CN105314782A - Method for cooperatively producing sodium alum and gypsum through activated clay industrial wastewater - Google Patents
Method for cooperatively producing sodium alum and gypsum through activated clay industrial wastewater Download PDFInfo
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- CN105314782A CN105314782A CN201510081788.8A CN201510081788A CN105314782A CN 105314782 A CN105314782 A CN 105314782A CN 201510081788 A CN201510081788 A CN 201510081788A CN 105314782 A CN105314782 A CN 105314782A
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Abstract
The invention discloses a method for cooperatively producing sodium alum and gypsum through activated clay industrial wastewater, and belongs to the technical field of activated clay wastewater treatment and inorganic salt preparation. The method comprises the steps that aluminum sulfate in the activated clay industrial wastewater is mixed with newly-added aluminum sulfate and sodium hydroxide, impurity removal, crystallization, filter pressing, water removal and the other steps are performed on the mixture to obtain a sodium alum product with the purity of 99.5% or above, and the left-over filtrate is neutralized through lime to obtain the gypsum. The activated clay wastewater can be effectively treated, the aluminum sulfate in the wastewater can be recycled, and the obtained gypsum meets the requirement for industrial application. The sodium alum prepared by the adoption of the technology is high in yield, production efficiency and purity, low in cost, short in period and easy to apply and popularize.
Description
[technical field]
The present invention relates to wastewater treatment and inorganic salt preparation field, be specifically related to a kind of method utilizing activated clay production waste coproduction sodium alum, gypsum.
[background technology]
Atlapulgite is mainly used in the decolorizing and refining of mineral oil, vegetables oil and animal grease, is a kind of important petrochemical complex and daily-use chemical industry raw material.Atlapulgite take wilkinite as raw material, and the main wet process acid metallization processes that adopts processes.Its production process comprises: wilkinite aquation, add sulfuric acid activated, washing, dry, pulverize.Because its product acid content is large, need acid content just can be made to be less than 0.2% through repeatedly washing, to reach the requirement of HG/T2569-94 product standard.Different according to method, the wastewater flow rate that water washing process produces has different, but the wastewater flow rate producing the generation of 1t atlapulgite is generally no less than 30-40t.Tai-Ace S 150 mainly containing the generation of wilkinite acidification reaction in this waste water and unreacted sulfuric acid etc., if directly discharge, not only waste a large amount of resources, and can cause serious pollution to environment.
In recent years, for activated clay production waste improvement and recycle and propose certain methods, as limestone vegetation method, carbide slag neutralisation, return acid activation method, and decompose china clay with process industry water conditioner Tai-Ace S 150 with it, dissolve iron filings and manufacture green vitriol etc.These methods, the governing problem solving activated clay production waste preferably had, as limestone vegetation method can make the acidity in waste water be neutralized by adding lime, make sulfate ion, aluminum ion and iron ion etc. form the precipitations such as calcium sulfate, aluminium hydroxide, ironic hydroxide and remove, but these throw outs are become new solid waste because not utilizing; The recycling problem solving resource in activated clay production waste preferably had, be exactly utilize the sulfuric acid in waste water to decompose china clay as decomposed china clay with it with the method for process industry water conditioner Tai-Ace S 150, aluminium in china clay is leached solution, Tai-Ace S 150 is obtained again through purification and impurity removal, evaporative crystallization, separation drying, crushing packing, although this method efficiently utilizes the resource such as sulfuric acid, Tai-Ace S 150 in activated clay production waste, but because the impurity such as iron ion can affect the quality of product Tai-Ace S 150, thus must be removed through purification and impurity removal process.Normal employing activated manganese dioxide method deironing at present, needs expensive manganese salt, causes processing cost higher.
There is the useful components such as a large amount of Tai-Ace S 150, ferric sulfate in activated clay production waste, how while effective process waste water, recycle these useful components, become the direction of our research.
[summary of the invention]
The invention provides a kind of method utilizing activated clay production waste coproduction sodium alum, gypsum, with solve activated clay production waste administer and Tai-Ace S 150, ferric sulfate recycle problem.The present invention can effectively process atlapulgite waste water, and both realized Tai-Ace S 150 in waste water and be recycled utilization, the gypsum also realizing obtaining reaches the requirement of industrial application; Adopt technique of the present invention to prepare sodium alum, the output of acquisition, production efficiency, purity are high, and cost is low, and the cycle is short, are easy to apply.
For solving above technical problem, the present invention by the following technical solutions:
Utilize a method for activated clay production waste coproduction sodium alum, gypsum, it is characterized in that: comprise the following steps:
S1: add Tai-Ace S 150 to activated clay production waste, stirring and dissolving Tai-Ace S 150 at temperature is 75-85 DEG C, adds sodium hydroxide to above-mentioned solution, makes Al in solution
3+: Na
+: SO
4 2-mol ratio be 1:1-1.06:2-2.06, adjust ph is 3.2-3.8, while hot solution is crossed and filter impurity, be 1.4-1.48g/mL by filtrate heating evaporation moisture to solution density, filter after solution crystallisation by cooling, obtain the thick sodium alum of filter cake, thick sodium alum is dropped in water, at being heated to 75-85 DEG C, dissolves thick sodium alum, then filter after solution crystallisation by cooling and obtain filter cake, gained filter cake is put in whizzer and removes moisture, be i.e. the sodium alum of obtained purity>=99.5%;
S2: collect all remaining filtrate in step S1, adds lime reaction and generates ironic hydroxide in filtrate, and it is after 7 that filtrate is neutralized to pH value, gained solution through Filter Press, namely obtains gypsum filter cake.
Preferably, the described method utilizing activated clay production waste coproduction sodium alum, gypsum, in step S1, the temperature of stirring and dissolving Tai-Ace S 150 is 80-85 DEG C.
Preferably, the described method utilizing activated clay production waste coproduction sodium alum, gypsum, Al in step S1
3+: Na
+: SO
4 2-mol ratio be 1:1-1.03:2-2.03.
Preferably, the described method utilizing activated clay production waste coproduction sodium alum, gypsum, adjust ph described in step S1 adopts sodium bicarbonate to regulate.
Preferably, the described method utilizing activated clay production waste coproduction sodium alum, gypsum, the temperature of the crystallisation by cooling of solution described in step S1 is less than 18 DEG C.
Preferably, the described method utilizing activated clay production waste coproduction sodium alum, gypsum, the mass concentration dropped in water after heating for dissolving by thick sodium alum in step S1 is 52%-60%.
Preferably, the described method utilizing activated clay production waste coproduction sodium alum, gypsum, in step S1, the dewatered rotating speed of whizzer is 3000-4000r/min, and the time dewatered is 10-15min.
Preferably, the described method utilizing activated clay production waste coproduction sodium alum, gypsum, step S2 also comprises: the method removing moisture obtained gypsum filter cake being adopted airing under the sun.
Preferably, the described method utilizing activated clay production waste coproduction sodium alum, gypsum, gained gypsum filter cake removing moisture is to water content≤10%.
Preferably, the described method utilizing activated clay production waste coproduction sodium alum, gypsum, gypsum obtained in step S2 uses as cement setting retarder.
The present invention has following beneficial effect:
(1) the present invention can solve activated clay production waste administer and Tai-Ace S 150, ferric sulfate recycle problem, both realized Tai-Ace S 150 in waste water to be recycled utilization and to prepare sodium alum, also the recycling realizing ferric sulfate obtains gypsum, and reach the requirement of industrial application, can increase economic efficiency;
(2) adopt technique of the present invention to prepare sodium alum, the output of acquisition, production efficiency, purity are high, and cost is low, and the cycle is short, are easy to apply.
[accompanying drawing explanation]
Fig. 1 is the process flow sheet utilizing activated clay production waste coproduction sodium alum, gypsum
[embodiment]
Embodiment 1
Utilize a method for activated clay production waste coproduction sodium alum, gypsum, comprise the following steps:
S1: add Tai-Ace S 150 to activated clay production waste, stirring and dissolving Tai-Ace S 150 at temperature is 75 DEG C, adds sodium hydroxide to above-mentioned solution, makes Al in solution
3+: Na
+: SO
4 2-mol ratio be 1:1:2, adding sodium bicarbonate adjust ph is 3.2, while hot solution is crossed and filter impurity, be 1.4g/mL by filtrate heating evaporation moisture to solution density, it is 18 DEG C of crystallization and filtration that solution is cooled to temperature, obtain the thick sodium alum of filter cake, thick sodium alum is dropped in water, thick sodium alum is dissolved at being heated to 75 DEG C, be mixed with the solution that mass concentration is 52%, then solution is cooled to temperature is that 18 DEG C of crystallization and filtration obtain filter cake, gained filter cake being put into rotating speed is remove moisture in 3000r/min whizzer, the time dewatered is 15min, namely obtained purity is the sodium alum of 99.5%.
S2: collect all remaining filtrate in step S1, in filtrate, add lime reaction generate ironic hydroxide, it is after 7 that filtrate is neutralized to pH value, gained solution through Filter Press, i.e. obtained gypsum filter cake, then method removing moisture to water content gained gypsum filter cake being adopted airing under the sun is 10%, and obtained gypsum uses as cement setting retarder.
Embodiment 2
Utilize a method for activated clay production waste coproduction sodium alum, gypsum, comprise the following steps:
S1: add Tai-Ace S 150 to activated clay production waste, stirring and dissolving Tai-Ace S 150 at temperature is 85 DEG C, adds sodium hydroxide to above-mentioned solution, makes Al in solution
3+: Na
+: SO
4 2-mol ratio be 1:1.06:2.06, adding sodium bicarbonate adjust ph is 3.8, while hot solution is crossed and filter impurity, be 1.48g/mL by filtrate heating evaporation moisture to solution density, it is 16 DEG C of crystallization and filtration that solution is cooled to temperature, obtain the thick sodium alum of filter cake, thick sodium alum is dropped in water, thick sodium alum is dissolved at being heated to 85 DEG C, be mixed with the solution that mass concentration is 60%, then solution is cooled to temperature is that 16 DEG C of crystallization and filtration obtain filter cake, gained filter cake being put into rotating speed is remove moisture in 4000r/min whizzer, the time dewatered is 10min, namely obtained purity is the sodium alum of 99.6%,
S2: collect all remaining filtrate in step S1, in filtrate, add lime reaction generate ironic hydroxide, it is after 7 that filtrate is neutralized to pH value, gained solution through Filter Press, i.e. obtained gypsum filter cake, then method removing moisture to water content gained gypsum filter cake being adopted airing under the sun is 8%, and obtained gypsum uses as cement setting retarder.
Embodiment 3
Utilize a method for activated clay production waste coproduction sodium alum, gypsum, comprise the following steps:
S1: add Tai-Ace S 150 to activated clay production waste, stirring and dissolving Tai-Ace S 150 at temperature is 80 DEG C, adds sodium hydroxide to above-mentioned solution, makes Al in solution
3+: Na
+: SO
4 2-mol ratio be 1:1.03:2.03, adding sodium bicarbonate adjust ph is 3.5, while hot solution is crossed and filter impurity, be 1.44g/mL by filtrate heating evaporation moisture to solution density, it is 15 DEG C of crystallization and filtration that solution is cooled to temperature, obtain the thick sodium alum of filter cake, thick sodium alum is dropped in water, thick sodium alum is dissolved at being heated to 80 DEG C, be mixed with the solution that mass concentration is 56%, then solution is cooled to temperature is that 15 DEG C of crystallization and filtration obtain filter cake, gained filter cake being put into rotating speed is remove moisture in 3500r/min whizzer, the time dewatered is 13min, namely obtained purity is the sodium alum of 99.8%,
S2: collect all remaining filtrate in step S1, in filtrate, add lime reaction generate ironic hydroxide, it is after 7 that filtrate is neutralized to pH value, gained solution through Filter Press, i.e. obtained gypsum filter cake, then method removing moisture to water content gained gypsum filter cake being adopted airing under the sun is 6%, and obtained gypsum uses as cement setting retarder.
Embodiment 4
Utilize a method for activated clay production waste coproduction sodium alum, gypsum, comprise the following steps:
S1: add Tai-Ace S 150 to activated clay production waste, stirring and dissolving Tai-Ace S 150 at temperature is 82 DEG C, adds sodium hydroxide to above-mentioned solution, makes Al in solution
3+: Na
+: SO
4 2-mol ratio be 1:1.02:2.02, adding sodium bicarbonate adjust ph is 3.3, while hot solution is crossed and filter impurity, be 1.42g/mL by filtrate heating evaporation moisture to solution density, it is 18 DEG C of crystallization and filtration that solution is cooled to temperature, obtain the thick sodium alum of filter cake, thick sodium alum is dropped in water, thick sodium alum is dissolved at being heated to 82 DEG C, be mixed with the solution that mass concentration is 54%, then solution is cooled to temperature is that 18 DEG C of crystallization and filtration obtain filter cake, gained filter cake being put into rotating speed is remove moisture in 4000r/min whizzer, the time dewatered is 10min, namely obtained purity is the sodium alum of 99.6%,
S2: collect all remaining filtrate in step S1, in filtrate, add lime reaction generate ironic hydroxide, it is after 7 that filtrate is neutralized to pH value, gained solution through Filter Press, i.e. obtained gypsum filter cake, then method removing moisture to water content gained gypsum filter cake being adopted airing under the sun is 10%, and obtained gypsum uses as cement setting retarder.
Embodiment 5
Utilize a method for activated clay production waste coproduction sodium alum, gypsum, comprise the following steps:
S1: add Tai-Ace S 150 to activated clay production waste, stirring and dissolving Tai-Ace S 150 at temperature is 78 DEG C, adds sodium hydroxide to above-mentioned solution, makes Al in solution
3+: Na
+: SO
4 2-mol ratio be 1:1.03:2.04, adding sodium bicarbonate adjust ph is 3.4, while hot solution is crossed and filter impurity, be 1.45g/mL by filtrate heating evaporation moisture to solution density, it is 16 DEG C of crystallization and filtration that solution is cooled to temperature, obtain the thick sodium alum of filter cake, thick sodium alum is dropped in water, thick sodium alum is dissolved at being heated to 78 DEG C, be mixed with the solution that mass concentration is 55%, then solution is cooled to temperature is that 16 DEG C of crystallization and filtration obtain filter cake, gained filter cake being put into rotating speed is remove moisture in 4000r/min whizzer, the time dewatered is 10min, namely obtained purity is the sodium alum of 99.7%,
S2: collect all remaining filtrate in step S1, in filtrate, add lime reaction generate ironic hydroxide, it is after 7 that filtrate is neutralized to pH value, gained solution through Filter Press, i.e. obtained gypsum filter cake, then method removing moisture to water content gained gypsum filter cake being adopted airing under the sun is 8%, and obtained gypsum uses as cement setting retarder.
Embodiment 6
Utilize a method for activated clay production waste coproduction sodium alum, gypsum, comprise the following steps:
S1: add Tai-Ace S 150 to activated clay production waste, stirring and dissolving Tai-Ace S 150 at temperature is 83 DEG C, adds sodium hydroxide to above-mentioned solution, makes Al in solution
3+: Na
+: SO
4 2-mol ratio be 1:1.04:2.05, adding sodium bicarbonate adjust ph is 3.5, while hot solution is crossed and filter impurity, be 1.46g/mL by filtrate heating evaporation moisture to solution density, it is 18 DEG C of crystallization and filtration that solution is cooled to temperature, obtain the thick sodium alum of filter cake, thick sodium alum is dropped in water, thick sodium alum is dissolved at being heated to 83 DEG C, be mixed with the solution that mass concentration is 54%, then solution is cooled to temperature is that 18 DEG C of crystallization and filtration obtain filter cake, gained filter cake being put into rotating speed is remove moisture in 3000r/min whizzer, the time dewatered is 15min, namely obtained purity is the sodium alum of 99.6%,
S2: collect all remaining filtrate in step S1, in filtrate, add lime reaction generate ironic hydroxide, it is after 7 that filtrate is neutralized to pH value, gained solution through Filter Press, i.e. obtained gypsum filter cake, then method removing moisture to water content gained gypsum filter cake being adopted airing under the sun is 8%, and obtained gypsum uses as cement setting retarder.
In embodiment, sodium alum purity check the results are shown in following table.
As seen from the above table, the present invention utilizes the sodium alum purity of the method gained of activated clay production waste coproduction sodium alum, gypsum to reach more than 99.5%, and not only purity is high and stable for the sodium alum that this technique is obtained as seen.
The foregoing is only embodiments of the invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. utilize a method for activated clay production waste coproduction sodium alum, gypsum, it is characterized in that: comprise the following steps:
S1: add Tai-Ace S 150 to activated clay production waste, stirring and dissolving Tai-Ace S 150 at temperature is 75-85 DEG C, adds sodium hydroxide to above-mentioned solution, makes Al in solution
3+: Na
+: SO
4 2-mol ratio be 1:1-1.06:2-2.06, adjust ph is 3.2-3.8, while hot solution is crossed and filter impurity, be 1.4-1.48g/mL by filtrate heating evaporation moisture to solution density, filter after solution crystallisation by cooling, obtain the thick sodium alum of filter cake, thick sodium alum is dropped in water, at being heated to 75-85 DEG C, dissolves thick sodium alum, then filter after solution crystallisation by cooling and obtain filter cake, gained filter cake is put in whizzer and removes moisture, be i.e. the sodium alum of obtained purity>=99.5%;
S2: collect all remaining filtrate in step S1, adds lime reaction and generates ironic hydroxide in filtrate, and it is after 7 that filtrate is neutralized to pH value, gained solution through Filter Press, namely obtains gypsum filter cake.
2. utilize the method for activated clay production waste coproduction sodium alum, gypsum according to claim 1, it is characterized in that: in step S1, the temperature of stirring and dissolving Tai-Ace S 150 is 80-85 DEG C.
3. utilize the method for activated clay production waste coproduction sodium alum, gypsum according to claim 1, it is characterized in that: Al in step S1
3+: Na
+: SO
4 2-mol ratio be 1:1-1.03:2-2.03.
4. utilize the method for activated clay production waste coproduction sodium alum, gypsum according to claim 1, it is characterized in that: adjust ph described in step S1 adopts sodium bicarbonate to regulate.
5. utilize the method for activated clay production waste coproduction sodium alum, gypsum according to claim 1, it is characterized in that: the temperature of the crystallisation by cooling of solution described in step S1 is less than 18 DEG C.
6. utilize the method for activated clay production waste coproduction sodium alum, gypsum according to claim 1, it is characterized in that: the mass concentration dropped in water after heating for dissolving by thick sodium alum in step S1 is 52%-60%.
7. utilize the method for activated clay production waste coproduction sodium alum, gypsum according to claim 1, it is characterized in that: in step S1, the dewatered rotating speed of whizzer is 3000-4000r/min, the time dewatered is 10-15min.
8. utilize the method for activated clay production waste coproduction sodium alum, gypsum according to claim 1, it is characterized in that: described step S2 also comprises: the method removing moisture obtained gypsum filter cake being adopted airing under the sun.
9. utilize the method for activated clay production waste coproduction sodium alum, gypsum according to claim 8, it is characterized in that: gained gypsum filter cake removing moisture is to water content≤10%.
10. utilize the method for activated clay production waste coproduction sodium alum, gypsum according to claim 1, it is characterized in that: gypsum obtained in step S2 uses as cement setting retarder.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106986366A (en) * | 2017-04-13 | 2017-07-28 | 广西隆安瑞丰工贸有限公司 | A kind of method that atlapulgite spent acid mother liquor prepares ammonia-alum |
| CN106986365A (en) * | 2017-04-13 | 2017-07-28 | 广西隆安瑞丰工贸有限公司 | A kind of method that atlapulgite spent acid mother liquor prepares potassium alum |
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| CN101671048A (en) * | 2009-09-30 | 2010-03-17 | 合肥工业大学 | Method for recovering and preparing alum from activated clay production waste liquid |
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2015
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101671048A (en) * | 2009-09-30 | 2010-03-17 | 合肥工业大学 | Method for recovering and preparing alum from activated clay production waste liquid |
Non-Patent Citations (1)
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| 吴杰: "膨润土制备活性白土及废液后处理研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106986366A (en) * | 2017-04-13 | 2017-07-28 | 广西隆安瑞丰工贸有限公司 | A kind of method that atlapulgite spent acid mother liquor prepares ammonia-alum |
| CN106986365A (en) * | 2017-04-13 | 2017-07-28 | 广西隆安瑞丰工贸有限公司 | A kind of method that atlapulgite spent acid mother liquor prepares potassium alum |
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