CN104140115A - Method and device for recovering anhydrous sodium sulfate from filtrate after purification treatment of desulfurated lead plasters - Google Patents
Method and device for recovering anhydrous sodium sulfate from filtrate after purification treatment of desulfurated lead plasters Download PDFInfo
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- CN104140115A CN104140115A CN201410417932.6A CN201410417932A CN104140115A CN 104140115 A CN104140115 A CN 104140115A CN 201410417932 A CN201410417932 A CN 201410417932A CN 104140115 A CN104140115 A CN 104140115A
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- filtrate
- anhydrous sodium
- sodium sulphate
- lead plaster
- purifying treatment
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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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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
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- Inorganic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method and device for recovering anhydrous sodium sulfate from a filtrate after purification treatment of desulfurated lead plasters. The method comprises the following steps: freezing and crystallizing; removing part of crystal water in vacuum; and drying. The device disclosed by the invention comprises a freezing crystallizer, a low-temperature vacuum drier and drying equipment and directly converts solid sodium sulfate decahydrate into anhydrous sodium sulfate. According to the method and device for recovering anhydrous sodium sulfate from the filtrate after purification treatment of desulfurated lead plasters, the filtrate of the desulfurated lead plasters is prevented from being discharged to the environment to lead to environmental pollution, so that the method and device have the advantages of being low in energy consumption and high in product purity.
Description
Technical field
The invention belongs to resource and reclaim and utilize technique, particularly after a kind of desulfurization lead plaster purifying treatment, filtrate is reclaimed method and the device thereof of anhydrous sodium sulphate, for the technological process from lead-acid accumulator reclaiming lead.
Background technology
Wet desulphurization at present-pyrometallurgical smelting reclaims one of important technology technique plumbous in lead-acid accumulator, to add sodium carbonate in waste lead acid battery lead cream, make lead sulfate change lead carbonate into, reacted desulfurization lead plaster press filtration filtrate is through the method for purification, crystalline sodium sulfate, and then lead carbonate pyrometallurgical smelting reclaims plumbous.Wherein filtrate crystallization being obtained to anhydrous sodium sulphate is an important step in this technique.In addition in industrial production, also there is the waste liquid of many contains sodium sulfate, as the factories such as chemical fibre, agricultural chemicals, White Carbon black all have sodium sulfate waste liquid need to process recovery anhydrous sodium sulphate.Yet the waste liquid of contains sodium sulfate source is different, composition differs greatly, and the processing method that reclaims anhydrous sodium sulphate from waste liquid is also different, such as, for the sodium sulfate waste liquid of some lower concentrations, must adopt the method for evaporating, concentrating and crystallizing to reclaim anhydrous sodium sulphate.Therefore, be necessary to design a kind of Technology that meets filtrate recovery anhydrous sodium sulphate from desulfurization lead plaster purifying treatment.
At present, no matter be filtrate or the method that reclaims anhydrous sodium sulphate from other waste liquid is all the method that adopts heating evaporation crystallization substantially from desulfurization lead plaster purifying treatment.But that the shortcoming of this method maximum is energy consumption is high, very easily fouling in vaporizer of product, scab, the phenomenon that greatly affects vaporization efficiency and cause equipment pipe to stop up.Although by adopting multiple-effect evaporation or flash evaporation technology can effectively reduce energy consumption, in actual production, equipment scaling, the problem that scabs are difficult to solve all the time.If sal glauberi is become to anhydrous sodium sulphate with the crystal water that directly loses of solid-state form, can avoid the problems referred to above.Yet, want the direct heating sal glauberi water that decrystallizes to have very large difficulty, because sal glauberi can the moisture absorption in heat-processed, melt and become liquid.
Sodium sulfate, has another name called Sodium sulfate anhydrous.min(99), is a kind of important Chemicals, 40 ℃ of aqueous sodium persulfate solutions following in water solubleness responsive especially to temperature variation, when lower than 37.2 ℃, with sal glauberi crystalline form, from solution, separate out.And sal glauberi crystal when higher than 40 ℃ rapidly weathering lose crystal water and become anhydrous sodium sulphate, therefore according to the larger practical situation of filtrate sodium sulfate concentration after this characteristic and desulfurization lead plaster purifying treatment, the energy consumption that design filtrate from desulfurization lead plaster purifying treatment is reclaimed anhydrous sodium sulphate is lower, and the simple Technology of maintenance of the equipment is very important.
Summary of the invention
The invention provides filtrate after a kind of desulfurization lead plaster purifying treatment and reclaim method and the device thereof of anhydrous sodium sulphate, avoid adopting that method of evaporating energy consumption is high, sodium sulfate easily fouling in equipment, the defect that scabs, realize and directly by sal glauberi solid state transformation, become anhydrous sodium sulphate.
After desulfurization lead plaster purifying treatment, filtrate is reclaimed a method for anhydrous sodium sulphate, comprises the steps:
(1) freezing and crystallizing: filtrate is reduced to temperature, separate out sal glauberi crystal under slowly stirring, enter whizzer separation;
(2) vacuum-drying: by step (1) gained sal glauberi crystal, be placed in low temperature vacuum drier and vacuumize and be dried to plane of crystal and no longer include crystal gloss, now partial crystallization water is sloughed;
(3) dry: by step (2) gained sal glauberi crystal block section dewatered product, be placed in further drying and dehydrating on dryer and obtain anhydrous sodium sulphate product.
In described step (1), filtrate temperature is reduced to-5～5 ℃.
In described step (2), drying temperature maintains 0～70 ℃, and pressure remains on 0.01～100 mmHg, until sal glauberi crystal weightlessness 20%～70%.
In described step (3), drying temperature maintains 70～300 ℃.
A device that reclaims anhydrous sodium sulphate for filtrate after above-mentioned desulfurization lead plaster purifying treatment, comprises the filtrate tanks, freezing and crystallizing equipment, whizzer, low temperature vacuum drier and the drying plant that by pipeline or conveying belt, connect successively.
After above-mentioned desulfurization lead plaster purifying treatment, filtrate is reclaimed the device of anhydrous sodium sulphate, and described filtrate tanks is with precooling facility; The lower low-concentration sulfuric acid sodium solution of temperature that after freezing and crystallizing, centrifugation goes out is delivered in filtrate tanks precooling facility as heat-eliminating medium through utilidor by vacuum primingpump.
After above-mentioned desulfurization lead plaster purifying treatment, filtrate is reclaimed the device of anhydrous sodium sulphate, and described low temperature vacuum drier is with weight of material display unit, the weightless situation while can be used for monitoring drying material in vacuum in real time.
Beneficial effect of the present invention is:
(1) the present invention adopts the method for cryogenic freezing crystallization to reclaim anhydrous sodium sulphate, and higher, the required energy consumption of gained anhydrous sodium sulphate purity is lower.
(2) the present invention can avoid equipment scaling that heating evaporation brings, problem scabs.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of apparatus of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further details, but the present invention is not limited to this.
As shown in Figure 1, the inventive system comprises the filtrate tanks with precooling facility that connects successively by pipeline or conveying belt, freezing and crystallizing equipment, whizzer, with low temperature vacuum drier and the drying plant of weight of material display unit.
Embodiment 1
The 250 L filtrates of sodium sulfate quality percentage concentration 26 % after desulfurization lead plaster purifying treatment in filtrate tanks, send in freezing and crystallizing equipment and be cooled to 5 ℃, crystallization is sent into centrifugation in whizzer together with mother liquor, the mother liquor of low temperature is delivered in the precooling facility of filtrate tanks as heat-eliminating medium, crystallized product sal glauberi is sent into the low temperature vacuum drier with weight of material display unit, when under the condition of 50 ℃, vacuum-drying to weight is original 50%, this material is sent in drying plant, under the condition of 110 ℃, constant pressure and dry is to constant weight, obtain 50 Kg anhydrous sodium sulphate.
Embodiment 2
The 250 L filtrates of sodium sulfate quality percentage concentration 26 % after desulfurization lead plaster purifying treatment in filtrate tanks, send in freezing and crystallizing equipment and be cooled to-5 ℃, crystallization is sent into centrifugation in whizzer together with mother liquor, the mother liquor of low temperature is delivered in the precooling facility of filtrate tanks as heat-eliminating medium, crystallized product sal glauberi is sent into the low temperature vacuum drier with weight of material display unit, when under the condition of 60 ℃, vacuum-drying to weight is original 60%, this material is sent in drying plant, under the condition of 120 ℃, constant pressure and dry is to constant weight, obtain anhydrous sodium sulphate 55 Kg.
Embodiment 3
The 300 L filtrates of sodium sulfate quality percentage concentration 28 % after desulfurization lead plaster purifying treatment in filtrate tanks, send in freezing and crystallizing equipment 2 and be cooled to-2 ℃, crystallization is sent into centrifugation in whizzer together with mother liquor, the mother liquor of low temperature is delivered in the precooling facility of filtrate tanks as heat-eliminating medium, crystallized product sal glauberi is sent into the low temperature vacuum drier with weight of material display unit, when under the condition of 55 ℃, vacuum-drying to weight is original 40%, this material is sent in drying plant, under the condition of 110 ℃, constant pressure and dry is to constant weight, obtain anhydrous sodium sulphate 65 Kg.
Claims (7)
1. a method for filtrate recovery anhydrous sodium sulphate after desulfurization lead plaster purifying treatment, comprises the steps:
(1) freezing and crystallizing: filtrate is reduced to temperature, separate out sal glauberi crystal under slowly stirring, enter whizzer separation;
(2) vacuum-drying: by step (1) gained sal glauberi crystal, be placed in low temperature vacuum drier and vacuumize and be dried to plane of crystal and no longer include crystal gloss, now partial crystallization water is sloughed;
(3) dry: by step (2) gained sal glauberi crystal block section dewatered product, be placed in further drying and dehydrating on dryer and obtain anhydrous sodium sulphate product.
2. after desulfurization lead plaster purifying treatment according to claim 1, filtrate is reclaimed the method for anhydrous sodium sulphate, and in described step (1), solution temperature is reduced to-5～5 ℃.
3. after desulfurization lead plaster purifying treatment according to claim 1, filtrate is reclaimed the method for anhydrous sodium sulphate, and in described step (2), drying temperature maintains 0～70 ℃, and pressure remains on 0.01～100 mmHg, until sal glauberi crystal weightlessness 20%～70%.
4. after desulfurization lead plaster purifying treatment according to claim 1, filtrate is reclaimed the method for anhydrous sodium sulphate, and in described step (3), drying temperature maintains 70～300 ℃.
5. for filtrate after the desulfurization lead plaster purifying treatment described in claim 1 to 4 any one, reclaim a device for anhydrous sodium sulphate, comprise the filtrate tanks, freezing and crystallizing equipment, whizzer, low temperature vacuum drier and the drying plant that by pipeline or conveying belt, connect successively.
6. after desulfurization lead plaster purifying treatment according to claim 5, filtrate is reclaimed the device of anhydrous sodium sulphate, and described filtrate tanks is with precooling facility; The lower low-concentration sulfuric acid sodium solution of temperature that after freezing and crystallizing, centrifugation goes out is delivered in filtrate tanks precooling facility as heat-eliminating medium through utilidor by vacuum primingpump.
7. after desulfurization lead plaster purifying treatment according to claim 5, filtrate is reclaimed the device of anhydrous sodium sulphate, and described low temperature vacuum drier is with weight of material display unit, the weightless situation during for monitoring drying material in vacuum in real time.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410417932.6A CN104140115A (en) | 2014-08-25 | 2014-08-25 | Method and device for recovering anhydrous sodium sulfate from filtrate after purification treatment of desulfurated lead plasters |
| PCT/CN2014/095969 WO2016029614A1 (en) | 2014-08-25 | 2014-12-31 | Method and apparatus for recovering anhydrous sodium sulfate from filtrate after purification treatment of desulfurated lead plasters |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410417932.6A CN104140115A (en) | 2014-08-25 | 2014-08-25 | Method and device for recovering anhydrous sodium sulfate from filtrate after purification treatment of desulfurated lead plasters |
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| Publication Number | Publication Date |
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| CN104140115A true CN104140115A (en) | 2014-11-12 |
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| CN201410417932.6A Pending CN104140115A (en) | 2014-08-25 | 2014-08-25 | Method and device for recovering anhydrous sodium sulfate from filtrate after purification treatment of desulfurated lead plasters |
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| CN (1) | CN104140115A (en) |
| WO (1) | WO2016029614A1 (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104724730A (en) * | 2015-04-02 | 2015-06-24 | 湘潭大学 | Method and device for crystallizing lead plaster desulphurization by-product sodium sulfate based on localized cooling and rapid crystal precipitation |
| WO2016029614A1 (en) * | 2014-08-25 | 2016-03-03 | 湖南江冶机电科技股份有限公司 | Method and apparatus for recovering anhydrous sodium sulfate from filtrate after purification treatment of desulfurated lead plasters |
| CN106367594A (en) * | 2016-08-25 | 2017-02-01 | 安徽华铂再生资源科技有限公司 | Low-energy-consumption, quick and recyclable lead paste desulfurization mother liquid desalinating process |
| CN107117632A (en) * | 2017-04-28 | 2017-09-01 | 湘潭大学 | A kind of comprehensive utilization process of lead-acid accumulator Waste Sulfuric Acid |
| CN107640778A (en) * | 2017-09-04 | 2018-01-30 | 超威电源有限公司 | A kind of method of the low cost recovery sodium sulphate from leaded desulfurization waste liquor |
| CN108264065A (en) * | 2018-03-16 | 2018-07-10 | 邯郸市同俊达矿山设备股份有限公司 | A kind of hopcalite agent waste water utilization device |
| TWI693097B (en) * | 2017-08-02 | 2020-05-11 | 日商Ｊｘ金屬股份有限公司 | Metal concentration method and metal recovery method |
| CN115445408A (en) * | 2022-09-13 | 2022-12-09 | 北京京诚科林环保科技有限公司 | Resourceful treatment method and system for sodium-based dry desulphurization byproducts of gas boiler |
Families Citing this family (4)
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| CN106946395A (en) * | 2017-05-09 | 2017-07-14 | 北京天地人环保科技有限公司 | A kind of method and device of desulfurization wastewater sub-prime crystallization treatment |
| CN110937611B (en) * | 2019-11-01 | 2023-05-23 | 临涣焦化股份有限公司 | System and method for improving purity of secondary salt of desulfurization waste liquid |
| CN111410354A (en) * | 2020-04-29 | 2020-07-14 | 河南碧云环保工程有限公司 | Recycling system of desulfurization and denitrification waste liquid and method for treating desulfurization and denitrification waste liquid |
| CN112707416A (en) * | 2020-12-30 | 2021-04-27 | 广西天源新能源材料有限公司 | Preparation method of anhydrous sodium sulphate based on lithium polymer |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016029614A1 (en) * | 2014-08-25 | 2016-03-03 | 湖南江冶机电科技股份有限公司 | Method and apparatus for recovering anhydrous sodium sulfate from filtrate after purification treatment of desulfurated lead plasters |
| CN104724730A (en) * | 2015-04-02 | 2015-06-24 | 湘潭大学 | Method and device for crystallizing lead plaster desulphurization by-product sodium sulfate based on localized cooling and rapid crystal precipitation |
| CN106367594A (en) * | 2016-08-25 | 2017-02-01 | 安徽华铂再生资源科技有限公司 | Low-energy-consumption, quick and recyclable lead paste desulfurization mother liquid desalinating process |
| CN107117632A (en) * | 2017-04-28 | 2017-09-01 | 湘潭大学 | A kind of comprehensive utilization process of lead-acid accumulator Waste Sulfuric Acid |
| TWI693097B (en) * | 2017-08-02 | 2020-05-11 | 日商Ｊｘ金屬股份有限公司 | Metal concentration method and metal recovery method |
| TWI779241B (en) * | 2017-08-02 | 2022-10-01 | 日商Ｊｘ金屬股份有限公司 | Sodium removal method |
| CN107640778A (en) * | 2017-09-04 | 2018-01-30 | 超威电源有限公司 | A kind of method of the low cost recovery sodium sulphate from leaded desulfurization waste liquor |
| CN108264065A (en) * | 2018-03-16 | 2018-07-10 | 邯郸市同俊达矿山设备股份有限公司 | A kind of hopcalite agent waste water utilization device |
| CN115445408A (en) * | 2022-09-13 | 2022-12-09 | 北京京诚科林环保科技有限公司 | Resourceful treatment method and system for sodium-based dry desulphurization byproducts of gas boiler |
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| Publication number | Publication date |
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| WO2016029614A1 (en) | 2016-03-03 |
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Application publication date: 20141112 |