CN101104592A - Method for preparing N-hydroxymethyl alkyl acrylamide - Google Patents
Method for preparing N-hydroxymethyl alkyl acrylamide Download PDFInfo
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- CN101104592A CN101104592A CNA2007100257519A CN200710025751A CN101104592A CN 101104592 A CN101104592 A CN 101104592A CN A2007100257519 A CNA2007100257519 A CN A2007100257519A CN 200710025751 A CN200710025751 A CN 200710025751A CN 101104592 A CN101104592 A CN 101104592A
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Abstract
The present invention discloses an environmental-friendly preparation method of N-hydroxymethyl-alkyl acrylamide, which is simple in process and mainly comprises the following steps: formaldehyde generating agent is added to the aqueous solution of alkyl acrylamide for reaction; in the reaction process, alkaline substances are used to control the pH value of the reaction solution between 9.0 and 11.0, and the reaction temperature is controlled to 20-50 DEG C; after the reaction solution is clarified, acidic substances are added to adjust the pH value of the reaction solution between 6 to 7; finally a proper amount of polymerization inhibitor is added to the solution, so that the transparent N-hydroxymethyl-alkyl acrylamide aqueous solution product. The product prepared through the method of the invention can be used to prepare acrylic resin dry strengthening agent and humidification strengthening agent.
Description
Technical field
The present invention relates to a kind of preparation method of N-hydroxymethyl alkyl acrylamide.
Background technology
The N-hydroxymethyl alkyl acrylamide is a kind of vinyl monomer linking agent, and product form has powder-type that aqueous solution type is also arranged, and it can have more the acrylic resin dry strength agent and the wet strength agent of high combination activity with other Acrylic Acid Monomer copolymerization.In the coating agent, be used as cross-linking monomer, can improve film forming water resisting property and good solubility-resistence.At present, the relevant report that does not still have the preparation method of relevant this product of discovery.
Summary of the invention
The preparation method who the purpose of this invention is to provide the N-hydroxymethyl alkyl acrylamide of the simple and environmental protection of a kind of technology.
For achieving the above object, the technical solution used in the present invention is: the preparation method of described N-hydroxymethyl alkyl acrylamide, comprise the steps: the formaldehyde propellant joined in the aqueous solution of alkyl acrylamide and react, pH value with alkaline matter control reaction solution in the reaction process is n, and the temperature of control reaction solution is T; To reaction solution clarification, add acidic substance again the pH value of reaction solution is adjusted to 6～7.Adding quality at last is the w stopper, fully stirs, and obtains N-hydroxymethyl alkyl acrylamide aqueous products.Its reaction equation is as follows:
X is CH in the following formula
3, C
2H
5, C
3H
7
Above-mentioned alkyl acrylamide: the mol ratio of formaldehyde propellant is 1.0: 1.2～1.5: 1.0.
Described formaldehyde propellant is selected from Paraformaldehyde 96, formalin or formaldehyde gas.
The pH value n of control reaction solution is 9.0～11.0 in the described reaction process.The temperature T of reaction solution is 20～50 ℃ in the reaction process.
Described stopper is selected from: to methylol methyl-phenoxide, Resorcinol, thiodiphenylamine, Sodium Nitrite, mantoquita.In addition, the add-on w of stopper can be 0.005%～1% of reaction solution gross weight.
Alkaline matter used in reaction process is selected from: mineral alkali, organic bases, weak acid strong alkali salt.
Above-mentioned acidic substance are selected from mineral acid, organic acid, strong acid weak base salt.
The invention has the beneficial effects as follows: 1, the content of residual formaldehyde, remaining alkyl acrylamide is lower in the product that obtains of described preparation method; 2, production process environmental protection does not have any three wastes; 3, drying-free step, energy consumption is low; 4, product stock good stability, like product is easy to polymerization in the aqueous solution.
Embodiment
The invention will be further described below by specific embodiment, but the present invention should not only limit to these embodiment.
Embodiment 1
Get the 188g deionized water, join in the four-hole bottle of 2000ml, start and stir.Add Methacrylamide 485g, controlled temperature is at 38～40 ℃, is that 5% alkaline solution is regulated pH to 10.0～11.0, adding formalin 320g with mass concentration.Constantly replenish alkaline solution, make pH be controlled between 9.0～11.0, react to solution and clarify.Then, under 40 ℃ of conditions, be incubated 2～2.5 hours.Add certain amount of H
2SO
4,, stirred 5 minutes pH regulator to 6～7.Add the 0.2g stopper at last, fully stir, obtain the aqueous products of stable homogeneous.
Embodiment 2
Get the 390g deionized water, join in the four-hole bottle of 2000ml, start and stir.Add Methacrylamide 490g, controlled temperature is at 20～25 ℃, is 5% alkaline solution adjusting pH to 9.0～11.0 with mass concentration.Be warmed up to 30～35 ℃, add the 137g Paraformaldehyde 96.Be warmed up to 38～40 ℃.Constantly replenish alkaline solution, make pH be controlled between 9.0～11.0, react to solution and clarify.38 ℃ of insulations 2～3 hours, add H then
2SO
4,, stirred 5 minutes pH regulator to 6～7.Add the 0.15g stopper at last, fully stir, obtain the aqueous products of stable homogeneous.
Embodiment 3
Get the 390g deionized water, join in the four-hole bottle of 2000ml, start and stir.Add Methacrylamide 490g, controlled temperature adds the 137g Paraformaldehyde 96 at 30～35 ℃.Be warmed up to 38～40 ℃.With mass concentration is that 5% alkaline solution is regulated between pH to 9.0～11.0, reacts to solution and clarifies.38 ℃ of insulations 2～3 hours, add H then
2SO
4,, stirred 5 minutes pH regulator to 6～7.Add the 0.15g stopper at last, fully stir, obtain the aqueous products of stable homogeneous.
Claims (9)
1.N-the preparation method of hydroxymethyl alkyl acrylamide, it is characterized in that: comprise the steps: the formaldehyde propellant joined in the aqueous solution of alkyl acrylamide and react, pH value with alkaline matter control reaction solution in the reaction process is n, and the temperature of control reaction solution is T; To reaction solution clarification, add acidic substance again the pH value of reaction solution is adjusted to 6～7.Adding quality at last is the w stopper, fully stirs, and obtains N-hydroxymethyl alkyl acrylamide aqueous products.Its reaction equation is as follows:
X is CH in the following formula
3, C
2H
5, C
3H
7
2. preparation method as claimed in claim 1 is characterized in that: described alkyl acrylamide: the mol ratio of formaldehyde propellant is 1.0: 1.2～1.5: 1.0.
3. preparation method as claimed in claim 1 or 2 is characterized in that: the formaldehyde propellant is selected from Paraformaldehyde 96, formalin or formaldehyde gas.
4. preparation method as claimed in claim 1 or 2 is characterized in that: the pH value n of control reaction solution is 9.0～11.0 in the reaction process.
5. preparation method as claimed in claim 1 or 2 is characterized in that: the temperature T of reaction solution is 20～50 ℃ in the reaction process.
6. preparation method as claimed in claim 1 or 2 is characterized in that: described stopper is selected from: to methylol methyl-phenoxide, Resorcinol, thiodiphenylamine, Sodium Nitrite, mantoquita.
7. preparation method as claimed in claim 1 or 2 is characterized in that: the add-on w of stopper is 0.005%～1% of a reaction solution gross weight.
8. preparation method as claimed in claim 1 or 2 is characterized in that: alkaline matter used in reaction process is selected from: mineral alkali, organic bases, weak acid strong alkali salt.
9. preparation method as claimed in claim 1 or 2 is characterized in that: described acidic substance are selected from mineral acid, organic acid, strong acid weak base salt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100257519A CN101104592A (en) | 2007-08-02 | 2007-08-02 | Method for preparing N-hydroxymethyl alkyl acrylamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100257519A CN101104592A (en) | 2007-08-02 | 2007-08-02 | Method for preparing N-hydroxymethyl alkyl acrylamide |
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| Publication Number | Publication Date |
|---|---|
| CN101104592A true CN101104592A (en) | 2008-01-16 |
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ID=38998699
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| CNA2007100257519A Pending CN101104592A (en) | 2007-08-02 | 2007-08-02 | Method for preparing N-hydroxymethyl alkyl acrylamide |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304057A (en) * | 2011-08-25 | 2012-01-04 | 吴江市北厍盛源纺织品助剂厂 | Preparation method for N-methylolacrylamide |
| CN102304058A (en) * | 2011-08-25 | 2012-01-04 | 吴江市北厍盛源纺织品助剂厂 | Method for preparing N-hydroxymethyl acrylamide by using trichloroethylene as reaction solvent |
| CN102304059A (en) * | 2011-08-25 | 2012-01-04 | 吴江市北厍盛源纺织品助剂厂 | Method for preparing N-hydroxymethyl acrylamide by using No.200 solvent oil as solvent |
| CN102351729A (en) * | 2011-08-25 | 2012-02-15 | 吴江市北厍盛源纺织品助剂厂 | Method for preparing N-hydroxymethyl acrylamide |
-
2007
- 2007-08-02 CN CNA2007100257519A patent/CN101104592A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304057A (en) * | 2011-08-25 | 2012-01-04 | 吴江市北厍盛源纺织品助剂厂 | Preparation method for N-methylolacrylamide |
| CN102304058A (en) * | 2011-08-25 | 2012-01-04 | 吴江市北厍盛源纺织品助剂厂 | Method for preparing N-hydroxymethyl acrylamide by using trichloroethylene as reaction solvent |
| CN102304059A (en) * | 2011-08-25 | 2012-01-04 | 吴江市北厍盛源纺织品助剂厂 | Method for preparing N-hydroxymethyl acrylamide by using No.200 solvent oil as solvent |
| CN102351729A (en) * | 2011-08-25 | 2012-02-15 | 吴江市北厍盛源纺织品助剂厂 | Method for preparing N-hydroxymethyl acrylamide |
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