CN104478764A - Method for reducing particle size of foaming agent - Google Patents
Method for reducing particle size of foaming agent Download PDFInfo
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- CN104478764A CN104478764A CN201410664678.XA CN201410664678A CN104478764A CN 104478764 A CN104478764 A CN 104478764A CN 201410664678 A CN201410664678 A CN 201410664678A CN 104478764 A CN104478764 A CN 104478764A
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- hydrazo
- dicarbonamide
- biurea
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- particle diameter
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Abstract
The invention discloses a method for reducing the particle size of a foaming agent. The method comprises the following steps: (1) adding water into a biurea solid to prepare a biurea suspension liquid of which the water content is 30% to 50%; (2) adding a defoaming agent of which the mass is 0.1% to 5% of the mass of the biurea into the biurea suspension liquid and adding a catalyst sodium bromide of which the mass is 1% to 5% of the mass of the biurea and a catalyst aid, namely an iron agent of which the mass is 0.5% to 2% of the mass of the biurea, and uniformly stirring; (3) continuously adding an excessive amount of an oxidant into the solution, continuously stirring at the temperature of 30 to 80 DEG C, and further stirring for 15-30 minutes after the oxidant is completely added dropwise; (4) after the reaction is ended, filtering and washing the solid, drying in an oven at the temperature of 105 DEG C until the solid is constant in weight, filtering and recycling the mother liquid. The method disclosed by the invention has the beneficial effects that the defoaming agent is taken as an additive, so that a remarkable particle size reduction effect is realized, and particles can be reduced from 40 micrometers to about 25 micrometers in particle size.
Description
Technical field
The present invention relates to ADC whipping agent field, be specifically related to a kind of method reducing whipping agent particle diameter.
Background technology
The production method of ADC whipping agent has Wyler's process, Raschig process and ketazine process.Wyler's process is domestic the most frequently used method, is urea and clorox to be reacted, and produce hydrazine hydrate, hydrazine hydrate carries out being condensed into hydrazo-dicarbonamide with urea again, and hydrazo-dicarbonamide and oxygenant generate ADC whipping agent.Current domestic general employing chlorine carries out the production of ADC whipping agent as oxygenant.But chlorine production can produce a large amount of hydrogenchloride, causes corrosion to equipment.The peroxide passivation of environmental protection is oxidized the parent being always subject to ADC whipping agent production industry and looks at, but its cost is increased, and has the too thick problem of particle diameter in process of production.
Domestic colleges and universities, institute and ADC whipping agent production industry are finding the method that can reduce ADC whipping agent particle diameter always.As improved from technique, as reduced technological temperature, Reaction time shorten, raising stirring velocity or add tensio-active agent (sodium laurylsulfonate) in reaction mother liquor.These means all can reduce the particle diameter of whipping agent to a certain extent, but reduce limitation, still do not reach ideal effect.
Tensio-active agent is added in system, after being easy to form bubble bubble formation, due to the effect of intermolecular forces, hydrophilic group in its molecule and hydrophobic group are adsorbed by walls, and formation rule arranges, and its hydrophilic group is towards aqueous phase, hydrophobic group is towards in bubble, thus elastica is formed on bubble interface, its stability is very strong, not easily breaks under normality.The appearance of foam brings numerous inconvenience to production, and first because present domestic production ADC whipping agent all adopts still reaction, the generation of foam is easy to form spray still phenomenon, still internal pressure is caused to increase, still material sprays, and gently then significant loss affects production yield, and serious even causes security incident.
Summary of the invention
The object of the invention is to solve the problem, and provide a kind of method reducing whipping agent particle diameter, it is additive that defoamer is added in a kind of employing, reduces the method for whipping agent particle diameter.
The object of the invention is to have come by following technical solution.The method of this reduction whipping agent particle diameter, the method comprises following step:
(1), in hydrazo-dicarbonamide solid add water, make the hydrazo-dicarbonamide suspension that water ratio is 30%-50%;
(2), by the defoamer of the 0.1%-5% of hydrazo-dicarbonamide quality add in above-mentioned hydrazo-dicarbonamide suspension, and add the catalyzer Sodium Bromide of 1 ~ 5% of hydrazo-dicarbonamide quality, hydrazo-dicarbonamide quality 0.5 ~ 2% promotor chalybeate, stir;
(3), in above-mentioned solution successively add excessive oxidant, constantly stir at 30-80 DEG C, to be oxidized dose dropwises, and continues to stir 15-30min;
(4), react complete, carried out by solid filtering, washing, in the baking oven of 105 DEG C, be dried to constant weight, the Recycling Mother Solution after filtration uses.
Described defoamer is one or more mixtures combined of TWEEN Series, polyvinyl ether, organo-siloxane.
Described oxygenant is the mixture of one or more combinations in chlorine, hydrogen peroxide and oxymuriate.
Beneficial effect of the present invention is: employing defoamer is additive, to the reduction Be very effective of particle diameter, can be that the particle of 40 μm is decreased to about 25 μm by particle diameter.Meanwhile, adopt the method also to solve the problem adopting traditional tensio-active agent can produce foam, improve production efficiency, ensure that production safety.
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.
The method of this reduction whipping agent particle diameter of the present invention, the method comprises following step:
(1), in hydrazo-dicarbonamide solid add water, make the hydrazo-dicarbonamide suspension that water ratio is 30%-50%;
(2), the defoamer of the 0.1%-5% of hydrazo-dicarbonamide quality is added in above-mentioned hydrazo-dicarbonamide suspension, and add the catalyzer Sodium Bromide of 1 ~ 5% of hydrazo-dicarbonamide quality, hydrazo-dicarbonamide quality 0.5 ~ 2% promotor chalybeate (iron(ic) chloride (or iron protochloride)), stir;
(3), in above-mentioned solution successively add excessive oxidant, constantly stir at 30-80 DEG C, to be oxidized dose dropwises, and continues to stir 15-30min;
(4), react complete, carried out by solid filtering, washing, in the baking oven of 105 DEG C, be dried to constant weight, the Recycling Mother Solution after filtration uses.
Described defoamer is one or more mixtures combined of TWEEN Series (preferred tween 80), polyvinyl ether, organo-siloxane.
Described oxygenant is the mixture of one or more combinations in chlorine, hydrogen peroxide and oxymuriate, preferred hydrogen peroxide.The consumption of oxygenant measures based on ratio by the theoretical chemistry mole that oxygenant and hydrazo-dicarbonamide react, and excessive 0.5%.
Embodiment 1:
Hydrazo-dicarbonamide is added water, makes the suspension liquid of water ratio 30%, and add catalyzer Sodium Bromide in suspension liquid, promotor iron(ic) chloride (or iron protochloride), and constantly stir, add the tween 80 of hydrazo-dicarbonamide quality 0.5%.Hydrogen peroxide is added dropwise in above-mentioned solution, and constantly stirs, and hydrogen peroxide dropwises, and continues stirring 0.5 hour, completely to filter ADC whipping agent, washs, dry, dry 2h at 105 DEG C.Adopt Beckman Ku Erte LS200 model particles distribution instrument to measure particle diameter, its median is 25 μm.And do blank test, blank test does not add tween 80, and the particle diameter obtained is 40 μm.
Embodiment 2:
Hydrazo-dicarbonamide is added water, makes the suspension liquid of water ratio 40%, and add catalyzer Sodium Bromide in suspension liquid, promotor iron(ic) chloride (or iron protochloride), and constantly stir, the tween 80 of hydrazo-dicarbonamide quality 5%.Hydrogen peroxide is added dropwise in above-mentioned solution, and constantly stirs, and hydrogen peroxide dropwises, and continues stirring 0.5 hour, completely to filter ADC whipping agent, washs, dry, dry 2h at 105 DEG C.Adopt Beckman Ku Erte LS200 model particles distribution instrument to measure particle diameter, its median is 20 μm.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of application claims.
Claims (3)
1. reduce a method for whipping agent particle diameter, it is characterized in that: the method comprises following step:
(1), in hydrazo-dicarbonamide solid add water, make the hydrazo-dicarbonamide suspension that water ratio is 30%-50%;
(2), by the defoamer of the 0.1%-5% of hydrazo-dicarbonamide quality add in above-mentioned hydrazo-dicarbonamide suspension, and add the catalyzer Sodium Bromide of 1 ~ 5% of hydrazo-dicarbonamide quality, hydrazo-dicarbonamide quality 0.5 ~ 2% promotor chalybeate, stir;
(3), in above-mentioned solution successively add excessive oxidant, constantly stir at 30-80 DEG C, to be oxidized dose dropwises, and continues to stir 15-30min;
(4), react complete, carried out by solid filtering, washing, in the baking oven of 105 DEG C, be dried to constant weight, the Recycling Mother Solution after filtration uses.
2. the method for reduction whipping agent particle diameter according to claim 1, is characterized in that: described defoamer is one or more mixtures combined of TWEEN Series, polyvinyl ether, organo-siloxane.
3. the method for reduction whipping agent particle diameter according to claim 1, is characterized in that: described oxygenant is the mixture of one or more combinations in chlorine, hydrogen peroxide and oxymuriate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410664678.XA CN104478764A (en) | 2014-11-19 | 2014-11-19 | Method for reducing particle size of foaming agent |
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| CN201410664678.XA CN104478764A (en) | 2014-11-19 | 2014-11-19 | Method for reducing particle size of foaming agent |
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| CN104478764A true CN104478764A (en) | 2015-04-01 |
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| CN201410664678.XA Pending CN104478764A (en) | 2014-11-19 | 2014-11-19 | Method for reducing particle size of foaming agent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111349022A (en) * | 2018-12-21 | 2020-06-30 | 江西世龙实业股份有限公司 | Preparation method of AC foaming agent with uniform and controllable particle size |
| CN114890919A (en) * | 2022-06-01 | 2022-08-12 | 宁夏日盛高新产业股份有限公司 | Production method of ADC foaming agent |
-
2014
- 2014-11-19 CN CN201410664678.XA patent/CN104478764A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 陈敏 等: "过氧化氢氧化法制备发泡剂ADC的机理研究", 《化学工程与装备》 * |
| 陈立军 等: "影响A(D) C发泡剂粒径因素的探讨", 《南昌航空工业学院学报(自然科学版)》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111349022A (en) * | 2018-12-21 | 2020-06-30 | 江西世龙实业股份有限公司 | Preparation method of AC foaming agent with uniform and controllable particle size |
| CN114890919A (en) * | 2022-06-01 | 2022-08-12 | 宁夏日盛高新产业股份有限公司 | Production method of ADC foaming agent |
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Application publication date: 20150401 |