CN105836930B - Membrane integrated treatment process for high-salt-content wastewater generated in preparation of hydrazine hydrate by ketazine method - Google Patents
Membrane integrated treatment process for high-salt-content wastewater generated in preparation of hydrazine hydrate by ketazine method Download PDFInfo
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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
- 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
- C02F1/20—Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
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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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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Abstract
The invention relates to a membrane-method integrated treatment process for high-salt-content wastewater of hydrazine hydrate prepared by a ketazine method. The invention adopts a membrane method integrated treatment technology, effectively realizes the separation of organic matters and inorganic salts, and has the advantages of advanced process, simple operation, stable and reliable effect and the like.
Description
Technical field
The invention belongs to environmentally friendly water treatment field, the high slat-containing wastewater embrane method for being related to a kind of preparation of hydrazine hydrate by use of ketazine is integrated
Treatment process.
Background technique
Hydrazine hydrate, also known as hydrazine hydrate are a kind of important fine chemical materials.Hydrazine hydrate can be used for synthesizing a variety of foaming
Agent, cleaning treatment agent, also can be used as the fields such as drug, herbicide, rubber chemicals, rocket fuel.The synthetic method master of hydrazine hydrate
There are Raschig process, urea method, ketazine process and hydrogen peroxide method etc..Raschig process is using ammonia as nitrogen source, with hypochlorite oxidation ammonia
Hydrazine hydrate processed also generates a large amount of sodium chloride and chlorination since the method need to use excess of ammonia while need to adding recyclable device
The salt such as ammonium.The environmental pollution that Raschig process generates is than more serious, and investment is big, and product yield is low, so method is eliminated substantially.Urea
Method makees oxidant with sodium hypochlorite, prepares hydrazine hydrate by nitrogen source of urea.Urea method has many advantages, such as that investment is low, and equipment is simple,
But since the raw material used are more expensive, thus, do not have competitiveness compared with other preparation methods.Hydrogen peroxide method by
Cheap in hydrogen peroxide source, this method has very big attraction, and rare inorganic byproduct is formed, but content of organics in product
It is higher by nearly a hundred times than urea method.Ketazine process has many advantages, such as that small investment, product yield are high, low energy consumption, at low cost.It adopts both at home and abroad
It is commonplace that hydrazine hydrate is prepared with the method.However, ketazine process can generate the very high waste water of salt content, sodium chloride concentration is very high,
In addition, COD value is also relatively high, and belonging to high saliferous difficult to deal with has also containing organic matters such as acetone, ketazines in the waste water
Machine waste water.
Summary of the invention
In view of the deficiencies of the prior art, the invention proposes a kind of high slat-containing wastewater embrane method collection of preparation of hydrazine hydrate by use of ketazine
At treatment process, efficiently separating for organic matter and inorganic salts is realized.
The technical solution of the present invention is as follows: a kind of high-salt wastewater embrane method integrated treatment process of preparation of hydrazine hydrate by use of ketazine,
Specific step is as follows:
1) absorption pretreatment is carried out to the high slat-containing wastewater of preparation of hydrazine hydrate by use of ketazine, reduces COD value.
2) micro-filtration processing is carried out to the waste water after absorption, is sent the filtered water purification of micro-filtration to nanofiltration system using high-pressure pump
Concentration is carried out, trapped fluid carries out Slag treatment.
3) pretreated to micro-filtration production water carries out nanofiltration processing, and concentrate is delivered to adsorption treatment, per-meate side be discharged into
Enter catalytic ozonation system.
4) stripping processing is carried out through catalytic ozonation treated waste water, further to remove volatile organic matter.
5) through stripping, treated that waste water is delivered to salt refining.
The conductivity of the high slat-containing wastewater of above-mentioned preparation of hydrazine hydrate by use of ketazine is 90000-300000 μ s/cm, CODCrFor
2500-4500mg/L；The conductivity of waste water is 80000-290000 μ s/cm, COD after absorption, micro-filtrationCrFor 1700-2800mg/
L；The conductivity that water is produced after nanofiltration is 75000-270000 μ s/cm, CODCrFor 500-800mg/L；After catalytic ozonation
Waste water conductivity be 75000-270000 μ s/cm, CODCrFor 60-120mg/L；The conductivity of waste water is after stripping
75000-270000 μ s/cm, CODCrFor 20-50mg/L.
Preferred adsorbent is one of silica gel, activated alumina, active carbon, molecular sieve or any several combination, is thrown
Dosage is 0.5-3wt.%, adsorption time 20-50min.
It is preferred that micro-filtration preprocessing process uses pressure actuated device for circulating pump, operating pressure 0.1-0.3MPa；Micro-filtration
Film is organic film or inoranic membrane, and film average pore size is 0.03-5 μm；Membrane module is tubular membrane, rolled film or hollow-fibre membrane.
It is preferred that nanofiltration process uses pressure actuated device for circulating pump, operating pressure 0.4-0.8MPa；Nanofiltration membrane is to have
Machine film or inoranic membrane, film average pore size are 1-5nm；Membrane module is tubular membrane, rolled film or hollow-fibre membrane.
It is preferred that the oxygen air inflow of ozone oxidation is 3-15L/min, ozone dosage 3-10g/L.Catalyst is preferably golden
Belong to oxide catalyst, is one of metal oxides such as Fe, Mn, Ni, La, Ce, Al, catalyst charge is reaction system
0.1-6wt.%.The residence time of pending water in a device is 5-200min, preferably 15-100min.
It is preferred that stripping gas-liquid volume ratio is 200-400, pH 9-13, stripping temperature is 30-100 DEG C, stripping time 1-
4h。
The utility model has the advantages that
The present invention conveys the high slat-containing wastewater of preparation of hydrazine hydrate by use of ketazine after absorption, micro-filtration pretreatment by high-pressure pump
Nanofiltration process is carried out to membrane filtration system, the water purification of per-meate side enters catalytic ozonation processing, after catalytic ozonation
Waste water carries out stripping processing, and stripping processing waste water is delivered to salt refining.The present invention is by film and catalytic ozonation, stripping process
It is coupled, the separation of the hydrazine hydrate useless Organic substance in water and inorganic salts of high saliferous is realized, with low energy consumption, technique is advanced, behaviour
Make the advantages that simple, effect stability is reliable.
Detailed description of the invention
Fig. 1 is the high slat-containing wastewater embrane method integrated treatment process flow chart for being preparation of hydrazine hydrate by use of ketazine.
Specific embodiment
Embodiment 1
It is 90000 μ s/cm, COD to conductivityCrAbsorption pretreatment is carried out for the hydrazine hydrate waste water of 2500mg/L, use
Adsorbent is active carbon powder, dosage 0.5wt.%, carries out micro-filtration pretreatment after adsorbing 20min, use membrane aperture for
0.03 μm of hollow-fibre membrane filters under conditions of transmembrane pressure is 0.3MPa, and production water conductivity is 80000 μ s/cm, CODCr
For 1700mg/L；Nanofiltration membrane system will be delivered to by high-pressure pump by micro-filtration pretreated penetrating fluid, using average
Aperture be 5nm ceramic alumina hollow fiber nanofiltration membrane carry out concentration, transmembrane pressure be 0.6MPa under conditions of into
Row filtering, the conductivity of per-meate side fresh water are 75000 μ s/cm, CODCrFor 500mg/L；Nanofiltration per-meate side production water enters ozone and urges
Change oxidation processes, the catalyst used loads manganese oxide, dosage 0.1wt.%, oxygen air inflow 3L/ for cellular oxidative aluminium
Min, ozone dosage 3g/L, residence time 5min, the conductivity of the waste water after catalytic ozonation are 75000 μ s/
Cm, CODCrFor 120mg/L；Waste water after catalytic ozonation is delivered to stripping processing, and the conductivity of stripping processed waste water is
75000 μ s/cm, CODCrFor 50mg/L, stripping gas-liquid volume ratio is 200, pH 13, and stripping temperature is 90 DEG C, and stripping time is
1h。
Embodiment 2
It is 300000 μ s/cm, COD to conductivityCrAbsorption pretreatment is carried out for the hydrazine hydrate waste water of 4500mg/L, use
Adsorbent is activated alumina, and dosage 3wt.% carries out micro-filtration pretreatment after adsorbing 50min, uses membrane aperture for 5 μm
Tubular membrane filters under conditions of transmembrane pressure is 0.1MPa, and production water conductivity is 290000 μ s/cm, CODCrFor 2800mg/L；
Nanofiltration membrane system will be delivered to by high-pressure pump by micro-filtration pretreated penetrating fluid, and use average pore size for 1nm's
Sulfonated polyphenyl sulfone rolled film carries out concentration, is filtered under conditions of transmembrane pressure is 0.8MPa, per-meate side fresh water
Conductivity is 270000 μ s/cm, CODCrFor 800mg/L；Nanofiltration per-meate side produces water and enters catalytic ozonation processing, and use is urged
Agent is cellular oxidative aluminium Supporting cerium oxide, dosage 6wt.%, oxygen air inflow 15L/min, ozone dosage 10g/
L, residence time 100min, the conductivity of the waste water after catalytic ozonation are 270000 μ s/cm, CODCrFor 120mg/L；
Waste water after catalytic ozonation is delivered to stripping processing, and the conductivity of waste water is 270000 μ s/cm, COD after strippingCrFor
20mg/L, stripping gas-liquid volume ratio are 400, pH 9, and stripping temperature is 30 DEG C, stripping time 4h.
Embodiment 3
It is 190000 μ s/cm, COD to conductivityCrAbsorption pretreatment is carried out for the hydrazine hydrate waste water of 3050mg/L, use
Adsorbent is inorganic silica gel, and dosage 0.5wt.% carries out micro-filtration pretreatment after adsorbing 40min, uses membrane aperture for 3 μm
Tubular membrane filters under conditions of transmembrane pressure is 0.2MPa, and production water conductivity is 170000 μ s/cm, CODCrFor 2570mg/L；
Nanofiltration membrane system will be delivered to by high-pressure pump by micro-filtration pretreated penetrating fluid, and use average pore size for 2nm's
Sulfonated polyether sulfone hollow-fibre membrane carries out concentration, is filtered under conditions of transmembrane pressure is 0.5MPa, per-meate side is light
The conductivity of water is 155200 μ s/cm, CODCrFor 629mg/L；Nanofiltration per-meate side produces water and enters catalytic ozonation processing, uses
Catalyst be cellular oxidative aluminium lanthanum oxide-carrying, dosage 5wt.%, oxygen air inflow 7.3L/min, ozone dosage is
6g/L, residence time 40min, the conductivity of the waste water after catalytic ozonation are 155200 μ s/cm, CODCrFor 77mg/
L；Waste water after catalytic ozonation is delivered to stripping processing, and the conductivity of waste water is 155200 μ s/cm, COD after taking offCrFor
32mg/L, stripping gas-liquid volume ratio are 350, pH 10, and stripping temperature is 50 DEG C, stripping time 3h.
Claims (3)
1. a kind of high slat-containing wastewater embrane method integrated treatment process of preparation of hydrazine hydrate by use of ketazine, the specific steps of which are as follows:
1) absorption pretreatment is carried out to the high slat-containing wastewater of preparation of hydrazine hydrate by use of ketazine, reduces COD value；
2) micro-filtration processing is carried out to the waste water after absorption, the filtered water purification of micro-filtration is sent to nanofiltration system using high-pressure pump and is carried out
Concentration, trapped fluid carry out Slag treatment；
3) production water pretreated to micro-filtration carries out nanofiltration processing, and concentrate is delivered to adsorption treatment, and per-meate side water outlet enters smelly
Oxygen catalytic oxidation system；
4) stripping processing is carried out through catalytic ozonation treated waste water, further to remove volatile organic matter；
5) through stripping, treated that waste water is delivered to salt refining；
The conductivity of the high slat-containing wastewater of preparation of hydrazine hydrate by use of ketazine is 90000-300000 μ s/cm, CODCr 2500-
4500mg/L；
The conductivity of waste water is 80000-290000 μ s/cm, COD after absorption, micro-filtrationCrFor 1700-2800mg/L；Through nanofiltration
The conductivity for producing water afterwards is 75000-270000 μ s/cm, CODCrFor 500-800mg/L；
The conductivity of waste water after catalytic ozonation is 75 000-270000 μ s/cm, CODCrFor 60-120mg/L；
The conductivity of waste water is 750 00-270000 μ s/cm, COD after strippingCrFor 20-50mg/L；
Adsorbent is one of silica gel, activated alumina, active carbon, molecular sieve or any several combination, dosage are
0.5-3wt.%, adsorption time 20-50min；
The oxygen air inflow of ozone oxidation is 3-15L/min, ozone dosage 3-10g/L；Catalyst be Fe, Mn, Ni, La,
One of Ce, Al metal oxide, catalyst charge are the 0.1-6wt.% of reaction system；Pending water is in a device
Residence time is 5-200min；
Stripping gas-liquid volume ratio is 200-400, and pH 9-13, stripping temperature is 30-90 DEG C, stripping time 1-4h.
2. technique according to claim 1, it is characterised in that micro-filtration preprocessing process uses pressure actuated device for circulation
Pump, operating pressure 0.1-0.3MPa；Microfiltration membranes are organic film or inoranic membrane, and film average pore size is 0.03-5 μm；Membrane module is
Tubular membrane, rolled film or hollow-fibre membrane.
3. technique according to claim 1, it is characterised in that nanofiltration treatment process uses pressure actuated device for circulating pump,
Operating pressure is 0.4-0.8MPa；Nanofiltration membrane is organic film or inoranic membrane, and film average pore size is 1-5nm；Membrane module be tubular membrane,
Rolled film or hollow-fibre membrane.
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| CN108128916A (en) * | 2017-11-21 | 2018-06-08 | 清华大学 | Water treatment method and device |
| CN107721023A (en) * | 2017-11-22 | 2018-02-23 | 天津海泽惠科技发展有限公司 | A kind of hydrazine hydrate wastewater treatment equipment and its technique |
| CN109133495A (en) * | 2018-07-23 | 2019-01-04 | 华南理工大学 | A kind of carbonless paper coating wastewater treatment and circulation reuse method |
| CN110240134B (en) * | 2019-06-06 | 2022-09-16 | 宜宾海丰和锐有限公司 | Removing Fe in ketazine process hydrazine hydrate 3+ And organic matter |
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| CN1792825A (en) * | 2005-11-22 | 2006-06-28 | 宜宾天原股份有限公司 | Process for treating hydrazine hydrate waste salt water by ketone linking nitrogen method |
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| CN104230080A (en) * | 2013-06-20 | 2014-12-24 | 天津市汉沽合佳化工有限责任公司 | Technique for producing caustic soda from spent brine generated in hydrazine hydrate production process |
| CN104724871A (en) * | 2015-03-20 | 2015-06-24 | 苏州聚智同创环保科技有限公司 | Technique for recycling ketazine-process hydrazine hydrate high-salt wastewater |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1792825A (en) * | 2005-11-22 | 2006-06-28 | 宜宾天原股份有限公司 | Process for treating hydrazine hydrate waste salt water by ketone linking nitrogen method |
| CN101391826A (en) * | 2008-10-17 | 2009-03-25 | 中国海洋大学 | A cyclone-membrane separation desalination method for seawater containing solid insoluble matter |
| CN103663769A (en) * | 2012-09-07 | 2014-03-26 | 中国石油化工股份有限公司 | Method for desalting sewage by using membrane separation technology |
| CN104230080A (en) * | 2013-06-20 | 2014-12-24 | 天津市汉沽合佳化工有限责任公司 | Technique for producing caustic soda from spent brine generated in hydrazine hydrate production process |
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