CN102659641A - Method for preparing azobisformamide by oxidizing biurea with sodium chlorate - Google Patents
Method for preparing azobisformamide by oxidizing biurea with sodium chlorate Download PDFInfo
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- CN102659641A CN102659641A CN2012101427166A CN201210142716A CN102659641A CN 102659641 A CN102659641 A CN 102659641A CN 2012101427166 A CN2012101427166 A CN 2012101427166A CN 201210142716 A CN201210142716 A CN 201210142716A CN 102659641 A CN102659641 A CN 102659641A
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Abstract
The invention discloses a method for preparing azobisformamide by oxidizing biurea with sodium chlorate. Biurea is oxidized to prepare the azobisformamide by using sodium chlorate as an oxidizer and iron-containing halide as a catalyst. The invention has the advantages of controllable product particle size, simple preparation technique and stable product quality, and has obvious economic and social benefits.
Description
Technical field
The present invention relates to chemical production technical field, be specifically related to the method that a kind of VAL-DROP oxidation hydrazo-dicarbonamide prepares Cellmic C 121.
Background technology
Adopt the chlorine oxidation hydrazo-dicarbonamide to prepare whipping agent Cellmic C 121 (ADC) traditionally, its advantage is that cost is low, but the difficult control of reaction end, and logical chlorine dose exceeds standard or leads to that the chlorine temperature is too high to be prone to cause whipping agent ADC to decompose; When logical chlorine dose was not enough, a small amount of hydrazo-dicarbonamide remained in and influences its quality among the whipping agent ADC.Simultaneously, the yield of this technology ADC product is low, and quality is unstable, and the effusion of acid that produces in the reaction and terminal point excessive chlorine is prone to cause problems such as environmental pollution.
Summary of the invention
The object of the present invention is to provide to the invention discloses the method that a kind of VAL-DROP oxidation hydrazo-dicarbonamide prepares Cellmic C 121, product cut size is controlled, and preparation technology is simple, and constant product quality possesses remarkable economical and social benefit.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
A kind of VAL-DROP oxidation hydrazo-dicarbonamide prepares the method for Cellmic C 121, and employing VAL-DROP is oxygenant, contains iron halide and prepares Cellmic C 121 for the catalyst oxidation hydrazo-dicarbonamide.
The described iron halide that contains is an iron(ic)chloride.
Described method may further comprise the steps: in oxidizing reactor, add hydrazo-dicarbonamide, Sodium Bromide, sulfuric acid and iron trichloride while stirring, treat that feed temperature is stable after, add VAL-DROP; Control VAL-DROP feeds intake pitch time or open cold liquid attemperation, and keeping temperature of reaction is 40-65 ℃, acidity 3.0-4.8N; Reaction 5-7h, reaction is repeatedly measured hydrazo-dicarbonamide residual volume in the feed liquid during near terminal point, treat qualified after; In time be discharged to filter vat, suction filtration, flushing, extremely neutral, filtered liq reclaims.The mass ratio of described hydrazo-dicarbonamide, VAL-DROP, Sodium Bromide is 100:28-33:0.5-1, and described VAL-DROP adopts solid directly to feed intake, and the concentration of iron trichloride is 1.5-4.2g/L in the reaction solution.
Beneficial effect of the present invention:
(1) product cut size is controlled, and preparation technology is simple, and constant product quality possesses remarkable economical and social benefit.
(2)It is domestic initiation that employing contains iron halide, and the person and surrounding environment is not worked the mischief.
(3)Adopt reaction mother liquor, catalyst recovery to reuse technology and reduce the spent acid quantity discharged, reduce environmental pollution, reduce expenses of environmental protection.
(4)Adopt the reaction that directly feeds intake of VAL-DROP solid, simplify procedures reduction labour intensity.
(5)Adopt the chemical regulation method to adjust the ADC product cut size, guarantee constant product quality.
(6)Technology ADC yield of the present invention is up to 95%.
Embodiment
Embodiment 1
Hydrazo-dicarbonamide 4000kg, temperature 50-54 ℃, 5 hours 30 minutes time, acidity 4.0N, Sodium Bromide 3kg, iron trichloride concentration 3.7g/L, VAL-DROP charging capacity 1112kg, ADC yield 95%.
Embodiment 2
Hydrazo-dicarbonamide 4000kg, temperature 50-54 ℃, 5 hours 10 minutes time, acidity 4.8N, Sodium Bromide 3kg, iron trichloride concentration 3.0g/L, VAL-DROP charging capacity 1100kg, ADC yield 92%.
Embodiment 3
Hydrazo-dicarbonamide 4000kg, temperature 45-48 ℃, 6 hours 50 minutes time, acidity 4.0N, Sodium Bromide 4kg, iron trichloride concentration 3.0g/L, VAL-DROP charging capacity 1100kg, ADC yield 95.2%.
The above is merely preferred embodiment of the present invention, and all equalizations of doing according to claim of the present invention change and modify, and all should belong to covering scope of the present invention.
Claims (4)
1. a VAL-DROP oxidation hydrazo-dicarbonamide prepares the method for Cellmic C 121, and it is characterized in that: employing VAL-DROP is oxygenant, contains iron halide and prepares Cellmic C 121 for the catalyst oxidation hydrazo-dicarbonamide.
2. VAL-DROP oxidation hydrazo-dicarbonamide according to claim 1 prepares the method for Cellmic C 121, it is characterized in that: the described iron halide that contains is an iron trichloride.
3. VAL-DROP oxidation hydrazo-dicarbonamide according to claim 1 prepares the method for Cellmic C 121, it is characterized in that: described method may further comprise the steps: in oxidizing reactor, add hydrazo-dicarbonamide, Sodium Bromide, sulfuric acid and iron trichloride while stirring; After treating that feed temperature is stable, add VAL-DROP, control VAL-DROP feeds intake pitch time or open cold liquid attemperation; Keeping temperature of reaction is 40-65 ℃, acidity 3.0-4.8N, reaction 5-7h; Reaction is repeatedly measured hydrazo-dicarbonamide residual volume in the feed liquid during near terminal point, treat qualified after, in time be discharged to filter vat; Suction filtration, flushing, extremely neutral, filtered liq reclaims.
4. VAL-DROP oxidation hydrazo-dicarbonamide according to claim 3 prepares the method for Cellmic C 121; It is characterized in that: the mass ratio of described hydrazo-dicarbonamide, VAL-DROP, Sodium Bromide is 100:28-33:0.5-1; Described VAL-DROP adopts solid directly to feed intake, and the concentration of iron trichloride is 1.5-4.2g/L in the reaction solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101427166A CN102659641A (en) | 2012-05-10 | 2012-05-10 | Method for preparing azobisformamide by oxidizing biurea with sodium chlorate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012101427166A CN102659641A (en) | 2012-05-10 | 2012-05-10 | Method for preparing azobisformamide by oxidizing biurea with sodium chlorate |
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| CN102659641A true CN102659641A (en) | 2012-09-12 |
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| CN2012101427166A Pending CN102659641A (en) | 2012-05-10 | 2012-05-10 | Method for preparing azobisformamide by oxidizing biurea with sodium chlorate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102850243A (en) * | 2012-09-24 | 2013-01-02 | 杭州海虹精细化工有限公司 | Preparation method of ADC (azodicarbonamide) foaming agent with uniform grain diameter |
| CN103058893A (en) * | 2013-01-21 | 2013-04-24 | 陈世豪 | Method for preparing azodicarbonamide by hydrogen peroxide oxidization method |
| CN103113266A (en) * | 2013-02-06 | 2013-05-22 | 陈世豪 | Method for chemically regulating particle size of azobisformamide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5398926A (en) * | 1977-02-09 | 1978-08-29 | Otsuka Chem Co Ltd | Preparation of azodicarbonamides |
| CN1045775A (en) * | 1989-03-22 | 1990-10-03 | 中国科学院福建物质结构研究所 | The high efficiency preparation method of Cellmic C 121 |
| CN101838224A (en) * | 2009-03-19 | 2010-09-22 | 华东理工大学 | Method for reducing grain size of AC foaming agent |
-
2012
- 2012-05-10 CN CN2012101427166A patent/CN102659641A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5398926A (en) * | 1977-02-09 | 1978-08-29 | Otsuka Chem Co Ltd | Preparation of azodicarbonamides |
| CN1045775A (en) * | 1989-03-22 | 1990-10-03 | 中国科学院福建物质结构研究所 | The high efficiency preparation method of Cellmic C 121 |
| CN101838224A (en) * | 2009-03-19 | 2010-09-22 | 华东理工大学 | Method for reducing grain size of AC foaming agent |
Non-Patent Citations (3)
| Title |
|---|
| 周沂: "氯酸钠氧化法制备发泡剂ADC工艺技术的研究", 《福建化工》 * |
| 杨季和和苏秉钧: "AC发泡剂新工艺研究-Ⅱ.氯酸盐氧化法", 《福州大学学报》 * |
| 陈世豪: "氯酸钠氧化法制偶氮二甲酰胺工艺的研究", 《塑料助剂》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102850243A (en) * | 2012-09-24 | 2013-01-02 | 杭州海虹精细化工有限公司 | Preparation method of ADC (azodicarbonamide) foaming agent with uniform grain diameter |
| CN103058893A (en) * | 2013-01-21 | 2013-04-24 | 陈世豪 | Method for preparing azodicarbonamide by hydrogen peroxide oxidization method |
| CN103113266A (en) * | 2013-02-06 | 2013-05-22 | 陈世豪 | Method for chemically regulating particle size of azobisformamide |
| CN103113266B (en) * | 2013-02-06 | 2014-06-04 | 陈世豪 | Method for chemically regulating particle size of azobisformamide |
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Application publication date: 20120912 |