CN103011100A - Method for synthesizing hydrazine hydrate through high-efficiency mixing by using structured packing - Google Patents
Method for synthesizing hydrazine hydrate through high-efficiency mixing by using structured packing Download PDFInfo
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- CN103011100A CN103011100A CN2012105446895A CN201210544689A CN103011100A CN 103011100 A CN103011100 A CN 103011100A CN 2012105446895 A CN2012105446895 A CN 2012105446895A CN 201210544689 A CN201210544689 A CN 201210544689A CN 103011100 A CN103011100 A CN 103011100A
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Abstract
The invention relates to a method for synthesizing hydrazine hydrate through high-efficiency mixing by using structured packing. The method comprises the following steps of: a, firstly, weighing a certain mass of urea, adding water to prepare a urea solution with the concentration being 350-450g/L, adding magnesium sulfate, accounting for 1-2% relative to the mass of the urea, to serve as a catalyst, and completely dissolving the magnesium sulfate; b, importing chlorine into a 25% sodium hydroxide solution to prepare a sodium hypochlorite solution with the available chlorine concentration being 105-115g/L and the free alkali concentration being 125-135g/L; c, mixing the urea solution and the sodium hypochlorite solution in a pipeline in which the structured packing is added by a pump according to a proportion, introducing the mixed materials into a heat exchanger, and controlling the temperature by adopting frozen saline water; d, controlling the temperature of the materials to be below 20 DEG C by controlling the flow rate of the frozen saline water; e, after the mixed materials are discharged from a structured packing mixing section, introducing the mixed materials into a hydrazine hydrate thermal reactor, and rapidly raising the temperature to 108-135 DEG C; and f, after the materials flow out of the thermal reactor, introducing the materials into a hydrazine hydrate collection tank. The method disclosed by the invention has the beneficial effects that on the premise of not adding other equipment or changing original equipment, a mixing effect better than that of a static mixer can be obtained just by adding the structured packing in the pipeline, and the method is simple and feasible.
Description
Technical field
The present invention relates to the oxo-synthesis of hydrazine hydrate field, be specifically related to a kind of method of utilizing structured packing high efficient mixed oxo-synthesis of hydrazine hydrate.
Background technology
Hydrazine hydrate has another name called hydrazine hydrate, is the monohydrate (N2H4H2O) of hydrazine, and outward appearance is colourless transparent liquid, can mix arbitrarily with water, alcohol, is insoluble to EC.Hydrazine hydrate is a kind of important fine-chemical intermediate, is widely used in synthetic pesticide, medicine, water treatment, whipping agent, initiator and solidifying agent etc., and exploitation prospect is wide.
At present the method for domestic production hydrazine hydrate mostly is Wyler's process production, be to adopt urea and clorox in basic solution, to react to obtain hydrazine hydrate, the hydrazine hydrate yield that the method obtains at 75-80%(in Cl) between.The present domestic yield that also has a lot of scholars and manufacturer to take effective measure to improve hydrazine hydrate, find that the principal element that affects the hydrazine hydrate yield is: after 1, urea and clorox mix, meeting moment heat release, temperature surpasses 30 ℃ of clorox, and the self-decomposition reaction can occur, reduced the concentration of available chlorine, simultaneously, clorox also can be decomposed into sodium chlorate and sodium-chlor, and sodium chlorate can be decomposed the hydrazine hydrate that has generated, thereby the yield of hydrazine hydrate is reduced.In order to prevent that the excess Temperature clorox from decomposing, currently used method is, urea and clorox are squeezed into static mixer with pump carry out cold reaction, after enter in the thermal reactor, the temperature of thermal reactor is 108-135 ℃, obtain hydrazine hydrate solution after the rapid reaction fully, the method can be increased to the yield of hydrazine hydrate 80%-85%(in Cl).
Summary of the invention
The object of the invention is to overcome the deficiency that prior art exists, and a kind of method of utilizing structured packing high efficient mixed oxo-synthesis of hydrazine hydrate is provided.The method is to add structured packing as the mixing device of clorox and urea in reacting pipe, pass through high efficient mixed, make clorox and urea can be rapidly, continuously, evenly mix, avoid causing local heating because mixing inequality, cause raw material to decompose and the yield of hydrazine hydrate descended.
The present invention proposes a kind of method of utilizing the continuous oxo-synthesis of hydrazine hydrate of filler high efficient mixed, the method adopts the way of adding structured packing in pipeline, replace original static mixer, urea and clorox are carried out high efficient mixed, material enters thermal reactor after mixing, obtain hydrazine hydrate solution after the reaction that is rapidly heated.Adopt the structured packing mixed phase than static mixing technological advantage be: the structured packing size is identical with internal diameter of the pipeline, does not have short circuit phenomenon.Its flow channels is a lot, its every layer each other 90 degree placement of structured packing, can guarantee the quick and complete mixing of raw material, turndown ratio is large, equal energy high efficient mixed in the scope that is not less than design production capacity 20%, avoided that static mixer is slow owing to mixing, mixed effect is subjected to flow rate effect causing mixing inequality causes localized hyperthermia, clorox generation decomposition reaction greatly.This device does not need additionally to increase other power-equipments, and is simple in the situation that does not change original system, just can guarantee the high efficient mixed of raw material, reduced the generation of side reaction, thereby can improve the yield of hydrazine hydrate.
The objective of the invention is to finish by following technical solution.This method of utilizing the continuous oxo-synthesis of hydrazine hydrate of structured packing high efficient mixed, the method comprises following step:
A. the urea of weighing certain mass at first adds water, is mixed with the urea soln of 350 ~ 450g/L, and the sal epsom that adds urea quality 1% ~ 2% is as catalyzer, and fully dissolving;
B. pass into chlorine in 25% sodium hydroxide solution, making effective chlorine density is 105-115g/L, the chlorine bleach liquor of free alkali concentration 125-135g/L;
C. urea soln and time sodium solution proportionally by having added the pipe-line blending of structured packing, enter interchanger by pump after the mixing, adopt the chilled brine temperature control;
D. by the flow velocity of chilled brine, the control temperature of charge remains on below 20 ℃;
E. material mixes out the laggard hydrazine hydrate thermal reactor that enters from the structured packing mixing section, and is warming up to rapidly 108-135 ℃;
F. material flows out the laggard hydrazine hydrate receiving tank that enters from thermal reactor.
As preferably, the structured packing of interpolation is ripple type or non-ripple type, is to arrange by even geometricdrawing, the filler of neatly piling up.
As preferably, the structured packing of interpolation is adopted the filler stack of single or multiple lift unit to fill and is installed, the number of plies be 1 layer or more than, and the stack between every layer is arranged according to 90 degree dislocation.
As preferably, the length of the structured packing of interpolation part is 1cm ~ 10m, according to material in ducted flow velocity, material viscosity and duct length increase and decrease.
As preferably, the structured packing material of interpolation is one or more of metal structured packing, plastic regular packing material, ceramic filler and carbon fibre regular filler.
As preferably, have before and after the filler and support and hold-down gear, fixedly filler.The structured packing of adding should be substantially and internal diameter of the pipeline big or small on an equal basis, apertured with internal diameter of the pipeline, seal with seal strip, avoid feed liquid to walk short circuit, incomplete mixing.In the pipeline of mixed occurrence in the material continuous conveying process, can realize continuous operation.
Beneficial effect of the present invention is: in the situation that does not increase other equipment or existing equipment is changed, only need to add structured packing in pipeline, just can obtain the mixed effect that many more effective than static mixer, method is simple.
Embodiment
The present invention is further elaborated below by embodiment, and embodiment will help to understand better the present invention, but the present invention is not limited only to following embodiment.
Embodiment 1
At first, compound concentration is the urea soln of 375g/L, the sal epsom of adding 1.5% is as catalyzer, and be in 25% sodium hydroxide solution with concentration, pass into chlorine, being prepared into effective chlorine density is 110g/L, free alkali concentration is the chlorine bleach liquor of 130g/L, with the charging proportioning of under meter control urea and clorox, according to the flow velocity mixing (volumetric flow rate is 55L/h, caliber DN10) of 0.3m/s, the mixing zone length of adding structured packing is 10cm, urea and clorox enter thermal reactor after mixing, reactor is warming up to rapidly 108 ℃, and material flows out the laggard hydrazine hydrate receiving tank that enters.After testing, the yield of hydrazine hydrate is that 85.6%(is in Cl).
Embodiment 2
At first, compound concentration is the urea soln of 375g/L, the sal epsom of adding 1.5% is as catalyzer, and be in 25% sodium hydroxide solution with concentration, pass into chlorine, being prepared into effective chlorine density is 110g/L, free alkali concentration is the chlorine bleach liquor of 130g/L, with the charging proportioning of under meter control urea and clorox, according to the flow velocity mixing (total treatment capacity is 150L/h, caliber DN10) of 0.8m/s, the mixing zone length of adding structured packing is 10cm, urea and clorox enter thermal reactor after mixing, reactor is warming up to rapidly 108 ℃, and material flows out the laggard hydrazine hydrate receiving tank that enters.After testing, the yield of hydrazine hydrate is that 87.3%(is in Cl).
Embodiment 3
At first, compound concentration is the urea soln of 375g/L, the sal epsom of adding 1.5% is as catalyzer, and be in 25% sodium hydroxide solution with concentration, pass into chlorine, being prepared into effective chlorine density is 110g/L, free alkali concentration is the chlorine bleach liquor of 130g/L, with the charging proportioning of under meter control urea and clorox, according to the flow velocity mixing (total treatment capacity is 185L/h, caliber DN10) of 1.0m/s, the mixing zone length of adding structured packing is 6cm, urea and clorox enter thermal reactor after mixing, reactor is warming up to rapidly 108 ℃, and material flows out the laggard hydrazine hydrate receiving tank that enters.After testing, the yield of hydrazine hydrate is that 87.8%(is in Cl).
Embodiment 4
At first, compound concentration is the urea soln of 375g/L, the sal epsom of adding 1.5% is as catalyzer, and be in 25% sodium hydroxide solution with concentration, pass into chlorine, being prepared into effective chlorine density is 110g/L, free alkali concentration is the chlorine bleach liquor of 130g/L, with the charging proportioning of under meter control urea and clorox, according to the flow velocity mixing (total treatment capacity is 240L/h, caliber DN10) of 1.3m/s, the mixing zone length of adding structured packing is 6cm, urea and clorox enter thermal reactor after mixing, reactor is warming up to rapidly 108 ℃, and material flows out the laggard hydrazine hydrate receiving tank that enters.After testing, the yield of hydrazine hydrate is that 88.2%(is in Cl).
Embodiment 5
At first, compound concentration is the urea soln of 375g/L, the sal epsom of adding 1.5% is as catalyzer, and be in 25% sodium hydroxide solution with concentration, pass into chlorine, being prepared into effective chlorine density is 110g/L, and free alkali concentration is the chlorine bleach liquor of 130g/L, with the charging proportioning of under meter control urea and clorox, mix according to the flow velocity of 1m/s that (total treatment capacity is 36m
3/ h, caliber DN200), the mixing zone length of adding structured packing is 1m, and urea and clorox enter thermal reactor after mixing, and reactor is warming up to rapidly 108 ℃, and material flows out the laggard hydrazine hydrate receiving tank that enters.After testing, the yield of hydrazine hydrate is that 87.3%(is in Cl).
Claims (5)
1. method of utilizing the continuous oxo-synthesis of hydrazine hydrate of structured packing high efficient mixed, it is characterized in that: the method comprises following step:
A. the urea of weighing certain mass at first adds water, is mixed with the urea soln of 350 ~ 450g/L, and the sal epsom that adds urea quality 1% ~ 2% is as catalyzer, and fully dissolving;
B. pass into chlorine in 25% sodium hydroxide solution, making effective chlorine density is 105-115g/L, the chlorine bleach liquor of free alkali concentration 125-135g/L;
C. urea soln and time sodium solution proportionally by having added the pipe-line blending of structured packing, enter interchanger by pump after the mixing, adopt the chilled brine temperature control;
D. by the flow velocity of chilled brine, the control temperature of charge remains on below 20 ℃;
E. material mixes out the laggard hydrazine hydrate thermal reactor that enters from the structured packing mixing section, and is warming up to rapidly 108-135 ℃;
F. material flows out the laggard hydrazine hydrate receiving tank that enters from thermal reactor.
2. the method for utilizing the continuous oxo-synthesis of hydrazine hydrate of structured packing high efficient mixed according to claim 1, it is characterized in that: the structured packing of interpolation is ripple type or non-ripple type, is to arrange by even geometricdrawing, the filler of neatly piling up.
3. the method for utilizing the continuous oxo-synthesis of hydrazine hydrate of structured packing high efficient mixed according to claim 1 and 2, it is characterized in that: the structured packing of interpolation is adopted the filler stack of single or multiple lift unit to fill and is installed, the number of plies be 1 layer or more than, and the stack between every layer is arranged according to 90 degree dislocation.
4. the method for utilizing the continuous oxo-synthesis of hydrazine hydrate of structured packing high efficient mixed according to claim 1 and 2 is characterized in that: the length of the structured packing part of interpolation is 1cm ~ 10m, according to material in ducted flow velocity, material viscosity and duct length increase and decrease.
5. the method for utilizing the continuous oxo-synthesis of hydrazine hydrate of structured packing high efficient mixed according to claim 1 and 2, it is characterized in that: the structured packing material of interpolation is one or more of metal structured packing, plastic regular packing material, ceramic filler and carbon fibre regular filler.
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| CN2012105446895A CN103011100A (en) | 2012-12-14 | 2012-12-14 | Method for synthesizing hydrazine hydrate through high-efficiency mixing by using structured packing |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106219504A (en) * | 2016-07-14 | 2016-12-14 | 北京国环清华环境工程设计研究院有限公司 | The method preparing hydrazine for raw material with urine |
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| CN201239612Y (en) * | 2008-06-30 | 2009-05-20 | 沈树荣 | Static state fluid mixer |
| CN201848207U (en) * | 2010-09-19 | 2011-06-01 | 南通利华农化有限公司 | Gas/gas and gas/liquid or liquid/liquid static mixer |
| CN102153056A (en) * | 2011-02-15 | 2011-08-17 | 杭州海虹精细化工有限公司 | Technology for continuously producing hydrazine hydrate |
| CN102774818A (en) * | 2012-07-24 | 2012-11-14 | 杭州海虹精细化工有限公司 | Method for circularly producing hydrazine hydrate by using causticizing method |
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- 2012-12-14 CN CN2012105446895A patent/CN103011100A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201239612Y (en) * | 2008-06-30 | 2009-05-20 | 沈树荣 | Static state fluid mixer |
| CN201848207U (en) * | 2010-09-19 | 2011-06-01 | 南通利华农化有限公司 | Gas/gas and gas/liquid or liquid/liquid static mixer |
| CN102153056A (en) * | 2011-02-15 | 2011-08-17 | 杭州海虹精细化工有限公司 | Technology for continuously producing hydrazine hydrate |
| CN102774818A (en) * | 2012-07-24 | 2012-11-14 | 杭州海虹精细化工有限公司 | Method for circularly producing hydrazine hydrate by using causticizing method |
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| 郑土英: "ADC发泡剂清洁生产工艺技术研究", 《中国硕士学位论文全文数据库（电子期刊）工程科技Ⅰ辑》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106219504A (en) * | 2016-07-14 | 2016-12-14 | 北京国环清华环境工程设计研究院有限公司 | The method preparing hydrazine for raw material with urine |
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Application publication date: 20130403 |