CN1927702A - Energy-saving process of producing hydrazine hydrate - Google Patents
Energy-saving process of producing hydrazine hydrate Download PDFInfo
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- CN1927702A CN1927702A CN 200610121111 CN200610121111A CN1927702A CN 1927702 A CN1927702 A CN 1927702A CN 200610121111 CN200610121111 CN 200610121111 CN 200610121111 A CN200610121111 A CN 200610121111A CN 1927702 A CN1927702 A CN 1927702A
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Abstract
The present invention relates to energy saving hydrazine hydrate producing technological process, and features the multieffect continuous evaporating, rectifying and concentrating process of low concentration hydrazine hydrate liquid; the direct continuous solid-solid refining separation of the separated sodium carbonate and sodium chloride crystal mixture from the evaporated and concentrated slurry in a serially connected multistage hydrocyclone; the centrifugal separation process for the solid-liquid separation of the light component slurry containing miniature sodium carbonate crystal obtained through separation in the hydrocyclone; and the recovery of heat energy and hydrazine hydrate of the vapor produced in the flash evaporation at the high temperature synthetic resultant outlet in a rectifying and concentrating tower.
Description
The present invention relates to a kind of energy-saving process of producing hydrazine hydrate.
Hydrazine hydrate is a kind of important chemical material, is widely used in medicine, agricultural chemicals, the plastics blowing agent production.Present stage, main sophisticated hydrazine hydrate production technique had ketazine technology and urea hypochlorite oxidation method technology (being called for short Wyler's process technology), the hydrazine hydrate quality product of ketazine explained hereafter is relatively poor, the purification difficulty is big, and the hydrazine hydrate product of this explained hereafter mostly is applied to plastics blowing agent production; Urea hypochlorite oxidation method technology comparative maturity, good quality of product, it is the main technique method of present domestic production hydrazine hydrate, this technology (mainly contains yellow soda ash since having solved by-product abraum salt alkali mud, sodium-chlor, caustic soda) pollution problem to environment has realized comprehensively recyling, its competitive capacity has obtained promoting greatly, but all be that to utilize the rectifying of single-action consecutive evaporation that the synthetic liquid (reaction solution that urea and clorox reaction with same mole obtain) of 4% lower concentration hydration hydrazine is carried dense to 80% finished product hydrazine hydrate in the existing manufacturing technique process, its steam consumption is up to 35 tons/ton, the direct hybrid filtering of sodium chloride crystal that small crystals of sodium carbonate that evaporating, concentrating and crystallizing is separated out and particle are thick, the filter cake that will filter gained again slurrying again carries out secondary separation, because caustic soda content height, the mixed crystal that viscosity makes the thick sodium-chlor of yellow soda ash that particle is small and particle form greatly is very difficult with the direct hybrid filtering of slurries that evaporation concentration liquid forms, the mixed crystal that filtration obtains (being commonly called as saline and alkaline mud) must add a large amount of dashing in carrying out the secondary separation process, wash, top water, increased circulating mother liquor amount (both mother liquor increments) so greatly, the required steam consumption of recycling increment mother liquor is increased greatly.The high temperature flash distillation gas that is entrained with 0.4% hydrazine hydrate that this technology also will be synthesized the liquid outlet discharges after condensation, has not only polluted environment but also reduced synthesis yield, has also wasted a large amount of heat energy and water coolant simultaneously.
The deficiency that the present invention strives urea hypochlorite oxidation method hydrazine hydrate production technique proposes, and first purpose of the present invention provides a kind of steam consumption of lower concentration hydration hydrazine evaporation and concentrating technology and method of cooling-water consumption of reducing; Second purpose of the present invention provides and a kind ofly solves the mixed crystal that evaporating concentration process separates out and be difficult to filtering method; The 3rd purpose of the present invention be solve because of mixed crystal (being commonly called as " saline and alkaline mud ") carries out using when secondary is saline and alkaline to be separated a large amount of dash, wash, top water causes the method that energy consumption that the mother liquor increase causes increases that reclaims; The 4th purpose of the present invention provides a kind of wild recovery and the hydrazine hydrate recovery of heat of improving the flash distillation gas that synthesizes the liquid outlet, solves the method for the flash distillation gas pollution on the environment of synthetic liquid outlet;
The object of the present invention is achieved like this:
1, the 3%-6% lower concentration hydration hydrazine raw material liq (promptly synthetic liquid) that the reaction of chlorine bleach liquor and urea soln is obtained carries out the rectifying of multiple-effect consecutive evaporation and carries dense, except that steam-heated cal(l)andria of the first effect use, all the other each effects all utilize a secondary steam of imitating generation to evaporate under certain temperature and pressure (or vacuum tightness) as the heating gas, because the boiling point and the water of hydrazine hydrate are near, hydrazine hydrate will evaporate with water vapour, the secondary steam that 1st effective evaporator steams in the event all needs to carry out one section rectifying and carries densely entering before down the 1st effective evaporator heating chamber carries out condensing heat-exchange, hydrazine hydrate is got rid of as the raffinate of rectifying Tata still.Except that the rectifying tower top water vapour of last effect directly with the cooling water condensation, the water vapour at the rectifying tower top of several effects in front is all as evaporator heating chamber's thermal source of next effect.The water vapor condensation at rectifying tower top obtains distillates the backflow of water of condensation small part as rectifying tower, and major part is sent to and carried out ammoniacal liquor rectifying denitrogenation processing.
Comprise and use multiple-effect rectifying finishing column to carry dense again and purification the hydrazine hydrate raffinate of above-mentioned rectifying Tata still eliminating.
Comprise triple effect, economic benefits and social benefits and following current thereof and counter-current process
During enforcement vacuum pressure system, heating system, liquid level and input and output material flow are all used automatic chain control
2, the slurries that form of the yellow soda ash that evaporating concentration process is separated out and sodium-chlor mixed crystal and evaporation concentration liquid by adopt the salt pump extraction again through placed in-line multistage wet cyclone directly consolidate continuously-controlling nocturnal emission with astringent drugs system separates (being that crystals of sodium carbonate separates with sodium chloride crystal), make the wet cyclone bottom flow out heavy component and obtain more purified thick sodium chloride crystal after solid-liquid separation, the effusive light component in wet cyclone top obtains more purified small crystals of sodium carbonate after solid-liquid separation.
3, wet cyclone is separated the light component slurries that contain small crystals of sodium carbonate that obtain and carry out centrifugal settling, make small crystals of sodium carbonate realize being separated from each other with mother liquor like a cork, the heavy constituent slurries that contain thick sodium chloride crystal that wet cyclone is obtained carry out the centrifuging separation, the timely Returning evaporimeter of mother liquor send the user to carry out deep processing respectively to reduce calorific loss, to separate the elementary yellow soda ash and the first grade sodium chloride that obtain.
4, the chlorine bleach liquor is mixed by the required mol ratio of reaction with urea soln, be heated to 105 ℃ of reactions, the gas that high temperature synthesis reaction solution outlet flash distillation produces directly feeds the interior heat energy and the hydrazine hydrate of reclaiming of rectifying concentration tower of consecutive evaporation, and liquid joins in the continuous multiple-effect evaporator through behind the surge tank again.
Comprise that the synthetic liquid before the flash distillation directly is passed into independent flash distillation rectifying tower reclaims heat energy and hydrazine hydrate.
Aforesaid a kind of energy-saving process of producing hydrazine hydrate is characterized in that: the present invention uses multiple-effect consecutive evaporation rectifying extracting and concentrating technology to realize that lower concentration hydration hydrazine evaporation of liquid carries dense; The slurries that yellow soda ash that evaporation concentration is separated out and sodium-chlor mixed crystal and evaporation concentration liquid form directly through placed in-line multistage wet cyclone consolidate continuously-controlling nocturnal emission with astringent drugs system separates; Used the centrifugal settling method that wet cyclone is separated the light component slurries that contain small crystals of sodium carbonate that obtain and carried out solid-liquid separation, the timely Returning evaporimeter of mother liquor that separation obtains is to reduce calorific loss; The gas that high temperature synthesis reaction solution outlet flash distillation is produced directly feeds recovery heat energy and hydrazine hydrate in the rectifying concentration tower.
This technology greatly reduces energy consumption and the cooling-water consumption that hydrazine hydrate is produced, improved the hydrazine hydrate yield, stopped environmental pollution, solved the slurries that mixed crystal and evaporation concentration liquid forms and be difficult to filtering problem, this technology has been accomplished low equipment investment, energy consumption is low, cost is low, simple to operate, level of automation is high.
Below be embodiments of the invention:
Figure of description is seen in the embodiment technical process
Clorox caustic soda soln a enters in the synthesis reactor 7 after pump pressurization merging mixes respectively with urea soln b again, in the time of 105 ℃, carry out building-up reactions and obtain synthetic liquid c, synthetic liquid c before the flash distillation enters synthetic liquid surge tank 8, the gas d that synthetic liquid flash distillation produces feeds first and imitates rectifying tower 12 behind vapor-liquid separation tank 11, synthetic liquid e after the flash distillation is with being pumped in second single-effect evaporator 13, in vacuum tightness 35-45Kpa (absolute pressure), carrying out vacuum-evaporation rectifying during 75-80 ℃ of secondary steam temperature carries dense, the hydrazine hydrate steam f2 that the evaporation of the second single-effect evaporator top obtains enters second and imitates rectifying tower 15 after vapor-liquid separation tank 14 is handled, the water vapour g2 of rectifying tower 15 cats head enters into water coolant and carries out condenser condensing 16, what condenser 16 condensations obtained distillates water of condensation k2 after separating through vapor-liquid separation tank 17, liquid k2 small part is back to the top of rectifying tower 15, and the k2 major part is sent ammoniacal liquor rectifying tower denitrogenation processing.Gas after vapor-liquid separation tank 17 separates enters vacuum pump behind vacuum buffer tank 18.The hydrazine hydrate raffinate i2 that rectifying tower 15 tower stills are got rid of carries out reconcentration with being pumped into an effect rectifying tower 12 middle parts.
Slurries h2 after second single-effect evaporator, 13 evaporation concentration is delivered to wet cyclone 10 with the pump extraction carry out solid-liquid separation, the overflowing liquid i that wet cyclone 10 tops obtain enters continuously in first single-effect evaporator 9 and carries out revaporization, and the slurries j that the bottom obtains squeezes into elementary wet cyclone 4 by pump and carries out saline and alkaline solid controlling nocturnal emission with astringent drugs system separation.First single-effect evaporator 9 is used steam-heated cal(l)andria, when 115-120 ℃ of vacuum tightness 95-100Kpa (absolute pressure), secondary steam temperature, carry out vacuum-evaporation, the hydrazine hydrate steam f1 that the evaporation of first single-effect evaporator, 9 tops obtains enters first and imitates rectifying tower 12 after vapor-liquid separation tank 11 is handled, the water vapour g1 of rectifying tower 12 cats head is as the heating chamber thermal source of second single-effect evaporator 13, and the hydrazine hydrate raffinate k1 of the 50-60% that rectifying tower 12 tower stills are got rid of goes the finished product rectification and purification to obtain 80% hydrazine hydrate product with pumping.Second single-effect evaporator, 13 heating chambers are got rid of distillates water of condensation k1, and small part k1 is back to the top of rectifying tower 12, and distillating that most of k1 and condenser 16 are got rid of sent ammoniacal liquor rectifying tower denitrogenation processing after water of condensation k2 merges.
The heavy constituent slurries j that slurries h1 after first single-effect evaporator, 9 evaporation concentration and wet cyclone 10 taken out converge the back be pumped to elementary wet cyclone 4 carry out saline and alkaline elementary solid-controlling nocturnal emission with astringent drugs system separates (being that crystals of sodium carbonate separates with sodium chloride crystal), elementary wet cyclone 4 tops obtain light constituent 4a bottom and obtain heavy constituent 4b, 4a again through pump further consolidate with wet cyclone 5-controlling nocturnal emission with astringent drugs system separates, wet cyclone 5 tops obtain light constituent 5a bottom and obtain heavy constituent 5b, the import that 5b turns back to pump 4 separation that circulates, top light constituent 5a again through pump further consolidate with wet cyclone 6-controlling nocturnal emission with astringent drugs system separates, wet cyclone 6 tops obtain light constituent 6a bottom and obtain heavy constituent 6b, the import that bottom heavy constituent 6b turns back to pump 5 separation that circulates, top light constituent 6a separates through 2 centrifugal settlings of decanter type horizontal screw centrifuge, obtain solid sodium carbonate 2a and mother liquor 2b respectively, mother liquor 2b carries out circulating and evaporating through pump delivery to first single-effect evaporator 9.
Elementary wet cyclone 4 separate the bottom heavy constituent 4b that obtains again through pump further consolidate with wet cyclone 3-controlling nocturnal emission with astringent drugs system separates, wet cyclone 3 tops obtain light constituent 3a bottom and obtain heavy constituent 3b, the import that top light constituent 3a turns back to pump 4 separation that circulates, bottom heavy constituent 3b enters into filtering type horizontal screw centrifuge 1 and carries out centrifuging, obtain solid sodium chloride 1a and mother liquor 1b respectively, mother liquor 1b is transported to first single-effect evaporator 9 through pump with mother liquor 2b and carries out circulating and evaporating.
Description of drawings: Fig. 1 is scaled down technical process full figure, and Fig. 2 is the preceding half range process flow sheet after amplifying, and Fig. 3 is the back half range process flow sheet after amplifying.
Claims (4)
1, a kind of energy-saving process of producing hydrazine hydrate is characterized in that: use multiple-effect consecutive evaporation rectifying extracting and concentrating technology to realize that lower concentration hydration hydrazine evaporation of liquid carries dense.
2, a kind of energy-saving process of producing hydrazine hydrate, it is characterized in that: continuously the slurries that form of yellow soda ash that evaporation concentration is separated out and sodium-chlor mixed crystal and evaporation concentration liquid directly through placed in-line multistage wet cyclone consolidate-controlling nocturnal emission with astringent drugs system separates, make the wet cyclone bottom flow out heavy component and obtain more purified thick sodium chloride crystal through separation, the effusive light component in wet cyclone top obtains more purified small crystals of sodium carbonate through separation.
3, a kind of energy-saving process of producing hydrazine hydrate, it is characterized in that: wet cyclone is separated the light component slurries that contain small crystals of sodium carbonate that obtain carry out centrifugal settling, make small crystals of sodium carbonate realize being separated from each other with mother liquor like a cork, the timely Returning evaporimeter of mother liquor that separation obtains is to reduce calorific loss.
4, a kind of energy-saving process of producing hydrazine hydrate is characterized in that: the gas that high temperature synthesis reaction solution outlet flash distillation is produced directly feeds recovery heat energy and hydrazine hydrate in the rectifying concentration tower.
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| CN 200610121111 CN1927702A (en) | 2006-08-16 | 2006-08-16 | Energy-saving process of producing hydrazine hydrate |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011101A (en) * | 2012-12-14 | 2013-04-03 | 杭州海虹精细化工有限公司 | Method for preparing alkali-free low-salt high-concentration hydrazinium by hydrazine hydrate in urea treatment |
| CN103043636A (en) * | 2013-01-06 | 2013-04-17 | 杭州海虹精细化工有限公司 | Method for increasing concentration of hydrazine hydrate |
| CN103396335A (en) * | 2013-08-21 | 2013-11-20 | 上海海唇机械设备工程技术有限公司 | Content-adjustable methylhydrazine synthetic-fluid refining apparatus and method |
| CN107311129A (en) * | 2017-06-26 | 2017-11-03 | 内蒙古锦洋化学工业有限公司 | Urea method hydrazine hydrate concentrates distillation technique |
| CN110325260A (en) * | 2016-11-08 | 2019-10-11 | 曼瑟森三汽油公司 | The method for removing moisture from hydrazine |
| CN110775950A (en) * | 2019-11-21 | 2020-02-11 | 江苏索普化工股份有限公司 | Method for recovering and refining saline-alkali from high-salt hydrazine hydrate solution |
-
2006
- 2006-08-16 CN CN 200610121111 patent/CN1927702A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011101A (en) * | 2012-12-14 | 2013-04-03 | 杭州海虹精细化工有限公司 | Method for preparing alkali-free low-salt high-concentration hydrazinium by hydrazine hydrate in urea treatment |
| CN103043636A (en) * | 2013-01-06 | 2013-04-17 | 杭州海虹精细化工有限公司 | Method for increasing concentration of hydrazine hydrate |
| CN103043636B (en) * | 2013-01-06 | 2015-07-08 | 杭州海虹精细化工有限公司 | Method for increasing concentration of hydrazine hydrate |
| CN103396335A (en) * | 2013-08-21 | 2013-11-20 | 上海海唇机械设备工程技术有限公司 | Content-adjustable methylhydrazine synthetic-fluid refining apparatus and method |
| CN103396335B (en) * | 2013-08-21 | 2014-12-10 | 上海海唇机械设备工程技术有限公司 | Content-adjustable methylhydrazine synthetic-fluid refining apparatus and method |
| CN110325260A (en) * | 2016-11-08 | 2019-10-11 | 曼瑟森三汽油公司 | The method for removing moisture from hydrazine |
| CN107311129A (en) * | 2017-06-26 | 2017-11-03 | 内蒙古锦洋化学工业有限公司 | Urea method hydrazine hydrate concentrates distillation technique |
| CN110775950A (en) * | 2019-11-21 | 2020-02-11 | 江苏索普化工股份有限公司 | Method for recovering and refining saline-alkali from high-salt hydrazine hydrate solution |
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