perfluorobutane sulfonyl fluoride is added, after the reaction is finished, the pH value of the solution is adjusted to be about 6 by hydrochloric acid, the product is floated on the liquid level, then the materials are centrifuged to obtain perfluorobutyl sulfonyl methylamine, 242.2 g of wet solid, 200 g of water is added, the temperature is increased to 50 ℃, the stirring is carried out for 4 hours, the temperature is reduced to room temperature and then the materials are spun, after the water washing, 223., vacuum drying at 50 deg.C gave 214.7 g (ca. 0.686mol) of finished product in 98.0% yield.
S2, immersing a 500mL four-neck flask reaction kettle with a motor-driven stirring and thermometer in an oil bath, adding 214.7 g of solid N-methyl perfluorobutyl sulfonamide obtained in S1, 2.8 g of anhydrous sodium carbonate and 150 g of heptane, keeping the temperature to reflux at 105 ℃, removing water by using a water separator, removing heptane when the water in the water separator is not increased any more, cooling to 98 ℃ when the temperature of the kettle rises to 110 ℃, evaporating no heptane in the water separator, slowly dropwise adding 63.8 g (0.72mol) of ethylene carbonate, and keeping the temperature to react for 11 hours to obtain the N-hydroxyethyl-N-methyl perfluorobutyl sulfonamide.
S3, adding 0.76 g of hydroquinone into the reaction kettle of S2, adding 70 g of methyl acrylate, adding 1 g of sodium methoxide solid, replacing three times with argon, keeping the temperature and stirring at 74-76 ℃, receiving methanol generated by the reaction by a water separator, keeping the temperature and reacting for 10 hours, receiving 27.1 g of liquid in the water separator, analyzing the 81.2 g of methanol and 18.8% of methyl acrylate by gas chromatography, adjusting the PH to about 7 by acetic acid, and evaporating redundant methyl acrylate under reduced pressure to obtain 280.2 g of (N-methyl perfluorobutane sulfonamide) ethyl acrylate with the yield of 99.4 percent.
Example 2
A preparation method of (N-methyl perfluorobutyl sulfonamide) ethyl acrylate comprises the following steps:
s1, immersing a 3000mL four-neck flask reaction kettle with a motor-driven stirring and thermometer in a water bath with the salt water temperature of-8 ℃, accurately weighing 325.5 g of 40% methylamine water solution (4.2mol), adding 1120 g of water, stirring uniformly, adding 131.5 g of sodium chloride, continuing stirring until the sodium chloride is completely dissolved, beginning to dropwise add 634.2 g (2.1mol) of perfluorobutyl sulfonyl fluoride when the temperature of the kettle is reduced to-8 to-4 ℃, inserting the bottom and slowly dropwise adding the kettle to keep the temperature below 0 ℃, keeping the temperature for reaction for 4 hours after the addition of the perfluorobutyl sulfonyl fluoride, adjusting the pH of the solution to be about 6 by using hydrochloric acid after the reaction is finished, generating a product to float on the liquid level, centrifugally throwing the material to obtain perfluorobutyl sulfonyl methylamine, 726.6 g of wet solid, adding 600 g of water, heating to 50 ℃, stirring for 4 hours, reducing the temperature to room temperature and then throwing the material, washing twice with water to obtain 666.5 g of wet material, vacuum drying at 50 ℃ to obtain 655.2 g (about 2.093mol) of finished product, the yield thereof was found to be 99.68%.
S2, immersing a 2000mL four-neck flask reaction kettle with a motor-driven stirring and thermometer in an oil bath, adding 655.2 g (2.093mL) of solid N-methyl perfluorobutyl sulfonamide obtained in S1 and 8.8 g of anhydrous sodium carbonate, adding 300 g of heptane, heating to 105 ℃, carrying out heat preservation and reflux, dehydrating by using a water separator until the water content in the phase separator is not increased, removing the heptane to the kettle temperature of 110 ℃, removing no heptane, cooling to 98 ℃, slowly dropwise adding 196.8 g (2.236mol) of ethylene carbonate, and carrying out heat preservation reaction for 11 hours to obtain the N-hydroxyethyl-N-methyl perfluorobutyl sulfonamide.
S3 adding 2.3 g hydroquinone into the reaction kettle of S2, adding 215.0 g methyl acrylate, adding 3.0 g sodium methoxide solid, converting with argon for three times, stirring at 74-76 ℃, receiving the methanol generated by the reaction by a water separator, reacting for 10 hours at the temperature, receiving 81.5 g liquid in the water separator, analyzing the methanol by gas chromatography to be 81.2 g and the methyl acrylate to be 18.8%, evaporating the redundant methyl acrylate under reduced pressure, adjusting the pH to be about 7 by hydrochloric acid, filtering and desalting at 50-55 ℃ at the temperature, obtaining 858.7 g ethyl acrylate (N-methyl perfluorobutanesulfonamide) with the yield of 99.8%.
Example 3
A preparation method of (N-methyl perfluorohexyl sulfonamide) ethyl acrylate comprises the following steps:
s1, a 1000ml four-neck flask reaction kettle with a motor-driven stirring and thermometer is soaked in a water bath with the salt water temperature of-8 ℃, 108.5 g of methylamine water solution (1.4mol) with the concentration of 40 percent is accurately weighed, 340 g of water is added, 34 g of sodium chloride is added after uniform stirring, the stirring is continued until the sodium chloride is completely dissolved, 281.4 g (0.7mol) of perfluorohexyl sulfonyl fluoride is dropwise added when the kettle temperature is reduced to-8-4 ℃, the bottom insertion is adopted for slow dropwise addition, the kettle temperature is kept below 4 ℃, the heat preservation reaction is carried out for 4 hours after the addition of perfluorohexyl sulfonyl fluoride, the pH value of the solution is adjusted to be about 6 by hydrochloric acid, the product is floated on the liquid level, then the centrifugal material throwing is carried out to obtain perfluorohexyl sulfonyl methylamine, 343.2 g of wet solid is added, 200 g of water is added, the temperature is raised to 50 ℃, the stirring is carried out for 4 hours, the temperature is reduced to room temperature, then 306.6 g of wet material is added, the 200 g of, cooling to room temperature, throwing to obtain 303.6 g of wet material with chloride ion concentration below 100PPM, and vacuum drying at 50 deg.C to obtain 284.7 g (about 0.69mol) of finished product with 98.5% yield and melting point of 68-72 deg.C.
S2, immersing a 500ml four-neck flask reaction kettle with a motor-driven stirring and thermometer in an oil bath, adding 284.7 g of solid N-methyl perfluorohexyl sulfonamide obtained in S1, 2.8 g of anhydrous sodium carbonate and 150 g of heptane, refluxing and separating at 105 ℃ by adopting a water separator, pouring out liquid in the water separator when the separated water is not increased any more, evaporating the heptane, cooling to 98-100 ℃ until the liquid is not increased in the water separator at 110 ℃, dropwise adding 63.8 g (0.72mol) of ethylene carbonate, and then carrying out heat preservation reaction for 11 hours to obtain the N-hydroxyethyl-N-methyl perfluorohexyl sulfonamide.
S3, adding 0.76 g of hydroquinone into a reaction kettle of S2, adding 70 g of methyl acrylate, adding 1 g of sodium methoxide solid, replacing three times with argon, carrying out heat preservation and stirring at 74-76 ℃, receiving methanol generated by the reaction by a water separator, carrying out heat preservation reaction for 10 hours, receiving 27.1 g of liquid in the water separator, analyzing 81.2 g of methanol and 18.8% of methyl acrylate by using gas chromatography, distilling out redundant methyl acrylate under reduced pressure, adjusting the pH value to about 7 by using hydrochloric acid, carrying out heat preservation at 50-55 ℃, filtering and desalting to obtain 347.4 g of acrylic acid (N-methyl perfluorohexyl sulfonamide) ethyl ester, wherein the yield is 98.6%.
Example 4
A preparation method of (N-methyl perfluorohexyl sulfonamide) ethyl acrylate comprises the following steps:
s1, immersing a 3000ml four-neck flask reaction kettle with a dynamic stirring and thermometer in a water bath with the salt water temperature of-8 ℃, accurately weighing 325.5 g of 40% methylamine water solution (4.2mol), adding 1120 g of water, stirring uniformly, adding 112 g of sodium chloride, continuously stirring until the sodium chloride is completely dissolved, beginning to dropwise add 844.2 g (2.1mol) perfluorohexyl sulfonyl fluoride when the temperature of the kettle is reduced to-8 to-4 ℃, slowly dropwise adding the kettle by inserting the bottom to keep the temperature below 4 ℃, keeping the temperature for reaction for 4 hours after the addition of the perfluorohexyl sulfonyl fluoride, adjusting the pH value to about 6 by using dilute hydrochloric acid to generate a product, floating on the liquid level, centrifuging and throwing the material to obtain perfluorohexyl sulfonyl methylamine, 1029.6 g of wet solid, adding 600 g of water, heating to 50 ℃, stirring for 4 hours, cooling to room temperature, throwing the material to obtain 919.8 g of wet material, adding 600 g of water, heating to 50 ℃, stirring for 4 hours, cooling to room temperature, throwing to obtain 910.8 g of wet material with chloride ion concentration below 100PPM, and vacuum drying at 50 deg.C to obtain 864.5 g (about 2.093mol) of final product with yield of 99.65% and melting point of 68-72 deg.C.
S2, immersing a 2000ml four-neck flask reaction kettle with a motor-driven stirring and thermometer in an oil bath, adding 864.5 g (2.093ml) of solid N-methyl perfluorohexyl sulfonamide obtained in S1, 8.8 g of anhydrous sodium carbonate, adding 300 g of heptane, heating to 105 ℃, refluxing and dividing water by a water separator until the mass of water in the water separator is not increased, recovering the heptane, cooling to 98 ℃, slowly dropwise adding 196.8 g (2.236mol) of ethylene carbonate, and carrying out heat preservation reaction for 11 hours to obtain the N-hydroxyethyl-N-methyl perfluorohexyl sulfonamide when the kettle temperature is increased to 110 ℃ and no heptane is evaporated out in the water separator.
S3, adding 2.3 g of hydroquinone into a reaction kettle of S2, adding 215.0 g of methyl acrylate, adding 3.0 g of sodium methoxide solid, replacing three times with argon, carrying out heat preservation and stirring at 74-76 ℃, receiving methanol generated by the reaction by a water separator, carrying out heat preservation reaction for 10 hours, receiving 81.5 g of liquid in the water separator, analyzing 81.2 g of methanol and 18.8% of methyl acrylate by using gas chromatography, decompressing and evaporating redundant methyl acrylate, adjusting the pH to about 7 by using hydrochloric acid, filtering and desalting at 50-55 ℃ to obtain 1064.3 g of acrylic acid (N-methyl perfluorohexyl sulfonamide) ethyl ester, wherein the yield is 99.5%, salt entrainment is caused during final salt filtering, water washing is carried out after salt filtering is collected, acrylic acid (N-methyl perfluorohexyl sulfonamide) ethyl ester is centrifugally recovered, and the water phase is applied to the first-step production, so as to achieve the aim of environmental protection.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A preparation method of (N-methyl perfluoroalkyl sulfonamide) ethyl acrylate is characterized by comprising the following steps:
s1, perfluoroalkyl sulfonyl fluoride and methylamine are used as raw materials, an inorganic salt aqueous solution is used as a solvent, and the reaction is carried out at a temperature lower than 4 ℃ to obtain N-methyl perfluoroalkyl sulfonyl amide, wherein the solute of the inorganic salt aqueous solution is any one or a mixture of sodium chloride, potassium chloride, sodium sulfate and potassium sulfate;
s2, under the action of an alkaline catalyst, reacting the N-methyl perfluoroalkyl sulfonamide prepared by the S1 with ethylene carbonate to obtain N-hydroxyethyl-N-methyl perfluoroalkyl sulfonamide;
s3, in the presence of hydroquinone, carrying out ester exchange reaction on the N-hydroxyethyl-N-methyl perfluoroalkyl sulfonamide prepared in the step S2 and methyl acrylate to obtain acrylic acid (N-methyl perfluoroalkyl sulfonamide) ethyl ester.
2. The method for preparing (N-methyl perfluoroalkyl sulfonamide) ethyl acrylate according to claim 1, wherein the specific step of S1 is as follows: adding methylamine water solution and inorganic salt water solution into a reaction kettle in a low-temperature environment below-8 ℃, stirring uniformly, starting to slowly dropwise add perfluoroalkyl sulfonyl fluoride to the bottom of the reaction solution through a bottom inserting tube at the temperature of-8 to-4 ℃, keeping the temperature of the reaction solution below 0 ℃ in the dropwise adding process, keeping the temperature below 0 ℃ after dropwise adding, fully reacting, floating the product on the liquid level, centrifuging, washing with water, and drying in vacuum to obtain the product.
3. The process for preparing (N-methyl perfluoroalkyl sulfonamide) ethyl acrylate according to claim 2, wherein the concentration of the aqueous methylamine solution is 40% by weight and the concentration of the aqueous inorganic salt solution is 5 to 22% by weight.
4. The process for producing (N-methylperfluoroalkylsulfonamido) ethyl acrylate according to claim 1, wherein the perfluoroalkylsulfonyl fluoride in S1 is any one of perfluorobutylsulfonyl fluoride and perfluorohexylsulfonyl fluoride.
5. The method for preparing (N-methyl perfluoroalkyl sulfonamide) ethyl acrylate according to claim 1, wherein the specific step of S2 is as follows: adding an alkaline catalyst, heptane and N-methyl perfluoroalkyl sulfonamide obtained from S1 into a reaction container, keeping the temperature at 105 ℃ for refluxing, removing water by using a water separator, heating to 110 ℃ for refluxing when the water in the water separator is not increased any more, cooling to 98 ℃ when no heptane is evaporated out from the water separator, slowly dropwise adding ethylene carbonate, and keeping the temperature for full reaction after dropwise adding is finished to obtain the catalyst.
6. The method for preparing (N-methyl perfluoroalkyl sulfonamide) ethyl acrylate according to claim 5, wherein the specific step of S3 is as follows: after S2 full reaction is completed, adding hydroquinone, methyl acrylate and sodium methoxide into a reaction container, heating to 74-76 ℃ under the protection of inert gas, stirring and preserving heat for reaction, receiving methanol generated by the reaction by a water separator during the reaction, fully reacting until the mass of the methanol in the water separator is not increased any more, stopping the reaction, adjusting the reaction liquid to be neutral by acetic acid, and decompressing and steaming out the redundant methyl acrylate to obtain the (N-methyl perfluoroalkyl sulfonamide) ethyl acrylate.
7. The process for preparing (N-methylperfluoroalkylsulfonamido) ethyl acrylate according to any one of claims 1 to 6, wherein the molar ratio of perfluoroalkylsulfonyl fluoride to methylamine in S1 is 1: 2.0-2.5.
8. The process for preparing (N-methylperfluoroalkylsulfonamido) ethyl acrylate according to any one of claims 1 to 6, wherein the amount ratio of perfluoroalkylsulfonyl fluoride to the aqueous inorganic salt solution in S1 is 1mol:350-450 g.
9. The process for preparing (N-methyl perfluoroalkylsulfonamido) ethyl acrylate according to any one of claims 1 to 6, wherein S1 is reacted while maintaining a temperature of less than 0 ℃.
10. The process for preparing (N-methyl perfluoroalkyl sulfonamide) ethyl acrylate according to any of claims 1 to 6, wherein the basic catalyst in S2 is sodium carbonate or potassium carbonate, and the molar ratio of N-methyl perfluoroalkyl sulfonamide to ethylene carbonate in S2 is 1: 1.05; N-hydroxyethyl-N-methyl perfluoroalkyl sulfonamide with methyl acrylate 1 in S3: 1.15-1.25.
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