CN114573471A - Preparation method of diacetone acrylamide - Google Patents
Preparation method of diacetone acrylamide Download PDFInfo
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- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
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- C07C45/68—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms
- C07C45/72—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms by reaction of compounds containing >C = O groups with the same or other compounds containing >C = O groups
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Abstract
The invention discloses a preparation method of diacetone acrylamide, which comprises the following steps: mixing acrylonitrile and acetone according to a weight ratio, and then adding concentrated sulfuric acid. In the preparation of diacetone acrylamide, reaction additives and interface reactants are added to enhance the reaction efficiency of the product, chitosan and acetic acid aqueous solution are fully mixed according to the weight ratio, and then sodium citrate and sodium dodecyl sulfate are added to obtain the reaction additives; the silane coupling agent, the polyethylene glycol and the ethanol are matched for stirring and mixing fully, and the reaction efficiency and the reaction speed of the product are enhanced by combining the silane coupling agent, the polyethylene glycol and the ethanol.
Description
Technical Field
The invention relates to the technical field of diacetone acrylamide, and particularly relates to a preparation method of diacetone acrylamide.
Background
Diacetone acrylamide, named as Diacetone acrylamide in English, has the CAS number of 2873-97-4 and the molecular formula of
Having two reactive groups: n-substituted amide and ketone are easy to copolymerize with other ethylene and monomer, so that ketone carbonyl group is introduced into polymer, and the chemical property of ketone carbonyl group can make the polymer produce cross-linking grafting reaction, etc. so as to prepare various adhesives, thickeners, paper reinforcing agent, cross-linking agent, etc.
Yield, also known as reaction yield, is commonly used in chemical and industrial processes and refers to the ratio of the actual product yield per unit amount of starting material charged to the theoretically calculated product yield in a chemical reaction or related chemical industrial process. The same chemical reaction will have different yields at different pressures and temperatures.
The existing diacetone acrylamide preparation method is simple, low in reaction yield, long in process time and low in preparation efficiency, and based on the method, the diacetone acrylamide is further improved and treated.
Disclosure of Invention
The invention aims to provide a preparation method of diacetone acrylamide, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of diacetone acrylamide comprises the following steps: the method comprises the following steps: mixing acrylonitrile and acetone according to the weight ratio of 1:2, and then adding concentrated sulfuric acid with the total amount of 10-20% of acetone; step two: then adding a reaction additive accounting for 1-3% of the total amount of the acrylonitrile, stirring and mixing to perform a first-stage reaction to obtain a body to be reacted; step three: adding 1-5% sodium hydroxide aqueous solution into the body to be reacted, then adding 1-3% interfacial agent into the body to be reacted, and continuing the secondary reaction for 10-20 min; step four: then adding ammonium bicarbonate aqueous solution for extraction, and finally recrystallizing to obtain the diacetone acrylamide.
Preferably, the preparation method of the reaction additive comprises the following steps: fully mixing chitosan and acetic acid aqueous solution according to the weight ratio of 2:5, then adding sodium citrate accounting for 1-5% of the total amount of chitosan and sodium dodecyl sulfate accounting for 1-3%, fully stirring at the rotating speed of 100-300r/min for 10-20min, and obtaining the reaction additive after the stirring is finished.
Preferably, the mass fraction of the acetic acid aqueous solution is 10-30%.
Preferably, the treatment temperature of the first-stage reaction is 55-60 ℃, the reaction time is 20-30min, and the reaction speed is 200-300 r/min.
Preferably, the preparation method of the interfacial reactant is as follows: stirring and mixing 10-20 parts of silane coupling agent KH560, 1-5 parts of polyethylene glycol and 20 parts of ethanol fully, then adding 1-3 parts of tetraethoxysilane and 3 parts of modified nano-silica, performing ultrasonic dispersion treatment, and finishing the treatment to obtain the interfacial reaction agent.
Preferably, the modification method of the modified nano-silica comprises the following steps: and (3) feeding the nano silicon dioxide into deionized water of which the volume is 2-3 times that of the nano silicon dioxide, adding hydrochloric acid to adjust the pH value to 5.0, fully dispersing, washing with water, and drying to obtain the modified nano silicon dioxide.
Preferably, the power of the ultrasonic dispersion treatment is 500W, and the ultrasonic time is 20 min.
Preferably, the mass fraction of the ammonium bicarbonate aqueous solution is 5-7%.
Preferably, the mass fraction of the ammonium bicarbonate aqueous solution is 6%.
Compared with the prior art, the invention has the following beneficial effects: in the preparation of diacetone acrylamide, reaction additives and interfacial reactants are added to enhance the reaction yield of the product, chitosan is added into an acetic acid aqueous solution according to the weight ratio of 2:5, the mixture is fully mixed, then sodium citrate accounting for 1-5% of the total amount of the chitosan and sodium dodecyl sulfate accounting for 1-3% of the total amount of the chitosan are added, the mixture is fully stirred at the rotating speed of 100 plus materials of 300r/min, the stirring time is 10-20min, and the reaction additives are obtained after the stirring is finished; mixing with 10-20 parts of silane coupling agent KH560 and 1-5 parts of polyethylene glycol, stirring and mixing fully with 20 parts of ethanol, then adding 1-3 parts of tetraethoxysilane and 3 parts of modified nano-silica, performing ultrasonic dispersion treatment, and finishing the treatment to obtain an interface reactant, wherein the interface reactant and the silane coupling agent are combined, so that the reaction yield and the reaction rate of the product are enhanced.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious 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 preparation method of diacetone acrylamide of the embodiment comprises the following steps: the method comprises the following steps: mixing acrylonitrile and acetone according to the weight ratio of 1:2, and then adding concentrated sulfuric acid with the total amount of 10-20% of acetone; step two: then adding a reaction additive accounting for 1-3% of the total amount of the acrylonitrile, stirring and mixing to perform a first-stage reaction to obtain a body to be reacted; step three: adding 1-5% sodium hydroxide aqueous solution into the body to be reacted, then adding 1-3% interfacial agent into the body to be reacted, and continuing the secondary reaction for 10-20 min; step four: then adding ammonium bicarbonate aqueous solution for extraction, and finally recrystallizing to obtain the diacetone acrylamide.
The preparation method of the reaction additive of this example was: fully mixing chitosan and acetic acid aqueous solution according to the weight ratio of 2:5, then adding 1-5% of sodium citrate and 1-3% of sodium dodecyl sulfate in the total amount of the chitosan, fully stirring at the rotating speed of 100-300r/min for 10-20min, and obtaining the reaction additive after the stirring is finished.
The mass fraction of the acetic acid aqueous solution in this example is 10-30%.
The first-stage reaction of the present embodiment has a treatment temperature of 55-60 ℃, a reaction time of 20-30min, and a reaction rotation speed of 200-300 r/min.
The preparation method of the interfacial reactant of the present embodiment comprises: stirring and mixing 10-20 parts of silane coupling agent KH560, 1-5 parts of polyethylene glycol and 20 parts of ethanol fully, then adding 1-3 parts of tetraethoxysilane and 3 parts of modified nano-silica, performing ultrasonic dispersion treatment, and finishing the treatment to obtain the interfacial reaction agent.
The modification method of the modified nano-silica of the embodiment comprises the following steps: and (3) feeding the nano silicon dioxide into deionized water of which the volume is 2-3 times that of the nano silicon dioxide, adding hydrochloric acid to adjust the pH value to 5.0, fully dispersing, washing with water, and drying to obtain the modified nano silicon dioxide.
The power of the ultrasonic dispersion treatment in this example was 500W, and the ultrasonic time was 20 min.
The mass fraction of the ammonium bicarbonate aqueous solution in this example is 5-7%.
The mass fraction of the ammonium bicarbonate aqueous solution in this example was 6%.
Example 1: the preparation method of diacetone acrylamide of the embodiment comprises the following steps: the method comprises the following steps: mixing acrylonitrile and acetone according to the weight ratio of 1:2, and then adding concentrated sulfuric acid accounting for 10% of the total amount of the acetone; step two: then adding a reaction additive accounting for 1 percent of the total amount of the acrylonitrile, stirring and mixing to perform a first-stage reaction to obtain a body to be reacted; step three: adding 1% sodium hydroxide aqueous solution into the body to be reacted, then adding 1% interfacial reaction agent into the body to be reacted, and continuing the secondary reaction for 10 min; step four: then adding ammonium bicarbonate aqueous solution for extraction, and finally recrystallizing to obtain the diacetone acrylamide.
The preparation method of the reaction additive of this example was: fully mixing chitosan and acetic acid aqueous solution according to the weight ratio of 2:5, then adding 1% of sodium citrate and 1% of sodium dodecyl sulfate in the total amount of chitosan, fully stirring at the rotating speed of 100r/min for 10min, and obtaining the reaction additive after stirring.
The mass fraction of the acetic acid aqueous solution in this example was 10%.
The first-order reaction of this example was carried out at a treatment temperature of 55 deg.C for 20min at a reaction speed of 2000 r/min. The preparation method of the interfacial reactant of the present embodiment comprises: stirring and mixing 10 parts of silane coupling agent KH560, 1 part of polyethylene glycol and 20 parts of ethanol fully, then adding 1 part of tetraethoxysilane and 3 parts of modified nano-silica, and performing ultrasonic dispersion treatment to obtain the interface reaction agent.
The modification method of the modified nano-silica of the embodiment comprises the following steps: and (3) feeding the nano silicon dioxide into 2 times of deionized water, adding hydrochloric acid to adjust the pH value to 5.0, fully dispersing, washing with water, and drying to obtain the modified nano silicon dioxide.
The power of the ultrasonic dispersion treatment in this example was 500W, and the ultrasonic time was 20 min.
The mass fraction of the ammonium bicarbonate aqueous solution in this example was 5%.
Example 2: the preparation method of diacetone acrylamide of the embodiment comprises the following steps: the method comprises the following steps: mixing acrylonitrile and acetone according to the weight ratio of 1:2, and then adding concentrated sulfuric acid accounting for 20% of the total amount of the acetone; step two: then adding a reaction additive accounting for 3 percent of the total amount of the acrylonitrile, stirring and mixing to perform a first-stage reaction to obtain a body to be reacted; step three: adding a 5% sodium hydroxide aqueous solution into the body to be reacted, then adding an interfacial reaction agent of 3% of the body to be reacted, and continuing the secondary reaction for 20 min; step four: then adding ammonium bicarbonate aqueous solution for extraction, and finally recrystallizing to obtain the diacetone acrylamide.
The preparation method of the reaction additive of this example was: fully mixing chitosan and acetic acid aqueous solution according to the weight ratio of 2:5, then adding sodium citrate accounting for 5% of the total amount of chitosan and sodium dodecyl sulfate accounting for 3%, fully stirring at the rotating speed of 300r/min for 20min, and obtaining the reaction additive after stirring.
The mass fraction of the acetic acid aqueous solution in this example was 30%.
The first-stage reaction of this example was carried out at a temperature of 60 ℃ for 30min at a rotation speed of 300 r/min. The preparation method of the interfacial reaction agent in the embodiment comprises the following steps: stirring and mixing 20 parts of silane coupling agent KH560, 5 parts of polyethylene glycol and 20 parts of ethanol fully, then adding 3 parts of tetraethoxysilane and 3 parts of modified nano-silica, and performing ultrasonic dispersion treatment to obtain the interface reaction agent.
The modification method of the modified nano-silica of the embodiment comprises the following steps: and (3) feeding the nano silicon dioxide into deionized water of which the volume is 3 times that of the nano silicon dioxide, adding hydrochloric acid to adjust the pH value to 5.0, fully dispersing, washing with water, and drying to obtain the modified nano silicon dioxide.
The power of the ultrasonic dispersion treatment in this example was 500W, and the ultrasonic time was 20 min.
The mass fraction of the ammonium bicarbonate aqueous solution in this example was 7%.
Example 3: the preparation method of diacetone acrylamide of the embodiment comprises the following steps: the method comprises the following steps: mixing acrylonitrile and acetone according to the weight ratio of 1:2, and then adding concentrated sulfuric acid accounting for 15% of the total amount of the acetone; step two: then adding a reaction additive accounting for 2 percent of the total amount of the acrylonitrile, stirring and mixing to perform a first-stage reaction to obtain a body to be reacted; step three: adding 3% sodium hydroxide aqueous solution into the body to be reacted, then adding 2% interfacial reaction agent into the body to be reacted, and continuing the secondary reaction for 15 min; step four: then adding ammonium bicarbonate aqueous solution for extraction, and finally recrystallizing to obtain the diacetone acrylamide.
The preparation method of the reaction additive of this example was: fully mixing chitosan and acetic acid aqueous solution according to the weight ratio of 2:5, then adding sodium citrate accounting for 3% of the total amount of chitosan and sodium dodecyl sulfate accounting for 2% of the total amount of chitosan, fully stirring at the rotating speed of 200r/min for 15min, and obtaining the reaction additive after the stirring is finished.
The mass fraction of the acetic acid aqueous solution in this example was 20%.
The first-order reaction in this example was carried out at a treatment temperature of 57 ℃ for 25min at a reaction rate of 250 r/min. The preparation method of the interfacial reaction agent in the embodiment comprises the following steps: stirring and mixing 15 parts of silane coupling agent KH560, 3 parts of polyethylene glycol and 20 parts of ethanol fully, then adding 2 parts of tetraethoxysilane and 3 parts of modified nano-silica, and performing ultrasonic dispersion treatment to obtain the interface reaction agent.
The modification method of the modified nano-silica of the embodiment comprises the following steps: and (3) feeding the nano silicon dioxide into deionized water of which the volume is 2.5 times that of the nano silicon dioxide, adding hydrochloric acid to adjust the pH value to 5.0, fully dispersing, washing with water, and drying to obtain the modified nano silicon dioxide.
The power of the ultrasonic dispersion treatment in this example was 500W, and the ultrasonic time was 20 min.
The mass fraction of the ammonium bicarbonate aqueous solution in this example was 6%.
Example 4: the preparation method of diacetone acrylamide of the embodiment comprises the following steps: the method comprises the following steps: mixing acrylonitrile and acetone according to the weight ratio of 1:2, and then adding concentrated sulfuric acid accounting for 15% of the total amount of the acetone; step two: then adding a reaction additive accounting for 2 percent of the total amount of the acrylonitrile, stirring and mixing to perform a first-stage reaction to obtain a body to be reacted; step three: adding 2% sodium hydroxide aqueous solution into the body to be reacted, then adding 2% interfacial reaction agent into the body to be reacted, and continuing the secondary reaction for 10-20 min; step four: then adding ammonium bicarbonate aqueous solution for extraction, and finally recrystallizing to obtain the diacetone acrylamide.
The preparation method of the reaction additive of the embodiment comprises the following steps: fully mixing chitosan and acetic acid aqueous solution according to the weight ratio of 2:5, then adding sodium citrate accounting for 2% of the total amount of the chitosan and sodium dodecyl sulfate accounting for 1.2%, fully stirring at the rotating speed of 120r/min for 10-20min, and obtaining the reaction additive after stirring.
The mass fraction of the acetic acid aqueous solution in this example was 12%.
The first-stage reaction of this example was carried out at a treatment temperature of 56 deg.C for 22min at a reaction rate of 220 r/min. The preparation method of the interfacial reaction agent in the embodiment comprises the following steps: stirring and mixing 12 parts of silane coupling agent KH560, 2 parts of polyethylene glycol and 20 parts of ethanol fully, then adding 1.2 parts of tetraethoxysilane and 3 parts of modified nano-silica, performing ultrasonic dispersion treatment, and finishing the treatment to obtain the interface reaction agent.
The modification method of the modified nano-silica of the embodiment comprises the following steps: and (3) feeding the nano silicon dioxide into deionized water of which the volume is 2.2 times that of the nano silicon dioxide, adding hydrochloric acid to adjust the pH value to 5.0, fully dispersing, washing with water, and drying to obtain the modified nano silicon dioxide.
The power of the ultrasonic dispersion treatment in this example was 500W, and the ultrasonic time was 20 min.
The mass fraction of the ammonium bicarbonate aqueous solution in this example was 5.2%.
Example 5: the preparation method of diacetone acrylamide of the embodiment comprises the following steps: the method comprises the following steps: mixing acrylonitrile and acetone according to the weight ratio of 1:2, and then adding concentrated sulfuric acid accounting for 18% of the total amount of the acetone; step two: then adding a reaction additive accounting for 3 percent of the total amount of the acrylonitrile, stirring and mixing to perform a first-stage reaction to obtain a body to be reacted; step three: adding a 4% sodium hydroxide aqueous solution into the body to be reacted, then adding an interfacial reaction agent of 2% into the body to be reacted, and continuing the secondary reaction for 18 min; step four: then adding ammonium bicarbonate aqueous solution for extraction, and finally recrystallizing to obtain the diacetone acrylamide.
The preparation method of the reaction additive of this example was: fully mixing chitosan and acetic acid aqueous solution according to the weight ratio of 2:5, then adding sodium citrate accounting for 4% of the total amount of the chitosan and sodium dodecyl sulfate accounting for 2% of the total amount of the chitosan, fully stirring at the rotating speed of 280r/min for 18min, and obtaining the reaction additive after the stirring is finished.
The mass fraction of the acetic acid aqueous solution in this example was 28%.
The first-stage reaction of this example was carried out at a treatment temperature of 58 ℃ for 28min at a reaction rate of 280 r/min. The preparation method of the interfacial reaction agent in the embodiment comprises the following steps: stirring and mixing 18 parts of silane coupling agent KH560, 4 parts of polyethylene glycol and 20 parts of ethanol fully, then adding 2 parts of tetraethoxysilane and 3 parts of modified nano-silica, and performing ultrasonic dispersion treatment to obtain the interface reaction agent.
The modification method of the modified nano-silica of the embodiment comprises the following steps: and (3) feeding the nano silicon dioxide into deionized water of which the volume is 2.8 times that of the nano silicon dioxide, adding hydrochloric acid to adjust the pH value to 5.0, fully dispersing, washing with water, and drying to obtain the modified nano silicon dioxide.
The power of the ultrasonic dispersion treatment in this example was 500W, and the ultrasonic time was 20 min.
The mass fraction of the ammonium bicarbonate aqueous solution in this example was 6%.
Example 1-5 reaction yield determination method refer to chinese patent 1911966a, a method for determining reaction yield of a pretreatment method for improving starch reaction yield and modified starch stability;
| reaction yield (%) | |
| Example 1 | 78.2 |
| Example 2 | 78.1 |
| Example 3 | 78.5 |
| Example 4 | 78.0 |
| Example 5 | 70.1 |
The reaction yield of the products prepared in the examples 1-5 reaches more than 70%, and the highest reaction yield of the products prepared in the example 3 can reach 78.5%, so that the reaction yield is excellent.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. The preparation method of diacetone acrylamide is characterized by comprising the following steps: the method comprises the following steps: mixing acrylonitrile and acetone according to the weight ratio of 1:2, and then adding concentrated sulfuric acid with the total amount of 10-20% of acetone; step two: then adding a reaction additive accounting for 1-3% of the total amount of the acrylonitrile, stirring and mixing to perform a first-stage reaction to obtain a body to be reacted; step three: adding 1-5% sodium hydroxide aqueous solution into the body to be reacted, then adding 1-3% interfacial agent into the body to be reacted, and continuing the secondary reaction for 10-20 min; step four: then adding ammonium bicarbonate aqueous solution for extraction, and finally recrystallizing to obtain the diacetone acrylamide; the preparation method of the reaction additive comprises the following steps: fully mixing chitosan and acetic acid aqueous solution according to the weight ratio of 2:5, then adding sodium citrate accounting for 1-5% of the total amount of chitosan and sodium dodecyl sulfate accounting for 1-3%, fully stirring at the rotating speed of 100-300r/min for 10-20min, and obtaining a reaction additive after the stirring is finished; the preparation method of the interfacial reaction agent comprises the following steps: stirring and mixing 10-20 parts of silane coupling agent KH560, 1-5 parts of polyethylene glycol and 20 parts of ethanol fully, then adding 1-3 parts of tetraethoxysilane and 3 parts of modified nano silicon dioxide, performing ultrasonic dispersion treatment, and finishing the treatment to obtain the interfacial reaction agent.
2. The method for preparing diacetone acrylamide as claimed in claim 1, wherein the mass fraction of the aqueous acetic acid solution is 10-30%.
3. The method as claimed in claim 1, wherein the first-stage reaction is carried out at a temperature of 55-60 deg.C for 20-30min at a rotation speed of 200-300 r/min.
4. The preparation method of diacetone acrylamide as claimed in claim 1, wherein the modification method of the modified nano silica comprises: and (3) feeding the nano silicon dioxide into deionized water of which the volume is 2-3 times that of the nano silicon dioxide, adding hydrochloric acid to adjust the pH value to 5.0, fully dispersing, washing with water, and drying to obtain the modified nano silicon dioxide.
5. The method for preparing diacetone acrylamide as claimed in claim 4, wherein the ultrasonic dispersion treatment is carried out at a power of 500W for a period of 20 min.
6. The method for preparing diacetone acrylamide as claimed in claim 1, wherein the mass fraction of the aqueous ammonium bicarbonate solution is 5-7%.
7. The method according to claim 6, wherein the mass fraction of the aqueous ammonium bicarbonate solution is 6-7%.
8. The method according to claim 7, wherein the mass fraction of the aqueous ammonium bicarbonate solution is 6%.
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| SU1456407A1 (en) * | 1987-04-13 | 1989-02-07 | Ярославский политехнический институт | Method of producing diacetone acrylamide |
| US20100217042A1 (en) * | 2007-05-11 | 2010-08-26 | Sascha Braune | process for working up diacetone acrylamide solutions for the preparation of pure diacetone acrylamide |
| CN104030939A (en) * | 2014-07-02 | 2014-09-10 | 山东天一化学股份有限公司 | Method for preparing diacetone acrylamide through diacetone alcohol |
| CN106565519A (en) * | 2016-11-01 | 2017-04-19 | 潍坊科麦化工有限公司 | Preparation method of diacetone acrylamide |
| CN110204452A (en) * | 2019-06-03 | 2019-09-06 | 万华化学集团股份有限公司 | A kind of preparation method of the Diacetone Acrylamide of low acrylamide content |
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2022
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US3649688A (en) * | 1969-07-10 | 1972-03-14 | Lubrizol Corp | Method for the preparation of n-3-oxohydrocarbon-substituted acrylamides |
| US4239885A (en) * | 1978-06-28 | 1980-12-16 | American Cyanamid Company | Process for the preparation of diacetone acrylamide |
| SU1456407A1 (en) * | 1987-04-13 | 1989-02-07 | Ярославский политехнический институт | Method of producing diacetone acrylamide |
| US20100217042A1 (en) * | 2007-05-11 | 2010-08-26 | Sascha Braune | process for working up diacetone acrylamide solutions for the preparation of pure diacetone acrylamide |
| CN104030939A (en) * | 2014-07-02 | 2014-09-10 | 山东天一化学股份有限公司 | Method for preparing diacetone acrylamide through diacetone alcohol |
| CN106565519A (en) * | 2016-11-01 | 2017-04-19 | 潍坊科麦化工有限公司 | Preparation method of diacetone acrylamide |
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