CN1045577A - Process of azo di-formamide - Google Patents
Process of azo di-formamide Download PDFInfo
- Publication number
- CN1045577A CN1045577A CN 89108525 CN89108525A CN1045577A CN 1045577 A CN1045577 A CN 1045577A CN 89108525 CN89108525 CN 89108525 CN 89108525 A CN89108525 A CN 89108525A CN 1045577 A CN1045577 A CN 1045577A
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- Prior art keywords
- dicarbonamide
- hydrazo
- cellmic
- present
- hydrazine
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention is the method that adopts alkaline composite technology preparation to produce the intermediate-hydrazo-dicarbonamide of Cellmic C 121 (AC whipping agent).Adopting urea and hydrazine is raw material, in alkaline medium, and reflux 4-8 hour, separate out the product hydrazo-dicarbonamide through cooling, hydrazo-dicarbonamide promptly gets Cellmic C 121 through oxidation.
The present invention has avoided the technology of the synthetic hydrazo-dicarbonamide of acid condensation of common employing to cause the serious disadvantage of equipment corrosion, has saved facility investment, has reduced cost, is suitable for suitability for industrialized production.
Description
The invention belongs to the organic compound preparation method.
Cellmic C 121, common name " AC " whipping agent is to use one of whipping agent the most widely.It can be used as the normal pressure or the pressure expansion of polyvinyl chloride, polyethylene, chloroprene rubber, natural rubber and silicon rubber.The tasteless nondiscoloration of plastics with this product foaming.
The method of producing Cellmic C 121 often adopted acid condensation process in the past, promptly used urea and hydrazine in the sulfuric acid medium liquid, and reflux is condensed into hydrazo-dicarbonamide, and hydrazo-dicarbonamide generates Cellmic C 121 through peroxidation.Because sulfuric acid and the by product-ammonium sulfate that produces in reaction process all have extremely strong corrodibility, cause structure deteriorate serious.Especially at high temperature just even more serious to the corrosion of reactor.In addition, the by product-ammonium sulphate waste liquor that generates during acid condensation hydrazo-dicarbonamide also causes certain pollution to environment.
The object of the present invention is to provide one little to equipment (reactor etc.) corrosion, the method that is suitable for the suitability for industrialized production Cellmic C 121 that environmental pollution is little.
The present invention adopts alkaline condensation to synthesize hydrazo-dicarbonamide, generates the method for Cellmic C 121 then through oxidation.Reaction formula is:
The mole ratio of hydrazine and urea is controlled at 1: 2～4, and the concentration of hydrazine is 20-60%, under the condition of reflux, and condensation 4-8 hour, be cooled to room temperature, filter, wash hydrazo-dicarbonamide with water and remove NH
4OH, drying.Promptly get purity and be not less than 98%,, fusing point is 250 ± 3 ℃ a hydrazo-dicarbonamide.The byproduct of reaction ammonia absorbs with acid solution by conduit, can recycle.Hydrazo-dicarbonamide promptly gets Cellmic C 121 through oxidation.
The success that experiment showed, the synthetic hydrazo-dicarbonamide technology of alkaline condensation not only makes prolong tens of times the work-ing life of reactor, but also has reduced environmental pollution, and the quality of hydrazo-dicarbonamide and yield all are better than the technology of the synthetic hydrazo-dicarbonamide of acid condensation.The by product ammonia can also be recycled.The success of the synthetic hydrazo-dicarbonamide technology of alkalescence condensation has very big practical value.
Example: get urea (technical grade) 288 grams, place in the there-necked flask of 11 liter, bottleneck is equipped with reflux exchanger.Electronic stirring and thermometer.Condenser is suitable for reading to connect a conduit so that absorb ammonia.In bottle, add hydrazine solution (25%NH
2NH
2) 200 milliliters, hydrazine solution will slowly add in batches.Under agitation refluxed 4-8 hour, till no longer including ammonia and emerging.Reaction finishes postcooling to room temperature, and hydrazo-dicarbonamide is leached, and washes the NH of absorption with water
4By products such as OH, drying gets the hydrazo-dicarbonamide that 160-170 restrains 250 ± 3 ℃ of fusing points approximately.Hydrazo-dicarbonamide gets Cellmic C 121 through chlorine oxidation.Product purity is more than 98%, and gas forming amount restrains at 210mL/, can pulverize to reach 400 purpose particles.
Claims (1)
1, the present invention system is about the preparation method of intermediate one hydrazo-dicarbonamide of synthetic Cellmic C 121 (AC whipping agent).It is characterized in that with urea and hydrazine be raw material, in alkaline medium, carry out condensation, can make hydrazo-dicarbonamide through reflux.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89108525 CN1045577A (en) | 1989-11-15 | 1989-11-15 | Process of azo di-formamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89108525 CN1045577A (en) | 1989-11-15 | 1989-11-15 | Process of azo di-formamide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1045577A true CN1045577A (en) | 1990-09-26 |
Family
ID=4857607
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89108525 Pending CN1045577A (en) | 1989-11-15 | 1989-11-15 | Process of azo di-formamide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1045577A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1095390C (en) * | 1996-05-30 | 2002-12-04 | 郑守樽 | Method and apparatus for eliminating acid mist and acid liquor created by ADC foaming agent condensation process |
| CN102584640A (en) * | 2011-12-27 | 2012-07-18 | 杭州海虹精细化工有限公司 | Process for continuously producing azodicarbonamide (ADC) foaming agents in multi-kettle serial-connection mode |
| CN101184765B (en) * | 2005-05-26 | 2013-06-26 | 罗狄亚化学公司 | Preparation method of organosilicium compounds |
-
1989
- 1989-11-15 CN CN 89108525 patent/CN1045577A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1095390C (en) * | 1996-05-30 | 2002-12-04 | 郑守樽 | Method and apparatus for eliminating acid mist and acid liquor created by ADC foaming agent condensation process |
| CN101184765B (en) * | 2005-05-26 | 2013-06-26 | 罗狄亚化学公司 | Preparation method of organosilicium compounds |
| CN102584640A (en) * | 2011-12-27 | 2012-07-18 | 杭州海虹精细化工有限公司 | Process for continuously producing azodicarbonamide (ADC) foaming agents in multi-kettle serial-connection mode |
| CN102584640B (en) * | 2011-12-27 | 2016-06-15 | 杭州海虹精细化工有限公司 | The technique that a kind of multi-floating bodies formula produces ADC foaming agent continuously |
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Legal Events
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| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |