CN109179453A - A kind of Crystallization Separation method for coking desulfurization waste water salt extraction extraction filter residue - Google Patents
A kind of Crystallization Separation method for coking desulfurization waste water salt extraction extraction filter residue Download PDFInfo
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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
- C01D5/18—Dehydration
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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
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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
- C01D5/004—Preparation in the form of granules, pieces or other shaped products
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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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The present invention relates to a kind of Crystallization Separation methods for coking desulfurization waste water salt extraction extraction filter residue；Under stirring action, coking desulfurization waste water salt extraction extraction filter residue is mixed with deionized water, 75~85 DEG C is warming up to, is completely dissolved extraction filter residue；Then quality is added into system is 4~7% active powdered carbon for extracting filter residue, is filtered after 1~3h of system adsorption bleaching；By the way of evaporative crystallization, adsorption bleaching filtrate is evaporated at 80 DEG C, obtains the crystal suspension of sodium sulphate, obtain technical grade sulfuric acid sodium product after filtration drying；The filtered mother liquor of evaporative crystallization is diluted with water, adding water quality is evaporate mother liquor quality 15~25%, feed liquid temperature is 70~80 DEG C, obtains the crystal suspension of sodium thiosulfate by the way of crystallisation by cooling afterwards, obtains technical grade sodium thiosulfate product after filtration drying.Anhydrous sodium sulfate product purity is up to 97.6% or more；Five water sodium thiosulfate product purities reach 99.2% or more.
Description
Technical field
The invention belongs to technical field of chemical separation, and in particular to a kind of to extract filter residue for coking desulfurization waste water salt extraction
Crystallization Separation method.
Background technique
Traditional thiosulfuric acid process for producing sodium is divided into the processes such as thio, oxidation, evaporation, crystallization, is by dilute sodium sulfide solution
It is concentrated and concentrated solution is made, then react at a certain temperature with Sulfur and generate sodium polysulfide solution, then rouse air oxygen metaplasia
Sodium thiosulfate finished product is made at dilute hypo solution, then through series of processes such as evaporation, concentration, crystallizations.Existing sulphur
Sodium thiosulfate preparation method complex process, the reaction time is long, and reaction process is difficult to control, pollution waste is serious, it is difficult to meet work
The needs that industry metaplasia produces.
The data that Chinese coking industry association announces show that the desulfurization wastewater that only coke plant generates can reach every
300~4,000,000 tons of year.Although complicated component and the chemical composition fluctuation of desulfurization wastewater are larger, application method for crystallising is extracted
Technical grade sulfur-bearing secondary salt out, not only can produce certain economic benefit can also realize the environmental protection concept of sustainable development.So
And it is big when that during extracting technical grade sodium sulfocyanate in coking desulfurization waste water, can be generated using extraction-crystallization coupling technique
Amount mainly contains the extraction filter residue of sodium thiosulfate and sodium sulphate.Because the extraction filter residue still remains organic pollutant,
Newest solid waste discharge standard is not met, is often arbitrarily stacked.But as the amount of extraction filter residue is increasing and sleet
Pollution of the extraction filter residue to soil caused by equal weather, so that more and more very urgent to the processing of this extraction filter residue.
It is comprehensive noted earlier as can be seen, one side sodium thiosulfate industrialized production is difficult but the huge market demand, separately
A large amount of sodium thiosulfate resources are wasted while desulfurization wastewater pollutes environment in one side coking industry, if can develop
The technique of purifying industrial grade sodium thiosulfate product, can solve above-mentioned two problems simultaneously from desulfurization wastewater.Currently, existing
Some documents study the method for coking desulfurization wastewater salt extraction extraction filter residue purification sodium thiosulfate, Chinese patent
CN105819406A is separated sodium thiosulfate using the method for crystallisation by cooling, and wherein it is total to account for extraction filter residue for sodium thiosulfate quality
The 75~85% of quality, 70~90 DEG C of solution temperature range, the dissolving ratio for extracting filter residue and clear water is 1.5~2.5:1, separation
Technique includes four dissolution, filtering, crystallisation by cooling, centrifuge separation steps, has obtained 1-3mm thiosulfuric acid sodium crystal.The technique
There are following three defects: (1) sodium thiosulfate crystal product granularity is smaller, is unable to satisfy the need of marketing industries grade product salt
It asks；(2) after isolating sodium thiosulfate, the new waste residue of sodium sulphate is mainly contained without further separation, there is no thoroughly solutions
Certainly pollution of the coking desulfurization waste water to environment；(3) isolated sodium thiosulfate purity and yield is unstable, i.e. separating technology weight
Renaturation is not high.
Summary of the invention
The extraction filter residue generated in desulfurization wastewater treatment process for further processing, separating-purifying of the present invention have obtained work
Industry grade sodium thiosulfate product and technical grade sulfuric acid sodium product.At the same time, the technical grade sodium thiosulfate product purified
Traditional Industrialization production pressure can be alleviated again, meet a certain amount of market demand.The invention discloses a kind of Crystallization Separation method,
Utilize ternary salt-water system Na2S2O3-Na2SO4-H2Evaporative crystallization-crystallisation by cooling coupling technique has been formulated in O phasor behavior.Phase
Than the reported separating technology in relation to extracting filter residue, purifying industrial grade sulphur can be efficiently separated using separating technology of the invention
Sodium thiosulfate and technical grade sulfuric acid sodium, realize the near-zero release of desulfurization wastewater, wherein technical grade sodium thiosulfate product granularity compared with
Big and even particle size distribution, and process repeatability is fine.
Technical scheme is as follows:
A kind of Crystallization Separation method for coking desulfurization waste water salt extraction extraction filter residue；Include the following steps:
1) under stirring action, coking desulfurization waste water salt extraction extraction filter residue is mixed with deionized water, is warming up to 75~85 DEG C,
It is completely dissolved extraction filter residue；
2) then into system be added quality be extraction filter residue 4~7% active powdered carbon, to system adsorption bleaching 1~
It is filtered after 3h；
3) by the way of evaporative crystallization, adsorption bleaching filtrate is evaporated at 80 DEG C, the crystal for obtaining sodium sulphate is suspended
Liquid obtains technical grade sulfuric acid sodium product after filtration drying；
4) the filtered mother liquor of evaporative crystallization is diluted with water, adding water quality is evaporate mother liquor quality 15~25%, material
Liquid temperature is 70~80 DEG C, the rear crystal suspension that sodium thiosulfate is obtained by the way of crystallisation by cooling, after filtration drying
Obtain technical grade sodium thiosulfate product.
The mass ratio of step 1) the deionized water dosage and coking desulfurization waste water salt extraction extraction filter residue dosage is preferably 1.0
~1.8:1.
In the step 3) evaporation and crystal process, the first evaporation rate evaporation 0.5 with opposite system gross mass 2~6%~
Anhydrous sodium sulfate crystal seed is added to system in 1.5h, and constant temperature 0.5~1h of growing the grain is then proceeded to opposite system gross mass 2~6%
Evaporation rate evaporate 3.0~4.0h, steam water in total and account for system gross mass 18%~25%, 0.5~1h of constant temperature.
During the step 4) crystallisation by cooling, first with the rate of temperature fall of 15~20 DEG C/h, material is cooled to 35~45
DEG C, five water sodium thiosulfate crystal seeds, constant temperature 0.5~1.0h of growing the grain, then with the rate of temperature fall of 5~10 DEG C/h, by material is added
10~20 DEG C are cooled to, 0.5~1.0h of constant temperature.
Crystal seed preferred mass is extract filter residue 0.05~0.1% in the step 3) or step 4).
The preferred drying condition of step 4) the technical grade sulfuric acid sodium is dry 1.0 in 50~60 DEG C of blast drier~
3.0h。
The preferred drying condition of step 4) the technical grade sodium thiosulfate is dry in 30~40 DEG C of blast drier
1.0~2.0h.
Sodium thiosulfate quality accounts for the 85~90% of gross mass in the coking desulfurization waste water salt extraction extraction filter residue, sulfuric acid
Sodium quality accounts for the 9~14% of gross mass, and the quality sum of sodium thiosulfate and sodium sulphate accounts for 99% of gross mass or more, remaining
Part is mainly the insoluble matters such as silt, and is filtered together with the active powdered carbon after absorption.Extract filter residue mainly from
Sodium sulfocyanate workshop section is extracted in upstream coking desulfurization waste water extraction-crystallization coupling.
Evaporative crystallization of the present invention-crystallisation by cooling coupling Crystallization Separation method, has been prepared technical grade sulfuric acid
Sodium and sodium thiosulfate product salt, using the dissolubility difference under sodium sulphate and sodium thiosulfate in water different temperatures, and base
In ternary salt-water system Na2S2O3-Na2SO4-H2The position of the total saturation point indicated in O phasor passes through control extraction waste residue and water
Proportion, evaporative crystallization operation condition and crystallisation by cooling operating condition, so that the purity and receipts of crystalline product be effectively ensured
Rate.
As shown in Fig. 1, the present invention is based on the Na at two temperature of 291.15K and 353.15K2S2O3-Na2SO4-H2O tri-
First phasor has studied optimal crystallization principle, and be applied successfully in conjunction with the concrete composition of coking desulfurization waste water salt extraction extraction filter residue
In the separating-purifying of coking desulfurization waste water salt extraction extraction filter residue, the sodium thiosulfate and sodium sulphate of technical grade are obtained, this is this
The technological innovation of invention.Because being different from being separated only by the purification biggish sodium thiosulfate of content in other documents, the present invention is first
It is that evaporative crystallization separating-purifying obtains the less technical grade sulfuric acid sodium of content, then to obtain content more for crystallisation by cooling separating-purifying
Technical grade sodium thiosulfate.Therefore, separating technology of the invention can not only obtain two kinds of technical grade inorganic salt products, moreover it is possible to maximum
Change ground and handle extraction filter residue to be separated, realize near-zero release and reduces environmental pollution.
It is that separation principle illustrates in the present invention below: gradually adds water, system group to extraction filter residue at 353.15K
At that will be moved along KW, eventually with solubility curve F5G5Point P is met at, filter residue is extracted at this time and is completely dissolved, water and extraction filter residue
Ratio is about 1.0~1.8:1.Being completely dissolved resulting solution and quality is added at 353.15K is extraction filter residue quality 4-7%
Active powdered carbon carries out adsorption bleaching 1-3h.Filtered clarified solution is evaporated crystallization at 353.15K, can be isolated
Anhydrous Na2SO4Product, system composition will be along curve PG5It is mobile, finally reaching total saturation point G5Preceding stopping evaporation,
Na2SO4Theoretical maximum yield be 85.84%.Obtained evaporation mother liquor will be filtered while hot to be diluted with water, system is formed edge
G5W is mobile, and with the G in 291.15K3C meets at point Q, and water addition ratio example is about evaporate mother liquor 20%, at this time at system composition
Na under 291.15K2S2O3Crystal region, after System Solution is cooled to 291.15K from 353.15K, it will obtain Na2S2O3·
5H2O product, theoretical maximum yield are 90.60%.
Current existing sodium thiosulfate preparation method complex process, the reaction time is long, and reaction process is difficult to control, pollutes
Waste is serious, it is difficult to meet the needs of industrialized production.Moreover, the technique of salt extraction at this stage for coking desulfurization waste water is being extracted
A kind of extraction filter residue can be obtained after sodium sulfocyanate out, which mainly contains sodium thiosulfate and sodium sulphate.Due to technique
Limitation, without suitably extract filter residue processing method, stacking can only be concentrated, environmental pollution is not only caused, also caused
The wasting of sodium thiosulfate.Crystallization Separation method of the invention can not only be successfully separated from extraction filter residue and purify out
Technical grade sodium thiosulfate and sodium sulphate product maximumlly prevent pollution of the extraction filter residue to environment, additionally it is possible to provide one
Kind raw material is easy to get and the sodium thiosulfate preparation method of simple process, reduces production cost, alleviates market pressure.Therefore, this hair
Bright Crystallization Separation method solves sodium thiosulfate industrialized production difficulty and coking desulfurization waste water salt extraction extraction filter residue simultaneously
Pollute two problems of environment.Compared to the separating technology for purifying sodium thiosulfate in existing document from extraction filter residue, using this hair
Crystallization Separation method in bright, can obtain 97.6% or more purity, 67.3% or more yield anhydrous sodium sulfate crystal produce
For product as byproduct, average particle size reaches 75.0 μm or more, meets the industry of II class qualified product in national standard GB/T 6009-2014
Quality Grade standard, crystal product form are as shown in Fig. 2；99.2% or more purity, 82.5% or more yield can also be obtained
Five water sodium thiosulfate crystal product, average particle size reaches 785.0 μm or more, meets excellent in national standard HG/T 2328-2006
The industrial level quality standard of equal product, crystal product form are as shown in Fig. 3.
Detailed description of the invention
Crystallization Separation schematic diagram Fig. 1 of the invention；
Fig. 2 anhydrous sodium sulfate crystal product prepared by the present invention；
Fig. 3 five water sodium thiosulfate crystal product prepared by the present invention.
Specific embodiment
Embodiment 1:
100.0g coking desulfurization waste water salt extraction is taken to extract filter residue solid material, wherein sodium thiosulfate quality accounts for gross mass
89%, sodium sulfate quality accounts for the 10% of gross mass, and solid material is added in 130.0g deionized water, under stirring plus
Heat is warming up to 80 DEG C until solid is completely dissolved；5g activity powdered carbon is added into system, filters out insoluble matter after adsorption bleaching 2h
With active powdered carbon；By adsorption bleaching filtrate at 80 DEG C evaporative crystallization, 1.0h is first evaporated with the evaporation rate of 10ml/h, to system
Middle addition anhydrous sodium sulfate crystal seed 0.1g, constant temperature growing the grain 0.5h are then proceeded to be evaporated 4.0h with the evaporation rate of 10ml/h, be steamed altogether
Water yield 50g, constant temperature 0.5h filter obtained sodium sulfate crystal suspension, and it is dry that obtained crystal product is put into 60 DEG C of air blast
Dry 1.0h in dry case, obtained sodium sulfate crystal product purity 97.8%, yield 68%, 76.0 μm of average particle size；It will evaporation
It crystallizes the mother liquor 167g being obtained by filtration to be added in crystallizer, and 30g deionized water is added, and be heated to 80 DEG C.First with 15 DEG C/
The rate of temperature fall of h is cooled to 35 DEG C, and five water sodium thiosulfate 0.05g are added, then constant temperature 1.0h continues to cool down with 5 DEG C/h, when
Constant temperature 1.0h when material reaches 15 DEG C, obtained sodium thiosulfate Crystal suspensions are filtered, and obtained crystal product is put into 30
Dry 1.5h, obtained sodium thiosulfate crystal product purity 99.5%, yield 83%, average particle size in DEG C air dry oven
790μm。
Embodiment 2:
100.0g coking desulfurization waste water salt extraction is taken to extract filter residue solid material, wherein sodium thiosulfate quality accounts for gross mass
90%, sodium sulfate quality accounts for the 9% of gross mass, and solid material is added in 100.0g deionized water, under stirring plus
Heat is warming up to 85 DEG C until solid is completely dissolved；4g activity powdered carbon is added into system, filters out insoluble matter after adsorption bleaching 3h
With active powdered carbon；By adsorption bleaching filtrate at 80 DEG C evaporative crystallization, 1.5h is first evaporated with the evaporation rate of 5ml/h, to system
Middle addition anhydrous sodium sulfate crystal seed 0.1g, constant temperature growing the grain 1.0h are then proceeded to be evaporated 4.0h with the evaporation rate of 10ml/h, be steamed altogether
Water yield 47g, constant temperature 0.8h filter obtained sodium sulfate crystal suspension, and it is dry that obtained crystal product is put into 55 DEG C of air blast
Dry 1.5h in dry case, obtained sodium sulfate crystal product purity 97.6%, yield 67.3%, 75.0 μm of average particle size；It will steam
The mother liquor 175g that hair crystallization is obtained by filtration is added in crystallizer, and 26g deionized water is added, and be heated to 70 DEG C.First with 15
DEG C/rate of temperature fall of h is cooled to 40 DEG C, and five water sodium thiosulfate 0.1g are added, then constant temperature 1.0h continues to drop with 10 DEG C/h
Temperature, the constant temperature 1.0h when material reaches 20 DEG C filter obtained sodium thiosulfate Crystal suspensions, and obtained crystal product is put
Enter and dries 1.5h in 35 DEG C of air dry ovens, obtained sodium thiosulfate crystal product purity 99.2%, yield 82.5%, averagely
785 μm of granularity.
Embodiment 3:
100.0g coking desulfurization waste water salt extraction is taken to extract filter residue solid material, wherein sodium thiosulfate quality accounts for gross mass
85%, sodium sulfate quality accounts for the 14% of gross mass, and solid material is added in 180.0g deionized water, under stirring plus
Heat is warming up to 75 DEG C until solid is completely dissolved；7g activity powdered carbon is added into system, filters out insoluble matter after adsorption bleaching 1h
With active powdered carbon；By adsorption bleaching filtrate at 80 DEG C evaporative crystallization, 0.5h is first evaporated with the evaporation rate of 15ml/h, to system
Middle addition anhydrous sodium sulfate crystal seed 0.1g, constant temperature growing the grain 1.0h are then proceeded to be evaporated 3.0h with the evaporation rate of 15ml/h, be steamed altogether
Water yield 52g, constant temperature 0.5h filter obtained sodium sulfate crystal suspension, and it is dry that obtained crystal product is put into 50 DEG C of air blast
Dry 3.0h in dry case, obtained sodium sulfate crystal product purity 98.2%, yield 67.5%, 77.0 μm of average particle size；It will steam
The mother liquor 160g that hair crystallization is obtained by filtration is added in crystallizer, and 40g deionized water is added, and be heated to 75 DEG C.First with 15
DEG C/rate of temperature fall of h is cooled to 35 DEG C, and five water sodium thiosulfate 0.05g are added, then constant temperature 0.5h continues to drop with 5 DEG C/h
Temperature, the constant temperature 0.5h when material reaches 10 DEG C filter obtained sodium thiosulfate Crystal suspensions, and obtained crystal product is put
Enter dry 1.0h in 35 DEG C of air dry ovens, obtained sodium thiosulfate crystal product purity 99.5%, yield 84%, average grain
803 μm of degree.
Embodiment 4:
100.0g coking desulfurization waste water salt extraction is taken to extract filter residue solid material, wherein sodium thiosulfate quality accounts for gross mass
88%, sodium sulfate quality accounts for the 11% of gross mass, and solid material is added in 150.0g deionized water, under stirring plus
Heat is warming up to 80 DEG C until solid is completely dissolved；5g activity powdered carbon is added into system, filters out insoluble matter after adsorption bleaching 2h
With active powdered carbon；By adsorption bleaching filtrate at 80 DEG C evaporative crystallization, 1.5h is first evaporated with the evaporation rate of 10ml/h, to system
Middle addition anhydrous sodium sulfate crystal seed 0.05g, constant temperature growing the grain 0.8h then proceed to evaporate 4.0h with the evaporation rate of 10ml/h, altogether
Water 55g, constant temperature 0.5h are steamed, obtained sodium sulfate crystal suspension is filtered, obtained crystal product is put into 60 DEG C of air blast
Dry 1.0h in drying box, obtained sodium sulfate crystal product purity 98.5%, yield 68.5%, 78.0 μm of average particle size；It will
The mother liquor 178g that evaporative crystallization is obtained by filtration is added in crystallizer, and 35g deionized water is added, and is heated to 75 DEG C.First with
The rate of temperature fall of 20 DEG C/h is cooled to 35 DEG C, and five water sodium thiosulfate 0.05g are added, then constant temperature 1.0h continues to drop with 6 DEG C/h
Temperature, the constant temperature 1.0h when material reaches 18 DEG C filter obtained sodium thiosulfate Crystal suspensions, and obtained crystal product is put
Enter dry 1.5h in 40 DEG C of air dry ovens, obtained sodium thiosulfate crystal product purity 99.5%, yield 83%, average grain
793 μm of degree.
Embodiment 5:
100.0g coking desulfurization waste water salt extraction is taken to extract filter residue solid material, wherein sodium thiosulfate quality accounts for gross mass
87%, sodium sulfate quality accounts for the 12% of gross mass, and solid material is added in 140.0g deionized water, under stirring plus
Heat is warming up to 75 DEG C until solid is completely dissolved；6g activity powdered carbon is added into system, filters out insoluble matter after adsorption bleaching 2h
With active powdered carbon；By adsorption bleaching filtrate at 80 DEG C evaporative crystallization, 1.5h is first evaporated with the evaporation rate of 10ml/h, to system
Middle addition anhydrous sodium sulfate crystal seed 0.1g, constant temperature growing the grain 0.5h are then proceeded to be evaporated 3.0h with the evaporation rate of 10ml/h, be steamed altogether
Water yield 45g, constant temperature 1.0h filter obtained sodium sulfate crystal suspension, and it is dry that obtained crystal product is put into 60 DEG C of air blast
Dry 1.0h in dry case, obtained sodium sulfate crystal product purity 98.0%, yield 67.5%, 76.4 μm of average particle size；It will steam
The mother liquor 176g that hair crystallization is obtained by filtration is added in crystallizer, and 40g deionized water is added, and be heated to 75 DEG C.First with 15
DEG C/rate of temperature fall of h is cooled to 45 DEG C, and five water sodium thiosulfate 0.1g are added, then constant temperature 1.0h continues to drop with 10 DEG C/h
Temperature, the constant temperature 1.0h when material reaches 15 DEG C filter obtained sodium thiosulfate Crystal suspensions, and obtained crystal product is put
Enter and dries 2.0h in 30 DEG C of air dry ovens, obtained sodium thiosulfate crystal product purity 99.8%, yield 84.3%, averagely
796 μm of granularity.
The Crystallization Separation method for the coking desulfurization waste water salt extraction extraction filter residue that the present invention is disclosed and proposed, those skilled in the art
Member can be by using for reference present disclosure, and the links such as appropriate feed change, technological parameter are realized.Method of the invention has passed through with product
Preferred embodiment is described, related technical personnel obviously can not depart from the content of present invention, in spirit and scope to this
Method described in text and product are modified or appropriate changes and combinations, to realize the technology of the present invention.In particular, it should be pointed out that
All similar replacements and change are apparent to those skilled in the art, they are considered as being included in this hair
In bright spirit, range and content.
Claims (7)
1. a kind of Crystallization Separation method for coking desulfurization waste water salt extraction extraction filter residue；It is characterized in that including the following steps:
1) under stirring action, coking desulfurization waste water salt extraction extraction filter residue is mixed with deionized water, 75~85 DEG C is warming up to, makes to extract
Filter residue is taken to be completely dissolved；
2) quality is then added into system is 4~7% active powdered carbon for extracting filter residue, after 1~3h of system adsorption bleaching
Filtering；
3) by the way of evaporative crystallization, adsorption bleaching filtrate is evaporated at 80 DEG C, obtains the crystal suspension of sodium sulphate, mistake
It is filtered dry dry rear acquisition technical grade sulfuric acid sodium product；
4) the filtered mother liquor of evaporative crystallization is diluted with water, adding water quality is evaporate mother liquor quality 15~25%, feed liquid temperature
Degree is 70~80 DEG C, obtains the crystal suspension of sodium thiosulfate by the way of crystallisation by cooling afterwards, obtains after filtration drying
Technical grade sodium thiosulfate product.
2. the method as described in claim 1, it is characterized in that step 1) deionized water dosage and the extraction of coking desulfurization waste water salt extraction
The mass ratio of filter residue dosage is 1.0~1.8:1.
3. the method as described in claim 1, it is characterized in that in step 3) evaporation and crystal process, first with opposite system gross mass 2
~6% evaporation rate evaporates 0.5~1.5h, is added anhydrous sodium sulfate crystal seed to system, constant temperature 0.5~1h of growing the grain, then after
The continuous evaporation rate with opposite system gross mass 2~6% evaporates 3.0~4.0h, steams water in total and accounts for system gross mass 18%
~25%, 0.5~1h of constant temperature.
4. the method as described in claim 1, it is characterized in that during step 4) crystallisation by cooling, first with the cooling of 15~20 DEG C/h
Material is cooled to 35~45 DEG C by rate, is added five water sodium thiosulfate crystal seeds, constant temperature 0.5~1.0h of growing the grain, then with 5~
Material is cooled to 10~20 DEG C, 0.5~1.0h of constant temperature by the rate of temperature fall of 10 DEG C/h.
5. method as claimed in claim 4, it is characterized in that crystal seed quality is extract filter residue 0.05 in step 3) or step 4)
~0.1%.
6. the method as described in claim 1, it is characterized in that the drying condition of step 4) technical grade sulfuric acid sodium is 50~60 DEG C
Dry 1.0~3.0h in blast drier.
7. the method as described in claim 1, it is characterized in that the drying condition of step 4) technical grade sodium thiosulfate is 30~40
DEG C blast drier in dry 1.0~2.0h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114715855A (en) * | 2022-01-17 | 2022-07-08 | 南方创业（天津）科技发展有限公司 | Method for extracting sodium thiosulfate pentahydrate by using alkaline residue wastewater |
| CN115893695A (en) * | 2021-09-29 | 2023-04-04 | 中国石油化工股份有限公司 | Method for producing sodium thiosulfate by utilizing catalytic cracking flue gas desulfurization wastewater |
Citations (2)
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| CN115893695A (en) * | 2021-09-29 | 2023-04-04 | 中国石油化工股份有限公司 | Method for producing sodium thiosulfate by utilizing catalytic cracking flue gas desulfurization wastewater |
| CN114715855A (en) * | 2022-01-17 | 2022-07-08 | 南方创业（天津）科技发展有限公司 | Method for extracting sodium thiosulfate pentahydrate by using alkaline residue wastewater |
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