CN108821244A - The recovery process of alkali and catalyst in a kind of desulfurization waste liquor - Google Patents

The recovery process of alkali and catalyst in a kind of desulfurization waste liquor Download PDF

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Publication number
CN108821244A
CN108821244A CN201810655359.0A CN201810655359A CN108821244A CN 108821244 A CN108821244 A CN 108821244A CN 201810655359 A CN201810655359 A CN 201810655359A CN 108821244 A CN108821244 A CN 108821244A
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doctor solution
concentration
kettle
alkali
catalyst
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项裕桥
何相君
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Ningbo Zhongke Far East Catalytic Engineering Technology Co Ltd
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Ningbo Zhongke Far East Catalytic Engineering Technology Co Ltd
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Priority to CN201810655359.0A priority Critical patent/CN108821244A/en
Publication of CN108821244A publication Critical patent/CN108821244A/en
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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
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/64—Thiosulfates; Dithionites; Polythionates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/22—Alkali metal sulfides or polysulfides
    • C01B17/32—Hydrosulfides of sodium or potassium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C3/00—Cyanogen; Compounds thereof
    • C01C3/20—Thiocyanic acid; Salts thereof
    • 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
    • C01D5/16—Purification
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D7/00—Carbonates of sodium, potassium or alkali metals in general
    • C01D7/22—Purification
    • C01D7/24—Crystallisation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/584—Recycling of catalysts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses the recovery process of alkali and catalyst in a kind of desulfurization waste liquor, include the following steps：Flush distillation concentration, filters pressing recycling, decoloration filters pressing, double evaporation-cooling concentration, crystallization centrifugation.Beneficial effects of the present invention are：The technique can not only extract sodium sulfocyanate, the sodium thiosulfate in desulfurization waste liquor, and can recycle alkali (sodium carbonate, sodium bicarbonate) and catalyst, improve the utilization of resources.

Description

The recovery process of alkali and catalyst in a kind of desulfurization waste liquor
Technical field
The present invention relates to desulfurization waste liquor processing, in particular to the recovery process of alkali and catalyst in a kind of desulfurization waste liquor.
Background technique
In China, atmosphere pollution is serious, and exhaust gas total emission volumn is in higher level.Therefore, we want strict control to pollute Discharge, the desulfurization workshop section of coke-oven plant are namely based on this reason and set up.Coke-oven plant of China generallys use wet desulphurization, correspondingly, Desulfurization workshop section will generate desulfurization waste liquor.Desulfurization waste liquor rationally using being equally control disposal of pollutants, improves the weight of the utilization of resources Want behave.
The Chinese patent of Publication No. CN103213953A discloses a kind of by desulfurization waste liquor extraction ATS (Ammonium thiosulphate), sulphur cyanogen The technique of ammonium.The technique is specific as follows：, through the filtered doctor solution of active carbon, will be pumped by conveying from desulphurization system One evaporator, for material after the heating of external heater, part returns to the first evaporator in the first evaporator, and part is sent into second and is steamed Send out device.Material partially returns to the second evaporator after the heating of external heater in second evaporator；Third evaporator is sent into part. Material returns to third evaporator after external heater indirect heating in third evaporator.Second evaporator, third evaporator The water vapour of the first evaporator evaporation generation is all made of as heat source.Third base of evaporator material is pumped into knot by crystallizing In brilliant device, crystallized liquid carries out separating treatment, and isolated solid is the product containing ATS (Ammonium thiosulphate), and centrifugate is further after collecting Crystallization, obtains the product containing ammonium thiocyanate.
But the technique only extracts ATS (Ammonium thiosulphate) from desulfurization waste liquor and ammonium thiocyanate, remaining waste water still need to outlet, leads It causes alkali (carbonate, bicarbonate) and catalyst in desulfurization waste liquor to be also discharged, causes the waste of resource, have much room for improvement.
Summary of the invention
The object of the present invention is to provide the recovery process of a kind of recycling alkali and catalyst.The technique can not only be useless to desulfurization Sodium sulfocyanate, sodium thiosulfate in liquid extract, and can recycle alkali (sodium carbonate, sodium bicarbonate) and catalyst, mention The high utilization of resources.
Above-mentioned technical purpose of the invention technical scheme is that：
The recovery process of alkali and catalyst in a kind of desulfurization waste liquor, includes the following steps：Flush distillation concentration, filters pressing are returned It receives, decoloration filters pressing, double evaporation-cooling concentration, crystallization centrifugation.
The present invention is further arranged to：The flush distillation concentration step includes the following steps：Desulfurization waste liquor is introduced into de- Sulphur flow container, then doctor solution preheater is pumped by once concentration charging, it is primary that the doctor solution after preheating enters doctor solution Concentration kettle；The pressure recovery step includes the following steps：Doctor solution after being once concentrated is pumped by soda ash filtering Soda ash filter is once filtered, and the filtrate once filtered enters bleacher, and the filter cake once filtered recycles；It is described de- Color filters pressing step includes the following steps：Active carbon is added while stirring the filtrate of bleacher, active carbon continues to stir after adding, It stands after mixing evenly, is then pumped into activated carbon filter with active carbon filtering and carries out secondary filter, the filter cake of secondary filter It recycles, the filtrate of secondary filter enters decoloration Clear liquid tank；The double evaporation-cooling concentration step includes the following steps：Decoloration is clear Filtrate in flow container is pumped into doctor solution secondary concentration kettle by secondary concentration charging；The crystallization centrifugation step includes following step Suddenly：Doctor solution after secondary concentration, which enters, carries out crystallisation by cooling in crystallization kettle, be centrifuged subsequently into centrifuge, Crude salt is obtained, filtrate recycles.
The present invention is further arranged to：The temperature of concentration kettle of doctor solution is 80-90 DEG C, and pressure is -0.1- 0.03MPa, the doctor solution are evaporated to doctor solution density in 1450-1650kg/m in concentration kettle of doctor solution3When be sent into Soda ash filter.
The present invention is further arranged to：The temperature of the doctor solution secondary concentration kettle is 80-90 DEG C, and pressure is -0.1- 0.03MPa, the doctor solution are sent into crystallization kettle when be concentrated by evaporation in concentration kettle of doctor solution to liquid in kettle into syrupy shape.
The present invention is further arranged to：Concentration kettle of the doctor solution and doctor solution secondary concentration kettle are passed through low pressure steaming Vapour.
The present invention is further arranged to：The pressure of the soda ash filter press is maintained at 0.5MPa.
The present invention is further arranged to：The additional amount of the active carbon is 1-3% of filtrate weight in bleacher, the work Property charcoal filtrate temperature is 80 DEG C in bleacher when being added, filtrate is added active carbon and stands 8h after mixing evenly in the bleacher.
The present invention is further arranged to：Crystallisation by cooling 1.5h in the crystallization centrifugation step.
The present invention is further arranged to：The steam condensate that concentration kettle of the doctor solution obtains enters doctor solution preheating Device.
The present invention is further arranged to：The steam that concentration kettle of the doctor solution obtains enters doctor solution secondary concentration Kettle.
In conclusion the invention has the advantages that：
1, alkali and catalyst are recycled before desulfurization waste liquor decoloration, the alkali and catalyst of recycling, which return to desulphurization system circulation, to be made With, not only reduce the consumption of alkali desulphurization system alkali and catalyst, but also due to extract sodium thiosulfate and sodium sulfocyanate it Before, alkali and catalyst are taken out, solid content when sodium thiosulfate and ammonium thiocyanate extraction is reduced, to reduce corresponding molten Agent and power consumption, thus reduce extract sodium thiosulfate, NaHS device operating cost, not only handled desulfurization waste liquor but also Increase benefit；
2, in flush distillation concentration process, sodium bicarbonate is heated to be decomposed into sodium carbonate, thus carbonic acid in increase system Sodium content, and then sodium carbonate in system is caused first to be in hypersaturated state and be precipitated, the sodium carbonate part of precipitation can absorb again Carbon dioxide and generate sodium bicarbonate.In double evaporation-cooling concentration process, sodium thiosulfate, NaHS and sodium sulphate are analysed Out.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Below in conjunction with attached drawing, invention is further described in detail.
1-5 low pressure steam of embodiment is the vapor of 0.4MPa, and desulfurization waste liquor, which derives from, uses sodium carbonate, carbonic acid Wet oxidation desulfurization system of the hydrogen sodium as alkali source.
In embodiment 1-5, the treating capacity of desulfurization waste liquor is 50m3The composition of/d, desulfurization waste liquor are shown in Table 1：
Embodiment 1
Referring to Fig.1, the recovery process of alkali and catalyst in a kind of desulfurization waste liquor, includes the following steps：Flush distillation concentration, Filters pressing recycling, decoloration filters pressing, double evaporation-cooling concentration, crystallization centrifugation.
Flush distillation concentration step includes the following steps：Desulfurization waste liquor is introduced into desulfurization flow container, then by be once concentrated into Material is pumped into doctor solution preheater and is preheated to 62 DEG C, and the doctor solution after preheating enters concentration kettle of doctor solution.Doctor solution One time concentration kettle is provided with agitating device and inner coil pipe, while being equipped with pressure gauge, thermometer and densitometer, is passed through low-pressure steam Vacuum evaporation operation is carried out, controlled at 80 DEG C, pressure 0.01MPa, is evaporated to doctor solution density in 1650kg/m3When give Enter soda ash filter.It is useless that the steam condensate that concentration kettle of doctor solution is evaporated returns to the pre- thermally desulfurizing of doctor solution preheater Liquid.
Pressure recovery step includes the following steps：Doctor solution after being once concentrated is pumped into soda ash by soda ash filtering Filter is once filtered, and the pressure of soda ash filter press is maintained at 0.5MPa, and the filtrate once filtered enters bleacher, and one The filter cake of secondary filtering is alkali (sodium carbonate, sodium bicarbonate) and catalyst, is recycled to the filter cake once filtered, and desulfurization is returned Workshop section uses as alkali source needed for desulfurization.
Decoloration filters pressing step includes the following steps：The filtrate for stirring bleacher is added 1% of filtrate weight in bleacher simultaneously Active carbon, control bleacher in filtrate temperature be 80 DEG C, active carbon continues to stir after adding, and stands 8h after mixing evenly, so Activated carbon filter is pumped into active carbon filtering afterwards and carries out secondary filter, and the filter cake of secondary filter is waste active carbon, to secondary The filter cake of filtering is recycled, and coal blending is sent to, and the filtrate of secondary filter enters decoloration Clear liquid tank.
Double evaporation-cooling concentration step includes the following steps：Filtrate in decoloration Clear liquid tank is pumped by secondary concentration charging Doctor solution secondary concentration kettle.Doctor solution secondary concentration evaporating kettle is provided with agitating device and inner coil pipe, while being equipped with pressure gauge And thermometer, it is passed through low-pressure steam and carries out vacuum evaporation operation, controlled at 80 DEG C, pressure 0.01MPa, be concentrated by evaporation extremely When liquid is at syrupy shape in kettle, terminate evaporation, is sent into crystallization kettle.Low-pressure steam in doctor solution secondary concentration evaporating kettle first uses The steam that concentration and evaporation of doctor solution comes out.When the steam deficiency that concentration and evaporation of doctor solution comes out, in addition supplement low Steam is pressed, steam consumption is saved, reduces operating cost.
Crystallization centrifugation step includes the following steps：Doctor solution after secondary concentration, which enters in crystallization kettle, carries out cooling knot Brilliant 1.5h, crystallization kettle are provided with electric mixing device and external jacket cooling device, are centrifuged subsequently into centrifuge, obtain To crude salt, filtrate recycling returns to former desulphurization system and continues reuse.
Embodiment 2
Referring to Fig.1, the recovery process of alkali and catalyst in a kind of desulfurization waste liquor, includes the following steps：Flush distillation concentration, Filters pressing recycling, decoloration filters pressing, double evaporation-cooling concentration, crystallization centrifugation.
Flush distillation concentration step includes the following steps：Desulfurization waste liquor is introduced into desulfurization flow container, then by be once concentrated into Material is pumped into doctor solution preheater and is preheated to 65 DEG C, and the doctor solution after preheating enters concentration kettle of doctor solution.Doctor solution One time concentration kettle is provided with agitating device and inner coil pipe, while being equipped with pressure gauge, thermometer and densitometer, is passed through low-pressure steam Vacuum evaporation operation is carried out, controlled at 82 DEG C, pressure is -0.03MPa, is evaporated to doctor solution density in 1450kg/m3When It is sent into soda ash filter.It is useless that the steam condensate that concentration kettle of doctor solution is evaporated returns to the pre- thermally desulfurizing of doctor solution preheater Liquid.
Pressure recovery step includes the following steps：Doctor solution after being once concentrated is pumped into soda ash by soda ash filtering Filter is once filtered, and the pressure of soda ash filter press is maintained at 0.5MPa, and the filtrate once filtered enters bleacher, and one The filter cake of secondary filtering is alkali (sodium carbonate, sodium bicarbonate) and catalyst, is recycled to the filter cake once filtered, and desulfurization is returned Workshop section uses as alkali source needed for desulfurization.
Decoloration filters pressing step includes the following steps：The same of the filtrate for stirring bleacher is added in the filtrate for stirring bleacher simultaneously When be added bleacher in filtrate weight 2% active carbon, control bleacher in filtrate temperature be 80 DEG C, active carbon adds subsequent Continuous stirring, stands 8h after mixing evenly, is then pumped into activated carbon filter with active carbon filtering and carries out secondary filter, secondary mistake The filter cake of filter is waste active carbon, is recycled to the filter cake of secondary filter, sends to coal blending, it is clear that the filtrate of secondary filter enters decoloration Flow container.
Double evaporation-cooling concentration step includes the following steps：Filtrate in decoloration Clear liquid tank is pumped by secondary concentration charging Doctor solution secondary concentration kettle.Doctor solution secondary concentration evaporating kettle is provided with agitating device and inner coil pipe, while being equipped with pressure gauge And thermometer, it is passed through low-pressure steam and carries out vacuum evaporation operation, controlled at 82 DEG C, pressure is -0.03MPa, is concentrated by evaporation When liquid is at syrupy shape in kettle, terminate evaporation, is sent into crystallization kettle.Low-pressure steam in doctor solution secondary concentration evaporating kettle is first adopted The steam come out with concentration and evaporation of doctor solution.When the steam deficiency that concentration and evaporation of doctor solution comes out, in addition supplement Low-pressure steam saves steam consumption, reduces operating cost.
Crystallization centrifugation step includes the following steps：Doctor solution after secondary concentration, which enters in crystallization kettle, carries out cooling knot Brilliant 1.5h, crystallization kettle are provided with electric mixing device and external jacket cooling device, are centrifuged subsequently into centrifuge, obtain To crude salt, filtrate recycling returns to former desulphurization system and continues reuse.
Embodiment 3
Referring to Fig.1, the recovery process of alkali and catalyst in a kind of desulfurization waste liquor, includes the following steps：Flush distillation concentration, Filters pressing recycling, decoloration filters pressing, double evaporation-cooling concentration, crystallization centrifugation.
Flush distillation concentration step includes the following steps：Desulfurization waste liquor is introduced into desulfurization flow container, then by be once concentrated into Material is pumped into doctor solution preheater and is preheated to 60 DEG C, and the doctor solution after preheating enters concentration kettle of doctor solution.Doctor solution One time concentration kettle is provided with agitating device and inner coil pipe, while being equipped with pressure gauge, thermometer and densitometer, is passed through low-pressure steam Vacuum evaporation operation is carried out, controlled at 84 DEG C, pressure is -0.06MPa, is evaporated to doctor solution density in 1500kg/m3When It is sent into soda ash filter.It is useless that the steam condensate that concentration kettle of doctor solution is evaporated returns to the pre- thermally desulfurizing of doctor solution preheater Liquid.
Pressure recovery step includes the following steps：Doctor solution after being once concentrated is pumped into soda ash by soda ash filtering Filter is once filtered, and the pressure of soda ash filter press is maintained at 0.5MPa, and the filtrate once filtered enters bleacher, and one The filter cake of secondary filtering is alkali (sodium carbonate, sodium bicarbonate) and catalyst, is recycled to the filter cake once filtered, and desulfurization is returned Workshop section uses as alkali source needed for desulfurization.
Decoloration filters pressing step includes the following steps：The filtrate for stirring bleacher is added 3% of filtrate weight in bleacher simultaneously Active carbon, control bleacher in filtrate temperature be 80 DEG C, active carbon continues to stir after adding, and stands 8h after mixing evenly, so Activated carbon filter is pumped into active carbon filtering afterwards and carries out secondary filter, and the filter cake of secondary filter is waste active carbon, to secondary The filter cake of filtering is recycled, and coal blending is sent to, and the filtrate of secondary filter enters decoloration Clear liquid tank.
Double evaporation-cooling concentration step includes the following steps：Filtrate in decoloration Clear liquid tank is pumped by secondary concentration charging Doctor solution secondary concentration kettle.Doctor solution secondary concentration evaporating kettle is provided with agitating device and inner coil pipe, while being equipped with pressure gauge And thermometer, it is passed through low-pressure steam and carries out vacuum evaporation operation, controlled at 84 DEG C, pressure is -0.06MPa, is concentrated by evaporation When liquid is at syrupy shape in kettle, terminate evaporation, is sent into crystallization kettle.Low-pressure steam in doctor solution secondary concentration evaporating kettle is first adopted The steam come out with concentration and evaporation of doctor solution.When the steam deficiency that concentration and evaporation of doctor solution comes out, in addition supplement Low-pressure steam saves steam consumption, reduces operating cost.
Crystallization centrifugation step includes the following steps：Doctor solution after secondary concentration, which enters in crystallization kettle, carries out cooling knot Brilliant 1.5h, crystallization kettle are provided with electric mixing device and external jacket cooling device, are centrifuged subsequently into centrifuge, obtain To crude salt, filtrate recycling returns to former desulphurization system and continues reuse.
Embodiment 4
Referring to Fig.1, the recovery process of alkali and catalyst in a kind of desulfurization waste liquor, includes the following steps：Flush distillation concentration, Filters pressing recycling, decoloration filters pressing, double evaporation-cooling concentration, crystallization centrifugation.
Flush distillation concentration step includes the following steps：Desulfurization waste liquor is introduced into desulfurization flow container, then by be once concentrated into Material is pumped into doctor solution preheater and is preheated to 67 DEG C, and the doctor solution after preheating enters concentration kettle of doctor solution.Doctor solution One time concentration kettle is provided with agitating device and inner coil pipe, while being equipped with pressure gauge, thermometer and densitometer, is passed through low-pressure steam Vacuum evaporation operation is carried out, controlled at 87 DEG C, pressure is -0.1MPa, is evaporated to doctor solution density in 1480kg/m3When give Enter soda ash filter.It is useless that the steam condensate that concentration kettle of doctor solution is evaporated returns to the pre- thermally desulfurizing of doctor solution preheater Liquid.
Pressure recovery step includes the following steps：Doctor solution after being once concentrated is pumped into soda ash by soda ash filtering Filter is once filtered, and the pressure of soda ash filter press is maintained at 0.5MPa, and the filtrate once filtered enters bleacher, and one The filter cake of secondary filtering is alkali (sodium carbonate, sodium bicarbonate) and catalyst, is recycled to the filter cake once filtered, and desulfurization is returned Workshop section uses as alkali source needed for desulfurization.
Decoloration filters pressing step includes the following steps：The same of the filtrate for stirring bleacher is added in the filtrate for stirring bleacher simultaneously When be added bleacher in filtrate weight 1% active carbon, control bleacher in filtrate temperature be 80 DEG C, active carbon adds subsequent Continuous stirring, stands 8h after mixing evenly, is then pumped into activated carbon filter with active carbon filtering and carries out secondary filter, secondary mistake The filter cake of filter is waste active carbon, is recycled to the filter cake of secondary filter, sends to coal blending, it is clear that the filtrate of secondary filter enters decoloration Flow container.
Double evaporation-cooling concentration step includes the following steps：Filtrate in decoloration Clear liquid tank is pumped by secondary concentration charging Doctor solution secondary concentration kettle.Doctor solution secondary concentration evaporating kettle is provided with agitating device and inner coil pipe, while being equipped with pressure gauge And thermometer, it is passed through low-pressure steam and carries out vacuum evaporation operation, controlled at 87 DEG C, pressure is -0.1MPa, is concentrated by evaporation extremely When liquid is at syrupy shape in kettle, terminate evaporation, is sent into crystallization kettle.Low-pressure steam in doctor solution secondary concentration evaporating kettle first uses The steam that concentration and evaporation of doctor solution comes out.When the steam deficiency that concentration and evaporation of doctor solution comes out, in addition supplement low Steam is pressed, steam consumption is saved, reduces operating cost.
Crystallization centrifugation step includes the following steps：Doctor solution after secondary concentration, which enters in crystallization kettle, carries out cooling knot Brilliant 1.5h, crystallization kettle are provided with electric mixing device and external jacket cooling device, are centrifuged subsequently into centrifuge, obtain To crude salt, filtrate recycling returns to former desulphurization system and continues reuse.
Embodiment 5
Referring to Fig.1, the recovery process of alkali and catalyst in a kind of desulfurization waste liquor, includes the following steps：Flush distillation concentration, Filters pressing recycling, decoloration filters pressing, double evaporation-cooling concentration, crystallization centrifugation.
Flush distillation concentration step includes the following steps：Desulfurization waste liquor is introduced into desulfurization flow container, then by be once concentrated into Material is pumped into doctor solution preheater and is preheated to 70 DEG C, and the doctor solution after preheating enters concentration kettle of doctor solution.Doctor solution One time concentration kettle is provided with agitating device and inner coil pipe, while being equipped with pressure gauge, thermometer and densitometer, is passed through low-pressure steam Vacuum evaporation operation is carried out, controlled at 90 DEG C, pressure 0.03MPa, is evaporated to doctor solution density in 1550kg/m3When give Enter soda ash filter.It is useless that the steam condensate that concentration kettle of doctor solution is evaporated returns to the pre- thermally desulfurizing of doctor solution preheater Liquid.
Pressure recovery step includes the following steps：Doctor solution after being once concentrated is pumped into soda ash by soda ash filtering Filter is once filtered, and the pressure of soda ash filter press is maintained at 0.5MPa, and the filtrate once filtered enters bleacher, and one The filter cake of secondary filtering is alkali (sodium carbonate, sodium bicarbonate) and catalyst, is recycled to the filter cake once filtered, and desulfurization is returned Workshop section uses as alkali source needed for desulfurization.
Decoloration filters pressing step includes the following steps：The filtrate for stirring bleacher is added 2% of filtrate weight in bleacher simultaneously Active carbon, control bleacher in filtrate temperature be 80 DEG C, active carbon continues to stir after adding, and stands 8h after mixing evenly, so Activated carbon filter is pumped into active carbon filtering afterwards and carries out secondary filter, and the filter cake of secondary filter is waste active carbon, to secondary The filter cake of filtering is recycled, and coal blending is sent to, and the filtrate of secondary filter enters decoloration Clear liquid tank.
Double evaporation-cooling concentration step includes the following steps：Filtrate in decoloration Clear liquid tank is pumped by secondary concentration charging Doctor solution secondary concentration kettle.Doctor solution secondary concentration evaporating kettle is provided with agitating device and inner coil pipe, while being equipped with pressure gauge And thermometer, it is passed through low-pressure steam and carries out vacuum evaporation operation, controlled at 90 DEG C, pressure 0.03MPa, be concentrated by evaporation extremely When liquid is at syrupy shape in kettle, terminate evaporation, is sent into crystallization kettle.Low-pressure steam in doctor solution secondary concentration evaporating kettle first uses The steam that concentration and evaporation of doctor solution comes out.When the steam deficiency that concentration and evaporation of doctor solution comes out, in addition supplement low Steam is pressed, steam consumption is saved, reduces operating cost.
Crystallization centrifugation step includes the following steps：Doctor solution after secondary concentration, which enters in crystallization kettle, carries out cooling knot Brilliant 1.5h, crystallization kettle are provided with electric mixing device and external jacket cooling device, are centrifuged subsequently into centrifuge, obtain To crude salt, filtrate recycling returns to former desulphurization system and continues reuse.
The present embodiment is only explanation of the invention, is not limitation of the present invention, and those skilled in the art exist It can according to need the modification that not creative contribution is made to the present embodiment after reading this specification, but as long as in the present invention Scope of the claims in all by the protection of Patent Law.

Claims (10)

1. the recovery process of alkali and catalyst in a kind of desulfurization waste liquor, it is characterized in that：Include the following steps：Flush distillation concentration, Filters pressing recycling, decoloration filters pressing, double evaporation-cooling concentration, crystallization centrifugation.
2. the recovery process of alkali and catalyst in desulfurization waste liquor according to claim 1, it is characterized in that：The flush distillation Concentration step includes the following steps：Desulfurization waste liquor is introduced into desulfurization flow container, then by once concentration charging to be pumped into doctor solution pre- Hot device, the doctor solution after preheating enter concentration kettle of doctor solution；The pressure recovery step includes the following steps：By Doctor solution after primary concentration is pumped into soda ash filter by soda ash filtering and is once filtered, and the filtrate once filtered enters Bleacher, the filter cake once filtered recycle；The decoloration filters pressing step includes the following steps：Stir the filtrate of bleacher Active carbon is added simultaneously, active carbon continues to stir, stand after mixing evenly after adding, and is then pumped into activity with active carbon filtering Charcoal filter carries out secondary filter, and the filter cake of secondary filter recycles, and the filtrate of secondary filter enters decoloration Clear liquid tank；It is described Double evaporation-cooling concentration step includes the following steps：Filtrate in decoloration Clear liquid tank is pumped into doctor solution two by secondary concentration charging Secondary concentration kettle；The crystallization centrifugation step includes the following steps：Doctor solution after secondary concentration, which enters in crystallization kettle, to carry out Crystallisation by cooling is centrifuged subsequently into centrifuge, obtains crude salt, and filtrate recycles.
3. the recovery process of alkali and catalyst in desulfurization waste liquor according to claim 2, it is characterized in that：The doctor solution one The temperature of secondary concentration kettle is 80-90 DEG C, and pressure is -0.1-0.03MPa, and the doctor solution evaporates in concentration kettle of doctor solution To doctor solution density in 1450-1650kg/m3When be sent into soda ash filter.
4. the recovery process of alkali and catalyst in desulfurization waste liquor according to claim 2, it is characterized in that：The doctor solution two The temperature of secondary concentration kettle is 80-90 DEG C, and pressure is -0.1-0.03MPa, and the doctor solution evaporates in concentration kettle of doctor solution Crystallization kettle is sent into when being concentrated into kettle liquid into syrupy shape.
5. the recovery process of alkali and catalyst in desulfurization waste liquor according to claim 2, it is characterized in that：The doctor solution one Secondary concentration kettle and doctor solution secondary concentration kettle are passed through low-pressure steam.
6. the recovery process of alkali and catalyst in desulfurization waste liquor according to claim 2, it is characterized in that：The soda ash filters pressing The pressure of machine is maintained at 0.5MPa.
7. the recovery process of alkali and catalyst in desulfurization waste liquor according to claim 2, it is characterized in that：The active carbon Additional amount is the 1-3% of filtrate weight in bleacher, and filtrate temperature is 80 DEG C in bleacher when the active carbon is added, described de- Filtrate is added active carbon and stands 8h after mixing evenly in color tank.
8. the recovery process of alkali and catalyst in desulfurization waste liquor according to claim 2, it is characterized in that：The crystallization centrifugation Crystallisation by cooling 1.5h in step.
9. the recovery process of alkali and catalyst in desulfurization waste liquor according to claim 2, it is characterized in that：The doctor solution one The steam condensate that secondary concentration kettle obtains enters doctor solution preheater.
10. the recovery process of alkali and catalyst in desulfurization waste liquor according to claim 2, it is characterized in that：The doctor solution The steam that concentration kettle obtains enters doctor solution secondary concentration kettle.
CN201810655359.0A 2018-06-23 2018-06-23 The recovery process of alkali and catalyst in a kind of desulfurization waste liquor Pending CN108821244A (en)

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CN110393975A (en) * 2019-08-19 2019-11-01 山信软件股份有限公司 Doctor solution proposes the control method and system of refined salt
CN112174411A (en) * 2020-08-03 2021-01-05 宜兴市阳洋塑料助剂有限公司 Recovery and utilization of neutralization water in production process of plasticizer DOTP

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Publication number Priority date Publication date Assignee Title
CN110393975A (en) * 2019-08-19 2019-11-01 山信软件股份有限公司 Doctor solution proposes the control method and system of refined salt
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CN112174411A (en) * 2020-08-03 2021-01-05 宜兴市阳洋塑料助剂有限公司 Recovery and utilization of neutralization water in production process of plasticizer DOTP

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Application publication date: 20181116