CN106219850A - The recycling and processing device of a kind of hydrazine hydrate waste liquid and recovery and treatment method - Google Patents
The recycling and processing device of a kind of hydrazine hydrate waste liquid and recovery and treatment method Download PDFInfo
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- CN106219850A CN106219850A CN201610675409.2A CN201610675409A CN106219850A CN 106219850 A CN106219850 A CN 106219850A CN 201610675409 A CN201610675409 A CN 201610675409A CN 106219850 A CN106219850 A CN 106219850A
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- hydrazine hydrate
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/16—Hydrazine; Salts thereof
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/08—Thin film evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
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- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The present invention provides recycling and processing device and the recovery and treatment method of a kind of hydrazine hydrate waste liquid, described recycling and processing device includes waste liquid holding vessel, waste drains pump, acidification reaction still, acidifying discharging pump and the evaporation concentrator being connected with high concentration hydrazine hydrate waste solution channel, the light phase material outlet of evaporation concentrator connects tail water drainer, heavy phase material outlet is sequentially connected with quaternization still, vacuum desiccator, the solid matter outlet of vacuum desiccator connects solid recovery unit, and gaseous substance outlet connects gas phase condenser and hydrazine hydrate receives flow container.Hydrazine hydrate component in energy high efficiente callback waste liquid of the present invention, isolate the component of inorganic salts of nonhazardous, the final tail water discharged gives up from danger and becomes common sewage, sewage plant can be directly entered and carry out biochemical treatment, save all danger to give up processing cost, the high purity hydrous hydrazine reclaimed is reused for production link, makes full use of resource, cost-effective and reduce the pollution to environment.
Description
Technical field
The invention belongs to danger wastes recycling field, be specifically related to the recycling and processing device of a kind of hydrazine hydrate waste liquid
And recovery and treatment method.
Background technology
Hydrazine hydrate, also known as hydrazine hydrate, is a kind of particularly significant, purposes fine chemical material widely, is using water
Closing the waste liquid produced in the chemical process of hydrazine, often containing a large amount of free hydrazine hydrates and each form hydrazonium salt, if not having
Effect processes the most directly discharge, the mankind and animals and plants is had strong toxic action, can cause Heavy environmental pollution.
At present, the conventional process mode of industry high-concentration hydrazine hydrate waste liquid is that high temperature destroys by fire, need to consume mass energy, processes
Costly, it is also possible to cause air secondary pollution.According to the disposal principle of garbage " resource, minimizing, innoxious ", should
When to the recycling as far as possible of the organic principle in refuse.
Summary of the invention
The technical problem to be solved in the present invention is to provide recycling and processing device and the recycling side of a kind of hydrazine hydrate waste liquid
Method, can separate the low-boiling-point organic compound in hydrazine hydrate waste liquid, high boiling point organic compound with inorganic matter, the water in high efficiente callback waste liquid
Close hydrazine.
For solving above-mentioned technical problem, embodiments of the invention provide the recycling and processing device of a kind of hydrazine hydrate waste liquid, bag
Include waste liquid holding vessel, waste drains pump, acidification reaction still, acidifying discharging pump, evaporation concentrator, tail water cooling condenser, tail water drainer, alkali
Change reactor, vacuum desiccator, solid recovery unit, gas phase condenser, hydrazine hydrate receipts flow container and Sewage Disposal, described waste liquid
Holding vessel, waste drains pump, acidification reaction still, acidifying discharging pump and evaporation concentrator are sequentially connected by pipeline, described acidification reaction
Still is provided with hydrochloric acid chemicals feeder；
Described evaporation concentrator top is provided with light phase material outlet, and bottom is provided with heavy phase material outlet, described light phase material outlet,
Tail water cooling condenser, tail water drainer and Sewage Disposal are sequentially connected by pipeline, described heavy phase material outlet, quaternization still
Being sequentially connected by pipeline with vacuum desiccator, described quaternization still is provided with Caustic soda chemicals feeder；
Described vacuum desiccator top is provided with gaseous substance outlet, and bottom is provided with solid matter and exports, the outlet of described gaseous substance,
Gas phase condenser and hydrazine hydrate are received flow container and are sequentially connected by pipeline, and the outlet of described solid matter is connected with solid recovery unit.
Wherein, described tail water drainer is received flow container with hydrazine hydrate and is all connected with a vacuum line, and described vacuum line sets
There are vacuum safety tank and vacuum pump.
Preferably, described evaporation concentrator is vertical scraper membrane evaporator.
Preferably, described vacuum desiccator is conduction heat transfer stirring type dryer.
The embodiment of the present invention also provides for the recovery and treatment method of a kind of above-mentioned hydrazine hydrate waste liquid, comprises the steps:
(1) hydrazine hydrate waste liquid is stored: store in hydrazine hydrate waste liquid is sent into waste liquid holding vessel by pipeline, hydrazine hydrate waste liquid
Contained main matter has: hydrazine hydrate, hydrazine hydrate hydrochlorate, alcohol, aldehyde, ketone Organic substance, inorganic salt；
(2) acidification reaction: the hydrazine hydrate waste liquid in waste liquid holding vessel, by waste drains pump pump to acidification reaction still, passes through hydrochloric acid simultaneously
It is the hydrochloric acid of 20 ~ 37% that chemicals feeder drips concentration in acidification reaction still, until the pH value in acidification reaction still is less than 6, stops dripping
Adding hydrochloric acid, in hydrazine hydrate waste liquid, free hydrazine hydrate stirs with hydrochloric acid mixed on low speed at normal temperatures and pressures, and acidification reaction, acidifying occur
Reaction equation is as shown in formula I, and after acidifying, feed liquid contained substance mainly has: hydrazine hydrate hydrochlorate, alcohol, aldehyde, ketone Organic substance, inorganic
Salt；
N2H4·H2O + HCl → N2H5Cl + H2O formula I；
(3) evaporation and concentration: in step (2), after acidifying, feed liquid is evaporated concentrating to evaporation concentrator by being acidified discharging pump pump,
Evaporation concentrator interior operation pressure is 500 ~ 5000 Pa, operation temperature is 40 ~ 100 DEG C, and chuck saturated vapor inlet pressure is
Feed liquid heat exchange after acidifying on 0.3 ~ 0.6 MPa, with evaporation concentrator inwall evaporating surface, by the water in feed liquid after acidifying, low boiling
Point Organic substance separates with hydrazonium salt, and evaporation forms light phase material and heavy phase material, and the most light phase material contained substance is: alcohol, aldehyde, ketone
Type organic, water；Heavy phase material contained substance is: hydrazine hydrate hydrochlorate, inorganic salt；
(4) tail water condensation: the light phase material in step (3) flows into tail water cooling via the light phase material outlet on evaporation concentrator top
Condensing in condenser, form the tail water without free hydrazine hydrate, tail water enters tail water drainer, then immediately proceeds at sewage
Reason station carries out biochemical treatment；
(5) quaternization: it is anti-that the heavy phase material in step (3) flows into alkalization via the heavy phase material outlet of evaporation concentrator bottom
Answering in still, add concentration in quaternization still by Caustic soda chemicals feeder is the Caustic soda of 20 ~ 50% simultaneously, abundant with heavy phase material
Stirring, until the caustic soda amount added reaches reaction equation proportional quantity, stops dropping Caustic soda, hydrazine hydrate hydrochlorate in heavy phase material
All with Caustic soda generation quaternization, quaternization formula is as shown in formula II, and after alkalization, feed liquid contained substance mainly has: hydrazine hydrate
And inorganic salt；
N2H5Cl + NaOH → N2H4·H2O+NaCl formula II；
(6) being dried separation: be dried separation during feed liquid is admitted to vacuum desiccator after alkalization, vacuum desiccator operation pressure is
500 ~ 5000 Pa, operation temperature be 40 ~ 100 DEG C, jacket steam inlet pressure is 0.3 ~ 0.6 MPa, be dried separate after pure
Sodium salt exports via the solid matter of vacuum desiccator bottom and enters in solid recovery unit, is dried the hydrazine hydrate after separating and water
The mixed gas of steam exports via the gaseous substance on vacuum desiccator top in flowing into gas phase condenser and carries out heat exchange condensation, cold
Hydrazine hydrate solution after Ning stores to hydrazine hydrate receipts flow container, in case being back to commercial production.
Wherein, in step (1), in hydrazine hydrate waste liquid, the concentration of hydrazine is 5 ~ 50%.
Wherein, in step (6), in condensed hydrazine hydrate solution, concentration of hydrazine hydrate is 10 ~ 60%.
Having the beneficial effect that of the technique scheme of the present invention: the present invention is solid by acidifying by high concentration hydrazine hydrate waste liquid
Salt, vacuum evaporation, alkalize, be vacuum dried separating treatment, the hydrazine hydrate in high efficiente callback waste liquid, isolated inorganic salt group
Divide and can do harmless process, and without hydrazine hydrate in the final tail water discharged, sewage plant can be directly entered and carry out biochemical treatment, reclaim
Hydrazine hydrate can be back to commercial production, make full use of resource, cost-effective and reduce the pollution to environment.
Accompanying drawing explanation
Fig. 1 is the structured flowchart of the embodiment of the present invention one.
Description of reference numerals:
1, waste liquid holding vessel；2, waste drains pump；3, acidification reaction still；4, hydrochloric acid chemicals feeder；5, acidifying discharging pump；6, evaporation and concentration
Device；600, light phase material outlet；601, heavy phase material outlet；7, tail water cooling condenser；8, tail water drainer；9, quaternization still；
10, Caustic soda chemicals feeder；11, vacuum desiccator；1100, gaseous substance outlet；1101, solid matter outlet；12, solid reclaims dress
Put；13, gas phase condenser；14, hydrazine hydrate receives flow container；15, vacuum safety tank；16, vacuum pump；17, Sewage Disposal.
Detailed description of the invention
For making the technical problem to be solved in the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing and tool
Body embodiment is described in detail.
As it is shown in figure 1, the recycling and processing device of a kind of hydrazine hydrate waste liquid, including waste liquid holding vessel 1, waste drains pump 2, acidifying instead
Answer still 3, acidifying discharging pump 5, evaporation concentrator 6, tail water cooling condenser 7, tail water drainer 8, quaternization still 9, vacuum desiccator
11, solid recovery unit 12, gas phase condenser 13, hydrazine hydrate receipts flow container 14 and Sewage Disposal 17, described waste liquid holding vessel 1,
Waste drains pump 2, acidification reaction still 3, acidifying discharging pump 5 and evaporation concentrator 6 are sequentially connected by pipeline, described acidification reaction still 3
It is provided with hydrochloric acid chemicals feeder 4.
Described evaporation concentrator 6 top is provided with light phase material outlet 600, and bottom is provided with heavy phase material outlet 601, described gently
Phase material outlet 600, tail water cooling condenser 7, tail water drainer 8 and Sewage Disposal 17 are sequentially connected by pipeline, described heavy phase
Material outlet 601, quaternization still 9 and vacuum desiccator 11 are sequentially connected by pipeline, and described quaternization still 9 is provided with burning
Alkali chemicals feeder 10.
Described vacuum desiccator 11 top is provided with gaseous substance outlet 1100, and bottom is provided with solid matter outlet 1101, institute
State gaseous substance outlet 1100, gas phase condenser 13 and hydrazine hydrate receipts flow container 14 to be sequentially connected by pipeline, described solid matter
Outlet 1101 is connected with solid recovery unit 12.
Described tail water drainer 8 is received flow container 14 with hydrazine hydrate and is all connected with a vacuum line, and described vacuum line is provided with
Vacuum safety tank 15 and vacuum pump 16, the purpose increasing vacuum safety tank 15 is to prevent from pouring in down a chimney.
In the present embodiment, described evaporation concentrator 6 selects vertical scraper membrane evaporator.Described vacuum desiccator 11 is selected
Conduction heat transfer stirring type dryer.
The present invention also provides for the recovery and treatment method of a kind of hydrazine hydrate waste liquid utilizing above-mentioned recycling and processing device, including such as
Lower step:
(1) hydrazine hydrate waste liquid is stored: sent in waste liquid holding vessel 1 by pipeline by the hydrazine hydrate waste liquid that the concentration of hydrazine is 5 ~ 50%
Storing, main matter contained by hydrazine hydrate waste liquid has: hydrazine hydrate, hydrazine hydrate hydrochlorate, alcohol, aldehyde, ketone Organic substance, inorganic salt
Deng；
(2) acidification reaction: the hydrazine hydrate waste liquid in waste liquid holding vessel 1, by waste drains pump 2 pump to acidification reaction still 3, passes through simultaneously
It is the hydrochloric acid of 20 ~ 37% that hydrochloric acid chemicals feeder 4 drips concentration in acidification reaction still 3, until the pH value in acidification reaction still 3 is less than
6, stop dropping hydrochloric acid, in hydrazine hydrate waste liquid there is acid with the stirring of hydrochloric acid mixed on low speed at normal temperatures and pressures in free hydrazine hydrate material
Changing reaction, acidification reaction formula is as shown in formula I, and after acidifying, feed liquid contained substance mainly has: hydrazine hydrate hydrochlorate, alcohol, aldehyde, ketone
Organic substance, inorganic salt etc.；
N2H4·H2O + HCl → N2H5Cl + H2O formula I；
(3) evaporation and concentration: after acidifying, feed liquid is dense to being evaporated in evaporation concentrator 6 by being acidified storing pump 5 pump in step (2)
Contracting, evaporation concentrator (6) operation pressure is 500 ~ 5000 Pa, and operation temperature is 40 ~ 100 DEG C, and jacket steam inlet pressure is
Feed liquid heat exchange after acidifying on 0.3 ~ 0.6 MPa, with evaporation concentrator 6 inwall evaporating surface, by the water in feed liquid after acidifying, low boiling
Point Organic substance separates with hydrazonium salt, and evaporation forms light phase material and heavy phase material, and the most light phase material contained substance is: alcohol, aldehyde, ketone
Type organic, water etc.；Heavy phase material contained substance is: hydrazine hydrate hydrochlorate, inorganic salt；
(4) tail water condensation: the light phase material in step (3) flows into tail via the light phase material outlet 600 on evaporation concentrator 6 top
Condensing in water condenser 7, form the tail water without free hydrazine hydrate, tail water enters tail water drainer 8, then immediately proceeds to
Sewage Disposal 17 carries out biochemical treatment；
(5) quaternization: the heavy phase material in step (3) flows into alkali via the heavy phase material outlet 601 of evaporation concentrator 6 bottom
Changing in reactor 9, add concentration in quaternization still 9 by Caustic soda chemicals feeder 10 is the Caustic soda of 20 ~ 50% simultaneously, with heavy phase
Material is sufficiently stirred for, until the caustic soda amount added reaches reaction equation proportional quantity, stops dropping Caustic soda, is hydrated in heavy phase material
Hydrazine hydrochloride all with Caustic soda generation quaternization, quaternization formula is as shown in formula II, and after alkalization, feed liquid contained substance is main
Have: hydrazine hydrate and inorganic salt；
N2H5Cl + NaOH → N2H4·H2O+NaCl formula II；
(6) it is dried separation: after alkalization, feed liquid is admitted to be dried separation during vacuum desiccator 11 is carried out, and vacuum desiccator 11 is grasped
Being 500 ~ 5000 Pa as pressure, operation temperature is 40 ~ 100 DEG C, and jacket steam inlet pressure is 0.3 ~ 0.6 MPa, is dried and separates
After pure sodium salt via vacuum desiccator 11 bottom solid matter export 1101 entrance solid recovery units 12 in, be dried point
Hydrazine hydrate after from exports 1100 inflow gas phases with the mixed gas of steam via the gaseous substance on vacuum desiccator 11 top
Carrying out heat exchange condensation in condenser 13, condensed hydrazine hydrate solution stores to hydrazine hydrate receipts flow container 14, condensed hydration
In hydrazine solution, concentration of hydrazine hydrate is 10 ~ 60%, in case being back to commercial production.
The hydrazine hydrate devil liquor recovery processing method and the effect thereof that there is provided the present invention with 4 specific embodiments below are carried out in detail
Thin description:
Embodiment 1: hydrazine concentration is waste liquid 1.0 m of 30%3, enter acidification reaction still through waste drains pump, add concentration 35% hydrochloric acid also
Completely, there is acidification reaction in stirring, after acidifying, the acidified discharging pump of feed liquid enters evaporation concentrator, evaporates shape when pH registration is 6
The light phase material become enters tail water cooling after tail water cooling condenser condenses and coagulates tank, forms the tail water without free hydrazine hydrate, can be direct
Enter Sewage Disposal and carry out biochemical treatment.Heavy phase material enters quaternization still, adds concentration by reaction equation proportional quantity
Caustic soda the stirring of 45% are complete, it is dried the pure sodium salt after separating and enters mixing of solid recovery unit, hydrazine hydrate and steam
Close in gas enters gas phase condenser and carry out heat exchange condensation, obtain 50% hydrazine hydrate solution after condensation and store to hydrazine hydrate receipts flow container
In, in case being back to commercial production.
In the present embodiment, evaporation concentrator is 1000 Pa with the operation pressure of vacuum desiccator, and operation temperature is 65 DEG C,
Chuck inlet steam pressure 0.3 MPa.
Embodiment 2: hydrazine concentration is waste liquid 1.0 m of 30%3, enter acidification reaction still through waste drains pump, add concentration 30%
Hydrochloric acid also stirs completely, and acidification reaction occurs when pH registration is 6, and after acidifying, the acidified discharging pump of feed liquid enters evaporation concentrator,
The light phase material that evaporation is formed enters tail water cooling after tail water cooling condenser condenses and coagulates tank, forms the tail water without free hydrazine hydrate,
Sewage Disposal can be directly entered and carry out biochemical treatment.Heavy phase material enters quaternization still, adds by reaction equation proportional quantity
Enter the Caustic soda of concentration 45% and stir completely, being dried the pure sodium salt after separating and enter solid recovery unit, hydrazine hydrate and steam
Mixed gas enter in gas phase condenser and carry out heat exchange condensation, obtain 50% hydrazine hydrate solution after condensation and store to hydrazine hydrate and receive
In flow container, in case being back to commercial production.
In the present embodiment, evaporation concentrator is 1000 Pa with the operation pressure of vacuum desiccator, and operation temperature is 65 DEG C,
Chuck inlet steam pressure 0.3 MPa.
Embodiment 3: hydrazine concentration is waste liquid 1.0 m of 30%3, enter acidification reaction still through waste drains pump, add concentration 35%
Hydrochloric acid also stirs completely, and acidification reaction occurs when pH registration is 6, and after acidifying, the acidified discharging pump of feed liquid enters evaporation concentrator,
The light phase material that evaporation is formed enters tail water cooling after tail water cooling condenser condenses and coagulates tank, forms the tail water without free hydrazine hydrate,
Sewage Disposal can be directly entered and carry out biochemical treatment.Heavy phase material enters quaternization still, adds by reaction equation proportional quantity
Enter the Caustic soda of concentration 30% and stir completely, being dried the pure sodium salt after separating and enter solid recovery unit, hydrazine hydrate and steam
Mixed gas enter in gas phase condenser and carry out heat exchange condensation, obtain 35% hydrazine hydrate solution after condensation and store to hydrazine hydrate and receive
In flow container, in case being back to commercial production.
In the present embodiment, evaporation concentrator is 1000 Pa with the operation pressure of vacuum desiccator, and operation temperature is 65 DEG C,
Chuck inlet steam pressure 0.3 MPa.
Embodiment 4: hydrazine concentration is waste liquid 1.0 m of 20%3, enter acidification reaction still through waste drains pump, add concentration 35%
Hydrochloric acid also stirs completely, and acidification reaction occurs when pH registration is 6, and after acidifying, the acidified discharging pump of feed liquid enters evaporation concentrator,
The light phase material that evaporation is formed enters tail water cooling after tail water cooling condenser condenses and coagulates tank, forms the tail water without free hydrazine hydrate,
Sewage Disposal can be directly entered and carry out biochemical treatment.Heavy phase material enters quaternization still, adds by reaction equation proportional quantity
Enter the Caustic soda of concentration 45% and stir completely, being dried the pure sodium salt after separating and enter solid recovery unit, hydrazine hydrate and steam
Mixed gas enter in gas phase condenser and carry out heat exchange condensation, obtain 50% hydrazine hydrate solution after condensation and store to hydrazine hydrate and receive
In flow container, in case being back to commercial production.
In the present embodiment, evaporation concentrator is 1000 Pa with the operation pressure of vacuum desiccator, and operation temperature is 65 DEG C,
Chuck inlet steam pressure 0.3 MPa.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, on the premise of without departing from principle of the present invention, it is also possible to make some improvements and modifications, these improvements and modifications are also
Should be regarded as protection scope of the present invention.
Claims (7)
1. the recycling and processing device of a hydrazine hydrate waste liquid, it is characterised in that include waste liquid holding vessel (1), waste drains pump (2), acid
Change reactor (3), acidifying discharging pump (5), evaporation concentrator (6), tail water cooling condenser (7), tail water drainer (8), quaternization
Still (9), vacuum desiccator (11), solid recovery unit (12), gas phase condenser (13), hydrazine hydrate are received at flow container (14) and sewage
Reason station (17), described waste liquid holding vessel (1), waste drains pump (2), acidification reaction still (3), acidifying discharging pump (5) and evaporation concentrator
(6) being sequentially connected by pipeline, described acidification reaction still (3) is provided with hydrochloric acid chemicals feeder (4)；
Described evaporation concentrator (6) top is provided with light phase material outlet (600), and bottom is provided with heavy phase material outlet (601), described
Light phase material outlet (600), tail water cooling condenser (7), tail water drainer (8) and Sewage Disposal (17) pass through pipeline phase successively
Even, described heavy phase material outlet (601), quaternization still (9) and vacuum desiccator (11) are sequentially connected by pipeline, described alkali
Change reactor (9) and be provided with Caustic soda chemicals feeder (10)；
Described vacuum desiccator (11) top is provided with gaseous substance outlet (1100), and bottom is provided with solid matter outlet (1101),
Described gaseous substance outlet (1100), gas phase condenser (13), hydrazine hydrate receive flow container (14) and vacuum safety tank (15) by pipe
Road is sequentially connected, and described solid matter outlet (1101) is connected with solid recovery unit (12).
The recycling and processing device of hydrazine hydrate waste liquid the most according to claim 1, it is characterised in that described tail water drainer
(8) receiving flow container (14) with hydrazine hydrate to be all connected with a vacuum line, described vacuum line is provided with vacuum safety tank (15) and very
Empty pump (16).
The recycling and processing device of hydrazine hydrate waste liquid the most according to claim 1, it is characterised in that described evaporation concentrator
(6) it is vertical scraper membrane evaporator.
The recycling and processing device of hydrazine hydrate waste liquid the most according to claim 1, it is characterised in that described vacuum desiccator
(11) it is conduction heat transfer stirring type dryer.
5. the recovery and treatment method of a hydrazine hydrate waste liquid as claimed in claim 1, it is characterised in that comprise the steps:
(1) hydrazine hydrate waste liquid is stored: store in hydrazine hydrate waste liquid is sent into waste liquid holding vessel (1) by pipeline, hydrazine hydrate
Contained by waste liquid, main matter has: hydrazine hydrate, hydrazine hydrate hydrochlorate, alcohol, aldehyde, ketone Organic substance, inorganic salt；
(2) acidification reaction: the hydrazine hydrate waste liquid in waste liquid holding vessel (1) is by waste drains pump (2) pump to acidification reaction still (3), same
Time to drip concentration in acidification reaction still (3) by hydrochloric acid chemicals feeder (4) be the hydrochloric acid of 20 ~ 37%, until acidification reaction still (3)
Interior pH value, less than 6, stops dropping hydrochloric acid, and in hydrazine hydrate waste liquid, free hydrazine hydrate stirs with hydrochloric acid mixed on low speed at normal temperatures and pressures
Mixing, acidification reaction occurs, acidification reaction formula is as shown in formula I, and after acidifying, feed liquid contained substance mainly has: hydrazine hydrate hydrochlorate,
Alcohol, aldehyde, ketone Organic substance, inorganic salt；
N2H4·H2O + HCl → N2H5Cl + H2O formula I；
(3) evaporation and concentration: in step (2), after acidifying, feed liquid is evaporated to evaporation concentrator (6) by being acidified discharging pump (5) pump
Concentrating, evaporation concentrator (6) interior operation pressure is 500 ~ 5000 Pa, operation temperature is 40 ~ 100 DEG C, and chuck saturated vapor enters
Mouth pressure is 0.3 ~ 0.6 MPa, with the acidifying on evaporation concentrator (6) inwall evaporating surface after feed liquid heat exchange, will acidifying after feed liquid
In water, low-boiling-point organic compound separate with hydrazonium salt, evaporation forms light phase material and heavy phase material, the most light phase material contained substance
For: alcohol, aldehyde, ketone Organic substance, water；Heavy phase material contained substance is: hydrazine hydrate hydrochlorate, inorganic salt；
(4) tail water condensation: the light phase material in step (3) flows into tail water cooling via the light phase material outlet on evaporation concentrator top
Condenser condenses in (7), forms the tail water without free hydrazine hydrate, and tail water enters tail water drainer (8), then immediately proceeds to
Sewage Disposal (17) carries out biochemical treatment；
(5) quaternization: it is anti-that the heavy phase material in step (3) flows into alkalization via the heavy phase material outlet of evaporation concentrator bottom
Answering in still (9), add concentration in quaternization still (9) by Caustic soda chemicals feeder (10) is the Caustic soda of 20 ~ 50% simultaneously, with weight
Phase material is sufficiently stirred for, until the caustic soda amount added reaches reaction equation proportional quantity, stops dropping Caustic soda, water in heavy phase material
Close hydrazine hydrochloride all with Caustic soda generation quaternization, quaternization formula as shown in formula II, feed liquid contained substance master after alkalization
Have: hydrazine hydrate and inorganic salt；
N2H5Cl + NaOH → N2H4·H2O+NaCl formula II；
(6) being dried separation: after alkalization, feed liquid is dried separation in being admitted to vacuum desiccator (11), vacuum desiccator (11) is grasped
Being 500 ~ 5000 Pa as pressure, operation temperature is 40 ~ 100 DEG C, and jacket steam inlet pressure is 0.3 ~ 0.6 MPa, is dried and separates
After pure sodium salt export via the solid matter of vacuum desiccator bottom and enter in solid recovery unit (12), be dried after separating
The mixed gas of hydrazine hydrate and steam export via the gaseous substance on vacuum desiccator (11) top and flow into gas phase condenser
(13) carrying out heat exchange condensation in, condensed hydrazine hydrate solution stores to hydrazine hydrate receipts flow container (14), in case being back to industry
Produce.
The recovery and treatment method of hydrazine hydrate waste liquid the most according to claim 5, it is characterised in that in step (1), hydrazine hydrate
In waste liquid, the concentration of hydrazine is 5 ~ 50%.
The recovery and treatment method of hydrazine hydrate waste liquid the most according to claim 5, it is characterised in that in step (6), after condensation
Hydrazine hydrate solution in concentration of hydrazine hydrate be 10 ~ 60%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610675409.2A CN106219850A (en) | 2016-08-17 | 2016-08-17 | The recycling and processing device of a kind of hydrazine hydrate waste liquid and recovery and treatment method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610675409.2A CN106219850A (en) | 2016-08-17 | 2016-08-17 | The recycling and processing device of a kind of hydrazine hydrate waste liquid and recovery and treatment method |
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| CN106219850A true CN106219850A (en) | 2016-12-14 |
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| CN201610675409.2A Pending CN106219850A (en) | 2016-08-17 | 2016-08-17 | The recycling and processing device of a kind of hydrazine hydrate waste liquid and recovery and treatment method |
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| CN111116431A (en) * | 2019-12-31 | 2020-05-08 | 中船重工（邯郸）派瑞特种气体有限公司 | Device and method for recovering trifluoromethanesulfonic acid from trifluoromethanesulfonic acid-containing wastewater |
| CN113754165A (en) * | 2021-09-08 | 2021-12-07 | 山东瑞纳特化工有限公司 | Initiator waste acid recycling device system and method |
| CN114470827A (en) * | 2022-02-22 | 2022-05-13 | 宁夏彩源科技有限公司 | Production method and production system of clean thiocarbohydrazide |
| CN115626612A (en) * | 2022-10-21 | 2023-01-20 | 武汉大学 | Preparation method and application of diamine salt |
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