CN106145496B - The comprehensive utilization process of viscose fiber acid waste water - Google Patents
The comprehensive utilization process of viscose fiber acid waste water 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
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
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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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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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
- C02F1/048—Purification of waste water by 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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/02—Temperature
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/03—Pressure
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/10—Solids, e.g. total solids [TS], total suspended solids [TSS] or volatile solids [VS]
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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
- C02F2303/00—Specific treatment goals
- C02F2303/10—Energy recovery
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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
- C02F2303/00—Specific treatment goals
- C02F2303/14—Maintenance of water treatment installations
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Abstract
A kind of comprehensive utilization process of viscose fiber acid waste water is first to be filtered viscose fiber acid waste water by filter, removes the suspended matter in waste water, and filtered solution enters next step processing；Then filtered solution is imported into counter-infiltration system, obtains film concentrate and film permeate, for film permeate directly as process water reuse, film concentrate enters step C processing；Finally after film concentrate that reverse osmosis treatment obtains imports multi-effect evaporator concentration, be sent into crystallizing tank crystallization, obtain sulfate crystal, crystalline mother solution is sulfuric acid, and contains sodium sulphate and zinc sulfate, can direct reuse into coagulating bath.The present invention realizes the recycling of sulfuric acid, zinc sulfate, sodium sulphate and water by using dual-membrane process, solves the problems, such as the problem of zinc discharge and solid waste, realizes the comprehensive utilization of resource.
Description
Technical field
The present invention relates to three-protection design more particularly to a kind of comprehensive utilization process of viscose fiber acid waste water.
Background technique
Viscose rayon is using natural fiber as regenerated celulose fibre made of raw material.It is generated in viscose fiber production process
A large amount of waste water.Mainly contained in these waste water sulfuric acid, zinc sulfate, sodium sulphate, carbon disulfide, hydrogen sulfide, dissolution organic matter,
Suspended matter etc. is one of primary pollution source of textile industry, brings very big harm to environment.
Acid waste water occurs mainly with spinning workshop, acid station and postprocessing working procedures.Including wash spinning machine water, acid station it is washed
Water and post treatment acid wash water are washed in filter draining.In addition, cleaning evaporation equipment, crystallizer also generate a certain amount of spent acidic
Water.Acid waste water mainly contains sulfuric acid, sodium sulphate, zinc sulfate etc..Wherein acid waste water is the maximum a kind of water that causes damages,
Acid content is high, and sodium sulphate content is high, and other pollutants are also higher, and processing difficulty is larger.In viscose production technology, spent acidic
Different advantage deviations of the temperature and concentration of water according to each producer's process conditions, typical temperature 90-95 degree, sulfuric acid 10-20g/L,
Sodium sulphate 40-60g/L, zinc sulfate 1-2g/L, remaining is organic matter and sulfide.
After viscose acid waste water processing at present is mostly neutralized with alkaline waste water, then use Physiochemical and biochemical two-stage treatment.General acid
Property waste water mixed with alkaline waste water after pH3.0 or so pH to 10- is adjusted using milk of lime after stripping removes volatile materials
11, zinc ion is precipitated, clear liquid uses Wastewater Treated by Activated Sludge Process, is settled, and qualified discharge is realized in draining.But due to zinc ion
The optimal pH of precipitating is relatively narrow, and milk of lime reacts during adding not exclusively or throwing amount is improper, zinc ion can be caused to precipitate
Not exclusively, cause subsequent biochemical water outlet not up to standard.The process bands carry out a large amount of reluctant solid waste containing zinc simultaneously, and make
At a large amount of wasting of resources.Therefore finding not only can solve above-mentioned problem, but also being able to achieve the technical solution of resource reclaim is viscose row
Industry there is an urgent need to.
Summary of the invention
The purpose of the present invention provides a kind of viscose of low cost exactly in order to solve the above-mentioned problems of the prior art
The comprehensive utilization process of fibrillary acidic waste water.
In order to achieve the above object, the invention adopts the following technical scheme: a kind of synthesis of viscose fiber acid waste water
Utilize technique, comprising the following steps:
A, it pre-processes
Viscose fiber acid waste water is filtered by filter, the suspended matter in waste water is removed, under filtered solution enters
One step process；
B, reverse osmosis
Filtered solution is imported into counter-infiltration system, obtains film concentrate and film permeate, film permeate is used directly as technique
Water reuse, film concentrate enter step C processing；
C, condensing crystallizing
After the film concentrate that reverse osmosis treatment obtains imports multi-effect evaporator concentration, it is sent into crystallizing tank crystallization, is obtained
Sulfate crystal, crystalline mother solution are sulfuric acid, and contain sodium sulphate and zinc sulfate, can direct reuse into coagulating bath.
The pretreatment further includes that viscose fiber acid waste water is reduced the temperature to≤40 DEG C by heat exchanger, the heat exchanger
It is placed on before filter or after filter.
Filter described in step A uses ultrafiltration membrane filter or microporous filtration, and pore size filter is 0.01-1 μm, mistake
Filtering method is dead-end filtration or cross-flow filtration or the combination using one or both of dead-end filtration, cross-flow filtration form, film
Element uses tubular type, board-like, dish-style, rolling or capillary type.
When using cross-flow filtration, film surface flow control is in 2~6 meter per seconds, and operating pressure control is in 0.1~1MPa, operation
Temperature is controlled at 1~90 DEG C.
When using dead-end filtration, membrane component uses external pressing type hollow fibrous membrane, and designs filtrate backwash and air bump rinse operation, when
When the transmembrane pressure of film is more than setting value, system starts backwash procedure；Filtrate is entered by producing water section into water survey, by film surface
Pollutant is taken away, to restore membrane flux.
The counter-infiltration system uses anti-pollution and acidproof reverse-osmosis membrane element, the anti-pollution and acidproof reverse-osmosis membrane element
To the interception capacity of sodium chloride 98% or more.
The equipment of the counter-infiltration system include feed water by reverse osmosis pump, reverse osmosis charge filter, reverse osmosis high-pressure pump and
Reverse osmosis units, each equipment are connected by pipeline, and the filtered solution come from filter is successively through feed water by reverse osmosis pump, reverse osmosis charging
Filter and reverse osmosis high-pressure pump enter reverse osmosis units, and after reverse osmosis treatment, film permeate is returned directly as process water
With film concentrate enters step C, is further concentrated.
The counter-infiltration system includes concatenated multi-stage reverse osmosis equipment, and the filtered solution come from filter initially enters first
Grade reverse osmosis equipment, the film concentrate of first order reverse osmosis equipment enter second level reverse osmosis equipment, second level reverse osmosis equipment
Film concentrate enter third level reverse osmosis equipment, the film concentrate of afterbody reverse osmosis equipment to concentrate transfer tank；Respectively
The film permeate of grade reverse osmosis equipment summarizes centralized collection as reverse osmosis produced water, which can be used as industrial water and return
With.
Every grade of the multi-stage reverse osmosis equipment respectively includes the reverse-osmosis circulating pump and one group of reverse osmosis membrane of series winding setting
Group, the film concentrate of the reverse osmosis membrane group of upper level reverse osmosis equipment enter next stage reverse osmosis equipment reverse-osmosis circulating pump or
Into concentrate transfer tank, the film concentrate of the reverse osmosis membrane group of afterbody reverse osmosis equipment is directly entered concentrate transfer
Tank；For the film permeate centralized collection of the reverse osmosis membrane group of reverse osmosis equipments at different levels as reverse osmosis produced water, which can
As industrial water reuse.
The operating pressure of the counter-infiltration system is controlled in 1-10Mpa.
Enter reverse osmosis equipment by pretreated filtered solution, operating pressure control is in 1-10Mpa, and total dissolved solidss are from 5-
8%, it is concentrated to 15-20%.To reduce concentration process energy consumption, energy recycle device can be used in reverse osmosis equipment.Water recycling
Rate reaches 60-80%, and the water quality of reverse osmosis filter liquor meets technical process water requirement.
The comprehensive utilization process of viscose fiber acid waste water of the present invention realizes sulfuric acid, sulphur by using dual-membrane process
The recycling of sour zinc, sodium sulphate and water solves the problems, such as the problem of zinc discharge and solid waste, realizes the comprehensive benefit of resource
With.Simultaneously because being dehydrated concentration using membrane combination technology, the cost of evaporation is greatly reduced, so that entire technique is compared to only with steaming
Dehydration is sent, there is better economy.
Pretreatment handles water, allows to meet reverse osmosis feed needs.It is designed especially with super-pressure,
The load of high concentration multiple operation, counter-infiltration system increases, it is easier to generate pollution.Therefore higher want is proposed for pretreatment
It asks.
It is concentrated by evaporation by the concentration of acid and salt, the crystallization of reverse osmosis initial concentration further, obtains sulfate crystal, it is real
The reuse of existing sodium sulphate.Sulfuric acid and zinc sulfate stay in crystalline mother solution, are back to use in coagulating bath, realize time of sulfuric acid and zinc sulfate
With.
In order to guarantee the stable operation of counter-infiltration system and prolong the service life have strict demand to water inlet.Viscose
Wash waste water to mainly contain: sulfuric acid, sodium sulphate, zinc sulfate, elemental sulfur, fiber, carbohydrate etc. are in yellow turbid solution.Wherein suspend
Object content is high, it is difficult to meet reverse osmosis water inlet requirement.Without suitable pretreatment, it is continuously steady counter-infiltration system is not can guarantee
Fixed operation.
It is pre-processed in this technique using Millipore filtration techniques or ultra filtration technology.By pre-processing, in waste water
Suspended matter, such as fiber, elemental sulfur insoluble substance are removed, and filtered solution enters counter-infiltration system.
Enter primary reverse osmosis system by pretreated waste water and clear liquid.Waste water is divided into two parts: film concentrate and film are saturating
Cross liquid.Wherein salinity includes that sodium sulphate, zinc sulfate, sulfuric acid etc. enter film concentrate end, realizes initial concentration.And film permeate end
Middle acid and zinc sulfate, sodium sulphate are removed, and can realize reuse directly as process water.And initial concentration is passed through at film concentrate end
Film concentrate, be further concentrated into two-pass reverse osmosis.Two-pass reverse osmosis is designed using super-pressure, will be inorganic in waste water
Salt, acid etc. are further concentrated, and concentrate enters back into evaporator and is evaporated concentration, carry out sulfate crystal.
By evaporator concentration, crystallization, mother liquor is the concentrated sulfuric acid, and contains a certain amount of sodium sulphate and zinc sulfate, can be straight
It connects and is back to use in coagulating bath as sulfuric acid.So that sulfuric acid and zinc sulfate are recycled.
Using above-mentioned dual-membrane process, the inexpensive reuse for realizing sodium sulphate, sulfuric acid, zinc sulfate, while without solid
The discharge of waste, water realize reuse.
Specific embodiment
Embodiment 1
90-95 degrees Celsius of acid waste water, consisting of: sulfuric acid 10-20g/L, sodium sulphate 40-60g/L, zinc sulfate 1-
2g/L, remaining is organic matter and sulfide.After the water is placed in storage tank stop a few hours, by being pumped into heat-exchange system, acid waste water
Temperature is reduced to 40 degrees Celsius, is then pre-processed, and suspended matter completely removes after ultrafiltration, filtrate clear, filtrate
Into counter-infiltration system.It is handled by primary reverse osmosis system, operating pressure≤4Mpa, temperature≤40 degree Celsius, film concentrate
In total TDS reach 8-10%, film concentrate enters two-stage reverse osmosis system.Two-pass reverse osmosis, operating pressure≤10MPa are dense
It is reduced to total TDS and reaches 10-18%.The film concentrate is after the multi-effect evaporator concentration with heat pump assembly, into crystallization
Tank crystallization, side charging, side crystallization cause sulfuric acid concentration to reach reuse requirement, are centrifuged, obtain sulfate crystal and crystallization
Mother liquor.By sulfate crystal through being dried to obtain anhydrous sodium sulfate.Crystalline mother solution is back to use in coagulating bath.
Sulfate crystal is as commodity selling.Mother liquor after separating sodium sulfate is mainly the concentrated sulfuric acid and zinc sulfate, is back to use
In acid bath, closed cycle is realized.
The implementation process of technique: the film concentrate of two-pass reverse osmosis is improved, evaporation knot is entered after heat-exchange system exchanges heat
Crystallographic system system.The heat source of heat exchange comes tap water (acid waste water), or the water with water heat exchange.
Embodiment 2
10M390-95 degrees Celsius of acid waste water, TDS 4%.It is stopped in merging tank, by plate heat exchanger by water temperature
40 degrees Celsius are dropped to, enters doughnut through pump and surpasses/microfiltration systems, filtrate is placed in tank.Hollow-fibre membrane surpasses/microfiltration systems,
Using 0.1 micron of membrane aperture.System is designed using constant current, and with the progress of filtering, the transmembrane pressure of system is gradually increased.Wait reach
System automatic back-washing after to setting pressure difference.The ultrafiltration water rate of recovery reaches 98%.Ultrafiltrate enters counter-infiltration system.
Delivered into counter-infiltration system from tank by pump by the filtrate of micro-filtration, operating pressure from 3 to 10MPa, with
The progress of concentration, the increase of concentrate end concentration, pressure are gradually increased.Reach 18% to concentrate TDS, concentrate enters second level
It is reverse osmosis.Filter liquor passes through activated-charcoal column, and direct reuse is into technique.Control temperature≤40 degree Celsius.
Concentrate enters evaporation and crystallization system condensing crystallizing.Reverse osmosis filtrate direct reuse.Or pass through activated carbon adsorption
Afterwards, reuse.
Reverse osmosis film concentrate enters multi-effect evaporator and is evaporated, until forming supersaturated solution, is sent into crystallizer,
The crystal constantly generated, material are separated by solid-liquid separation by centrifuge, and clear liquid sends multiple-effect after Clear liquid tank and the mixing of overflow clear liquid back to
Evaporator continues evaporation, crystallization, solid phase discharge system.Sulfate crystal is obtained, dry, temperature obtains anhydrous sodium sulfate knot
It is brilliant.It is so repeated several times, until the acid concentration of centrifugal clear liquid meets reuse concentration.Crystalline mother solution is the concentrated sulfuric acid and zinc sulfate.
It is back to use in acid bath.
Embodiment 3
10M390-95 degrees Celsius of acid waste water, TDS 8%.It is stopped in merging tank, enters ceramics through pump and surpass/micro-filtration system
System, filtrate are placed in tank.Ceramic membrane surpasses/microfiltration systems, using 0.1 micron of membrane aperture.System is designed using constant current, with filtering
Progress, the transmembrane pressure of system gradually increases.The ultrafiltration water rate of recovery reaches 98%.Ultrafiltrate passes through plate heat exchanger for water
Temperature drop is directly entered dish-style counter-infiltration system to 40 degrees Celsius.Operating pressure 4MPa to 10MPa.As the concentration of concentrate increases
Add, pressure is stepped up.TDS reaches 20% from 8% in concentrate.Concentrate enters evaporation and crystallization system condensing crystallizing.Second level
After reverse osmosis filtrate is directly over activated carbon adsorption, direct reuse.
Reverse osmosis film concentrate enters with after multi-effect evaporator evaporation, and subsequent technique is the same as embodiment 2.
Claims (8)
1. a kind of comprehensive utilization process of viscose fiber acid waste water, which comprises the following steps:
A, it pre-processes
Viscose fiber acid waste water is filtered by filter, removes the suspended matter in waste water, filtered solution enters in next step
Rapid processing；
B, reverse osmosis
Filtered solution is imported into counter-infiltration system, obtains film concentrate and film permeate, film permeate is returned directly as process water
With film concentrate enters step C processing；
C, condensing crystallizing
After the film concentrate that reverse osmosis treatment obtains imports multi-effect evaporator concentration, it is sent into crystallizing tank crystallization, obtains sulfuric acid
Sodium crystallization, crystalline mother solution is sulfuric acid, and contains sodium sulphate and zinc sulfate, and direct reuse is into coagulating bath；
Viscose fiber acid waste water contains sulfuric acid, sodium sulphate, zinc sulfate；
The pretreatment further includes that viscose fiber acid waste water is reduced the temperature to≤40 DEG C by heat exchanger, which is placed on
Before filter or after filter；
The counter-infiltration system uses anti-pollution and acidproof reverse-osmosis membrane element, and the anti-pollution and acidproof reverse-osmosis membrane element are to chlorine
Change the interception capacity of sodium 98% or more.
2. the comprehensive utilization process of viscose fiber acid waste water as described in claim 1, which is characterized in that mistake described in step A
Filter use ultrafiltration membrane filter or microporous filtration, pore size filter be 0.01-1 μm, filter method be dead-end filtration or
Cross-flow filtration or using one or both of dead-end filtration, cross-flow filtration form combination, membrane component using tubular type, it is board-like,
Dish-style, rolling or capillary type.
3. the comprehensive utilization process of viscose fiber acid waste water as claimed in claim 2, which is characterized in that use cross-flow filtration
When, film surface flow control is controlled in 0.1~1MPa, operation temperature at 1~90 DEG C in 2~6 meter per seconds, operating pressure control.
4. the comprehensive utilization process of viscose fiber acid waste water as claimed in claim 2, which is characterized in that use dead-end filtration
When, membrane component uses external pressing type hollow fibrous membrane, and designs filtrate backwash and air bump rinse operation, when the transmembrane pressure of film is more than setting
When value, system starts backwash procedure；Filtrate enters influent side by producing water section, film surface pollutant is taken away, to restore
Membrane flux.
5. the comprehensive utilization process of viscose fiber acid waste water as described in claim 1, which is characterized in that the reverse osmosis system
The equipment of system includes that feed water by reverse osmosis pump, reverse osmosis charge filter, reverse osmosis high-pressure pump and reverse osmosis units, each equipment pass through
Pipeline is connected, and the filtered solution come from filter is successively pumped through feed water by reverse osmosis pump, reverse osmosis charge filter and reverse osmosis high-pressure
Into reverse osmosis units, after reverse osmosis treatment, film permeate enters step C directly as process water reuse, film concentrate,
Further concentration.
6. the comprehensive utilization process of viscose fiber acid waste water as described in claim 1, which is characterized in that the reverse osmosis system
System includes concatenated multi-stage reverse osmosis equipment, and the filtered solution come from filter initially enters first order reverse osmosis equipment, the first order
The film concentrate of reverse osmosis equipment enters second level reverse osmosis equipment, and the film concentrate of second level reverse osmosis equipment enters the third level
Reverse osmosis equipment, the film concentrate of afterbody reverse osmosis equipment to concentrate transfer tank；The film of reverse osmosis equipments at different levels penetrates
Liquid summarizes centralized collection as reverse osmosis produced water, and the reverse osmosis produced water is as industrial water reuse.
7. the comprehensive utilization process of viscose fiber acid waste water as claimed in claim 6, which is characterized in that the multistage reverse osmosis
Saturating every grade of equipment respectively includes the reverse-osmosis circulating pump and one group of reverse osmosis membrane group of series winding setting, upper level reverse osmosis equipment
The film concentrate of reverse osmosis membrane group enters the reverse-osmosis circulating pump of next stage reverse osmosis equipment or enters concentrate transfer tank, finally
The film concentrate of the reverse osmosis membrane group of first-stage reverse osmosis equipment is directly entered concentrate transfer tank；The reverse osmosis of reverse osmosis equipments at different levels
The film permeate centralized collection of permeable membrane group is as reverse osmosis produced water, and the reverse osmosis produced water is as industrial water reuse.
8. the comprehensive utilization process of viscose fiber acid waste water as described in claim 1, which is characterized in that the reverse osmosis system
The operating pressure of system is controlled in 1-10Mpa.
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| CN111362444A (en) * | 2020-04-24 | 2020-07-03 | 莱特莱德（北京）环境技术股份有限公司 | Viscose fiber acid wastewater sulfuric acid recycling system and recycling method |
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| CN112390440B (en) * | 2020-10-16 | 2023-05-23 | 唐山三友远达纤维有限公司 | Method for recycling acidic water in spinning workshop |
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