CN104803886A - Method for producing high-purity superfine ADC (azodicarbonamide) foaming agent - Google Patents
Method for producing high-purity superfine ADC (azodicarbonamide) foaming agent Download PDFInfo
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- CN104803886A CN104803886A CN201510180432.XA CN201510180432A CN104803886A CN 104803886 A CN104803886 A CN 104803886A CN 201510180432 A CN201510180432 A CN 201510180432A CN 104803886 A CN104803886 A CN 104803886A
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- whipping agent
- adc
- adc whipping
- foaming agent
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Abstract
The invention discloses a method for producing a high-purity superfine ADC (azodicarbonamide) foaming agent. The method specifically comprises steps as follows: an ADC foaming agent is added to high-purity water, the mass ratio of the ADC foaming agent to the high-purity water is in a range of 1:(10-20), the mixture is heated to the temperature of 70-100 DEG C while stirring, the temperature is kept for 15-60 min, centrifugation is performed, and vacuum drying is performed at the temperature of 60-80 DEG C; then the purified ADC foaming agent is added to DMF (dimethylformamide), the mass ratio of the purified ADC foaming agent to the DMF is in a range of 1:(10-30), the mixture is heated to the temperature of 60-120 DEG C, the ADC foaming agent is dissolved, subjected to heat-insulated filtration for impurity removal, then cooled to the temperature of 0-10 DEG C, centrifuged, washed with the high-purity water and subjected to vacuum drying at the temperature of 80-90 DEG C, and the high-purity superfine ADC foaming agent with the purity higher than 99.9% and the particle size ranging from 0.1-10 mu m is obtained. The method has the benefits as follows: the common ADC foaming agent is added to the high-purity water, impurities capable of being dissolved in hot water are extracted, and then the high-purity superfine ADC foaming agent is produced through recrystallization by the aid of the DMF.
Description
Technical field
The present invention relates to the technical field of ADC whipping agent, be specifically related to a kind of method of producing high purity, ultra-fine ADC whipping agent.
Background technology
ADC whipping agent, Chinese: Cellmic C 121, molecular formula: C
2h
4o
2n
4, molecular weight: 116, outward appearance: pale yellow powder.It is insoluble to acid, alcohol, benzene, gasoline, pyridine equal solvent, is insoluble in water, and is dissolved in methyl sulfoxide, dimethyl formamide and sodium hydroxide solution.This product property is stablized, and can prolongedly store under normal temperature, and nontoxic, odorless itself, does not pollute, nondiscoloration, never degenerate.Foam agent ADC is that gas forming amount is maximum, and best performance is got over, broad-spectrum whipping agent.It is applied to polyvinyl chloride, polyethylene, polypropylene, polystyrene, polymeric amide, ABC and plants the synthetic materialss such as rubber.Be widely used in the foaming such as slippers, sole, shoe-pad, plastic wallpaper, top ceiling, flooring laminate, leatheroid, thermal insulation, sound-proof material.
The method of conventional production ultra-fine ADC whipping agent is sent in micronizer mill by common ADC whipping agent to carry out pulverizing to obtain ultra-fine ADC whipping agent.Ultra-fine ADC whipping agent major advantage has foaming product abscess fine and closely woven, and foaming process is stablized easy to control, and the complete impurity that foams is few.
Summary of the invention
Object of the present invention just in order to overcome the deficiency of above-mentioned technology, and provides a kind of method of producing high purity, ultra-fine ADC whipping agent, is mainly used in electronic industry, foodstuffs industry and other higher-end businesses.
The object of the invention is to have come by following technical solution.The method of this production high purity, ultra-fine ADC whipping agent, the method concrete steps are as follows: add in high purity water by ADC whipping agent, the mass ratio of ADC whipping agent and high purity water is 1:10-20, under agitation be heated to 70-100 DEG C, insulation 15-60 minute, centrifugal, vacuum-drying under 60-80 DEG C of condition; Again the ADC whipping agent after purification is added in dimethyl formamide DMF, ADC whipping agent after purification and the mass ratio of dimethyl formamide DMF are 1:10-30, be heated to 60-120 DEG C, after ADC whipping agent is dissolved, being incubated and filtering impurity, be cooled to 0-10 DEG C, centrifugal, and with after high purity water washing, under 80-90 DEG C of condition, namely vacuum-drying obtain high purity, ultra-fine ADC whipping agent, purity more than 99.9%, particle diameter 0.1-10 μm.
Extract in common ADC whipping agent the impurity that can be dissolved in hot water with high purity water, realize the object of purifying.With dimethyl formamide, the ADC whipping agent of acquisition is carried out recrystallization, realize the object of again purifying, realize the object of producing ultra-fine ADC whipping agent.With dimethyl formamide, the ADC whipping agent that 1 obtains is carried out recrystallization, ADC foaming dosage and speed of cooling can be dissolved according to dimethyl formamide, produce the ultra-fine ADC whipping agent of different-grain diameter.The present invention needs dry ADC whipping agent under vacuum-drying condition, to prevent in Optimization of Gas Flow Drying the mechanical impuritys such as airstrip ash charge dirt.
Beneficial effect of the present invention is: add in high purity water by common ADC whipping agent, extracts the impurity that can be dissolved in hot water, then uses dimethyl formamide (DMF) recrystallization production high purity, ultra-fine ADC whipping agent.
Embodiment
Below by embodiment, the present invention is further elaborated, and help is understood the present invention by embodiment better, but the present invention is not limited only to following embodiment.
Mechanism of the present invention: the ADC whipping agent product that ordinary method is produced is because of many reasons, also contain unreacted hydrazo-dicarbonamide in product, do not wash most urea, ammonium chloride, ammonium sulfate, and the mechanical impurity etc. that warm air and raw material are brought in drying process, general purity is in 97.0-98% (hydrazine hydrate reduction method).Particularly in dry ADC whipping agent process, carry out drying with warm air, the air of heating is general not through dust removal process, causes the impurity such as koniology to enter in product.And unreacted hydrazo-dicarbonamide, do not wash most ammonium chloride, ammonium sulfate, urea etc. and be dissolved in hot water.Can hydrazo-dicarbonamide, ammonium chloride, ammonium sulfate, urea etc. in extracted products by hot water, realize the object of purifying.And mechanical impurity can dissolve ADC whipping agent by dimethyl formamide, the method for filtering is taked to be removed.Be dissolved in dimethyl formamide solution at ADC whipping agent, by cooling, the ADC whipping agent be dissolved in dimethyl formamide solution is slowly separated out, thus obtains the thinner ADC whipping agent of particle diameter.
Solvent for use DMF also known as DMF, colourless, to have light amine taste liquid.Molecular formula C
3h
7nO.Molecular weight 73.10, relative density 0.9445 (25 DEG C), fusing point-61 DEG C, boiling point 152.8 DEG C.Be 100 DEG C of 62g/L through testing its solubleness, 80 DEG C of 57g/L, 50 DEG C of 42g/L, 10 DEG C of 14g/L, 0 DEG C of 6g/L.
The method of this production high purity of the present invention, ultra-fine ADC whipping agent, the method concrete steps are as follows: be that 97.0-98.0%ADC whipping agent adds in high purity water by common purity, the mass ratio of ADC whipping agent and high purity water is 1:10-20, under agitation be heated to 70-100 DEG C, insulation 15-60 minute, centrifugal, vacuum-drying under 60-80 DEG C of condition, obtaining purity is 99.0-99.5%ADC whipping agent; Again the ADC whipping agent after purification is added in dimethyl formamide DMF, ADC whipping agent after purification and the mass ratio of dimethyl formamide DMF are 1:10-30, be heated to 60-120 DEG C, after ADC whipping agent is dissolved, being incubated and filtering impurity, be cooled to 0-10 DEG C, centrifugal, and with after high purity water washing, under 80-90 DEG C of condition, namely vacuum-drying obtain high purity, ultra-fine ADC whipping agent, purity more than 99.9%, particle diameter 0.1-10 μm.
Embodiment 1:
(1) by common purity be 97.%ADC whipping agent 100Kg, add in 1500Kg high purity water, under agitation be heated to 70-100 DEG C, insulation 15-60 minute, make hydrazo-dicarbonamide, ammonium chloride, ammonium sulfate, urea etc. be dissolved in the high purity water of heat, send in whizzer centrifugal, vacuum-drying under 60-80 DEG C of condition, obtain 95.2Kg, purity is 99.2%ADC whipping agent.
(2) the ADC whipping agent 1Kg after (1) being purified adds in 20Kg dimethyl formamide (DMF), be heated to 100 DEG C, make ADC whipping agent dissolve, insulation filter (accurate filter with filtering accuracy 0.1 μm) remove mechanical impurity, be cooled to 0 DEG C again, send in whizzer centrifugal, and with after high purity water washing, under 80-90 DEG C of condition, namely vacuum-drying obtain 0.8Kg, and purity is 99.92%ADC whipping agent.Particle size distribution range 0.1-4.5 μm, median size 3.85 μm.
Embodiment 2:
ADC whipping agent 0.7Kg after embodiment one (1) being purified adds in 20Kg dimethyl formamide (DMF), be heated to 80 DEG C, make ADC whipping agent dissolve, insulation filter (accurate filter with filtering accuracy 0.1 μm) remove mechanical impurity, progressively cool to 0 DEG C again, send in whizzer centrifugal, and with after high purity water washing, under 80-90 DEG C of condition, namely vacuum-drying obtain 0.52Kg, and purity is 99.94%ADC whipping agent.Particle size distribution range 0.03-3.8 μm, median size 2.43 μm.
Claims (2)
1. produce the method for high purity, ultra-fine ADC whipping agent for one kind, it is characterized in that: the method concrete steps are as follows: ADC whipping agent is added in high purity water, the mass ratio of ADC whipping agent and high purity water is 1:10-20, under agitation be heated to 70-100 DEG C, insulation 15-60 minute, centrifugal, vacuum-drying under 60-80 DEG C of condition; Again the ADC whipping agent after purification is added in dimethyl formamide DMF, ADC whipping agent after purification and the mass ratio of dimethyl formamide DMF are 1:10-30, be heated to 60-120 DEG C, after ADC whipping agent is dissolved, being incubated and filtering impurity, be cooled to 0-10 DEG C, centrifugal, and with after high purity water washing, under 80-90 DEG C of condition, namely vacuum-drying obtain high purity, ultra-fine ADC whipping agent, purity more than 99.9%, particle diameter 0.1-10 μm.
2. the method for production high purity according to claim 1, ultra-fine ADC whipping agent, it is characterized in that: be 97.%ADC whipping agent 100Kg by common purity, add in 1500Kg high purity water, under agitation be heated to 70-100 DEG C, insulation 15-60 minute, sends in whizzer centrifugal, vacuum-drying under 60-80 DEG C of condition, obtain 95.2Kg, purity is 99.2%ADC whipping agent; ADC whipping agent 1Kg after purifying is added in 20Kg dimethyl formamide DMF, be heated to 100 DEG C, ADC whipping agent is made to dissolve, be incubated and filter mechanical impurity, be cooled to 0 DEG C again, send in whizzer centrifugal, and with after high purity water washing, under 80-90 DEG C of condition, namely vacuum-drying obtain 0.8Kg, purity is 99.92%ADC whipping agent, particle size distribution range 0.1-4.5 μm, median size 3.85 μm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510180432.XA CN104803886A (en) | 2015-04-16 | 2015-04-16 | Method for producing high-purity superfine ADC (azodicarbonamide) foaming agent |
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|---|---|---|---|
| CN201510180432.XA CN104803886A (en) | 2015-04-16 | 2015-04-16 | Method for producing high-purity superfine ADC (azodicarbonamide) foaming agent |
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| CN201510180432.XA Pending CN104803886A (en) | 2015-04-16 | 2015-04-16 | Method for producing high-purity superfine ADC (azodicarbonamide) foaming agent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276309A (en) * | 2018-03-23 | 2018-07-13 | 湖南工业大学 | A kind of foaming agent and its preparation method and application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6422851A (en) * | 1987-07-17 | 1989-01-25 | Sumitomo Electric Industries | Production of azodicarbonamide fine particles |
-
2015
- 2015-04-16 CN CN201510180432.XA patent/CN104803886A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6422851A (en) * | 1987-07-17 | 1989-01-25 | Sumitomo Electric Industries | Production of azodicarbonamide fine particles |
Non-Patent Citations (1)
| Title |
|---|
| 瞿波 等: "AC发泡剂的发泡机理以及改性", 《化工管理》, no. 11, 31 December 2013 (2013-12-31) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276309A (en) * | 2018-03-23 | 2018-07-13 | 湖南工业大学 | A kind of foaming agent and its preparation method and application |
| CN108276309B (en) * | 2018-03-23 | 2020-08-07 | 湖南工业大学 | Foaming agent and preparation method and application thereof |
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Application publication date: 20150729 |