CN105293553A - Method for preparing tschermigite by utilizing activated clay production wastewater - Google Patents
Method for preparing tschermigite by utilizing activated clay production wastewater Download PDFInfo
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- CN105293553A CN105293553A CN201510081832.5A CN201510081832A CN105293553A CN 105293553 A CN105293553 A CN 105293553A CN 201510081832 A CN201510081832 A CN 201510081832A CN 105293553 A CN105293553 A CN 105293553A
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Abstract
The invention discloses a method for preparing tschermigite by utilizing activated clay production wastewater, and belongs to the technical field of activated clay wastewater treatment and inorganic salt preparation. The method comprises the following steps: adding aluminum sulfate into the activated clay production wastewater, dissolving the added aluminum sulfate to be saturated with the original aluminum sulfate, conducting reaction with ammonia water, and conducting the steps of purification, crystallization, filter pressing, dehydration and the like to prepare the tschermigite product of which the purity is 99.5% or above. The activated clay wastewater can be effectively treated, aluminum sulfate in the activated clay production wastewater can be fully utilized, and the purposes of saving energy, reducing emission and turning waste into treasure are achieved. Compared with the prior art, aluminum sulfate with lower cost is adopted to replace aluminum hydroxide, so that the production cost is lower; centrifugal dehydration is adopted to replace temperature rising dehydration, so that the production efficiency is higher, and the period is shorter; the process parameters are optimized, so that the purity of tschermigite is higher.
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 to prepare tschermigite.
[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, Tai-Ace S 150, 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.
Tschermigite is mainly used in water purification, the aftertreatment of plating, paper industry, the process of tanning and fur, the production of aluminum oxide and corundum, and printing and dyeing industry is used as mordant, is pharmaceutically used as astringent matter, diuretic(s), emetic and cathartic, foodstuff additive etc.The current main production process of this product obtains Tai-Ace S 150 with vitriolization bauxite, then reacts with ammonium sulfate, then through purification, evaporation, crystallisation by cooling, filtration, drying and obtaining.
Patent " reclaims the method (patent No.: ZL200910185137.8) producing alum " from activated clay production waste, disclose the sulfuric acid utilized in activated clay production waste, Tai-Ace S 150, react with aluminium hydroxide and ammoniacal liquor, filter, evaporate, thick alum, then after purification and impurity removal, dry 7-8 hour purity be more than 99% tschermigite finished product.This invention solves Problems existing in the improvement of activated clay production waste and recoverying and utilizing method, but the method also also exists problems such as preparing tschermigite production efficiency, purity is low, and production cost is high, and the cycle is long.
[summary of the invention]
The problems such as the invention provides a kind of method utilizing activated clay production waste to prepare tschermigite, prepare tschermigite production efficiency to solve activated clay production waste in prior art, purity is low, production cost is high, and the cycle is long.The present invention can effectively process atlapulgite waste water, the Tai-Ace S 150 in activated clay production waste is fully used, the object reach energy-saving and emission-reduction, turning waste into wealth; The present invention is compared with prior art: adopt the Tai-Ace S 150 that price is lower to replace aluminium hydroxide, make production cost lower, adopt centrifuge dehydration to replace intensification and dewater, such that production efficiency is higher, the cycle is shorter, by Optimizing Process Parameters, make the purity of tschermigite higher.
For solving above technical problem, the present invention by the following technical solutions:
Utilize activated clay production waste to prepare a method for tschermigite, 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 ammoniacal liquor to above-mentioned solution, makes NH in solution
4 +: Al
3+: SO
4 2-mol ratio be 1-1.06:1:2-2.06, and pH value is 3.2-3.6, is crossed by solution while hot and filters impurity, gained solution crystallisation by cooling, and then press filtration obtains the thick tschermigite of filter cake;
S2: thick tschermigite is dropped in water, heat and stirs thick tschermigite is dissolved completely after again remove impurity while hot, gained solution again after crystallisation by cooling press filtration obtain filter cake, gained filter cake is put in whizzer and removes moisture, namely obtain pure tschermigite.
Preferably, the described method utilizing activated clay production waste to prepare tschermigite, in step S1, stirring and dissolving Tai-Ace S 150 temperature is 80-85 DEG C.
Preferably, the described method utilizing activated clay production waste to prepare tschermigite, in step S1, the concentration of ammoniacal liquor is 28%-32%.
Preferably, the described method utilizing activated clay production waste to prepare tschermigite, NH in step S1
4 +: Al
3+: SO
4 2-mol ratio be 1-1.03:1:2-2.03.
Preferably, the described method utilizing activated clay production waste to prepare tschermigite, in step S1 and step S2, the temperature of crystallisation by cooling is less than 16 DEG C.
Preferably, the described method utilizing activated clay production waste to prepare tschermigite, the pressure of press filtration in step S1 and step S2 is 0.9-1.0Mpa.
Preferably, the described method utilizing activated clay production waste to prepare tschermigite, drops into the water yield and makes concentration of polymer solution be 56%-60% in step S2.
Preferably, the described method utilizing activated clay production waste to prepare tschermigite, in step S2, the dewatered rotating speed of whizzer is 4000-5000r/min, and the time dewatered is 8-10min.
The present invention has following beneficial effect:
(1) the present invention can effectively process atlapulgite waste water, the Tai-Ace S 150 in activated clay production waste is fully used, the object reach energy-saving and emission-reduction, turning waste into wealth;
(2) the present invention compared with prior art: adopt the Tai-Ace S 150 that price is lower to replace Tai-Ace S 150, make production cost lower, adopt centrifuge dehydration to replace intensification and dewater, such that production efficiency is higher, the cycle is shorter, by Optimizing Process Parameters, make the purity of tschermigite higher.
[accompanying drawing explanation]
Fig. 1 is the process flow sheet utilizing activated clay production waste to prepare tschermigite
[embodiment]
Embodiment 1
Utilize activated clay production waste to prepare a method for tschermigite, 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 to above-mentioned solution the ammoniacal liquor that concentration is 28%, make NH in solution
4 +: Al
3+: SO
4 2-mol ratio be 1:1:2, and pH value is 3.2, is crossed by solution while hot and filters impurity, and it is 16 DEG C of crystallizations that gained solution is cooled to temperature, and then under pressure is 0.9Mpa, press filtration obtains the thick tschermigite of filter cake;
S2: thick tschermigite is dropped in water, the thick tschermigite of heating for dissolving, be configured to the solution that mass concentration is 56%, again remove impurity while hot, it is that after 16 DEG C of crystallizations, under pressure is 0.9Mpa, press filtration obtains filter cake that gained solution is cooled to temperature again, gained filter cake being put into rotating speed is remove moisture in the whizzer of 4000r/min, and the time dewatered is 10min, and namely obtained purity is the tschermigite of 99.6%.
Embodiment 2
Utilize activated clay production waste to prepare a method for tschermigite, 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 to above-mentioned solution the ammoniacal liquor that concentration is 32%, make NH in solution
4 +: Al
3+: SO
4 2-mol ratio be 1.06:1:2.06, and pH value is 3.6, is crossed by solution while hot and filters impurity, and it is 15 DEG C of crystallizations that gained solution is cooled to temperature, and then under pressure is 1.0Mpa, press filtration obtains the thick tschermigite of filter cake;
S2: thick tschermigite is dropped in water, the thick tschermigite of heating for dissolving, be configured to the solution that mass concentration is 60%, again remove impurity while hot, it is that after 15 DEG C of crystallizations, under pressure is 1.0Mpa, press filtration obtains filter cake that gained solution is cooled to temperature again, gained filter cake being put into rotating speed is remove moisture in the whizzer of 5000r/min, and the time dewatered is 8min, and namely obtained purity is the tschermigite of 99.5%.
Embodiment 3
Utilize activated clay production waste to prepare a method for tschermigite, 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 to above-mentioned solution the ammoniacal liquor that concentration is 30%, make NH in solution
4 +: Al
3+: SO
4 2-mol ratio be 1.03:1:1.03, and pH value is 3.4, is crossed by solution while hot and filters impurity, and it is 14 DEG C of crystallizations that gained solution is cooled to temperature, and then under pressure is 0.95Mpa, press filtration obtains the thick tschermigite of filter cake;
S2: thick tschermigite is dropped in water, the thick tschermigite of heating for dissolving, be configured to the solution that mass concentration is 58%, again remove impurity while hot, it is that after 14 DEG C of crystallizations, under pressure is 0.95Mpa, press filtration obtains filter cake that gained solution is cooled to temperature again, gained filter cake being put into rotating speed is remove moisture in the whizzer of 4500r/min, and the time dewatered is 9min, and namely obtained purity is the tschermigite of 99.8%.
Embodiment 4
Utilize activated clay production waste to prepare a method for tschermigite, 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 77 DEG C, adds to above-mentioned solution the ammoniacal liquor that concentration is 29%, make NH in solution
4 +: Al
3+: SO
4 2-mol ratio be 1.01:1:2.01, and pH value is 3.3., is crossed by solution while hot and filters impurity, and it is 13 DEG C of crystallizations that gained solution is cooled to temperature, and then under pressure is 0.9Mpa, press filtration obtains the thick tschermigite of filter cake;
S2: thick tschermigite is dropped in water, the thick tschermigite of heating for dissolving, be configured to the solution that mass concentration is 57%, again remove impurity while hot, it is that after 13 DEG C of crystallizations, under pressure is 0.9Mpa, press filtration obtains filter cake that gained solution is cooled to temperature again, gained filter cake being put into rotating speed is remove moisture in the whizzer of 4000r/min, and the time dewatered is 10min, and namely obtained purity is the tschermigite of 99.6%.
Embodiment 5
Utilize activated clay production waste to prepare a method for tschermigite, 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 to above-mentioned solution the ammoniacal liquor that concentration is 30%, make NH in solution
4 +: Al
3+: SO
4 2-mol ratio be 1.02:1:2.02, and pH value is 3.4, is crossed by solution while hot and filters impurity, and it is 16 DEG C of crystallizations that gained solution is cooled to temperature, and then under pressure is 0.9Mpa, press filtration obtains the thick tschermigite of filter cake;
S2: thick tschermigite is dropped in water, the thick tschermigite of heating for dissolving, be configured to the solution that mass concentration is 56%, again remove impurity while hot, it is that after 16 DEG C of crystallizations, under pressure is 0.9Mpa, press filtration obtains filter cake that gained solution is cooled to temperature again, gained filter cake being put into rotating speed is remove moisture in the whizzer of 5000r/min, and the time dewatered is 8min, and namely obtained purity is the tschermigite of 99.5%.
Embodiment 6
Utilize activated clay production waste to prepare a method for tschermigite, 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 to above-mentioned solution the ammoniacal liquor that concentration is 32%, make NH in solution
4 +: Al
3+: SO
4 2-mol ratio be 1.04:1:2.04, and pH value is 3.2, is crossed by solution while hot and filters impurity, and it is 15 DEG C of crystallizations that gained solution is cooled to temperature, and then under pressure is 1.0Mpa, press filtration obtains the thick tschermigite of filter cake;
S2: thick tschermigite is dropped in water, the thick tschermigite of heating for dissolving, be configured to the solution that mass concentration is 58%, again remove impurity while hot, it is that after 15 DEG C of crystallizations, under pressure is 1.0Mpa, press filtration obtains filter cake that gained solution is cooled to temperature again, gained filter cake being put into rotating speed is remove moisture in the whizzer of 4500r/min, and the time dewatered is 9min, and namely obtained purity is the tschermigite of 99.6%.
Embodiment 7
Utilize activated clay production waste to prepare a method for tschermigite, 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 81 DEG C, adds to above-mentioned solution the ammoniacal liquor that concentration is 32%, make NH in solution
4 +: Al
3+: SO
4 2-mol ratio be 1.05:1:2.06, and pH value is 3.6, is crossed by solution while hot and filters impurity, and it is 16 DEG C of crystallizations that gained solution is cooled to temperature, and then under pressure is 1.0Mpa, press filtration obtains the thick tschermigite of filter cake;
S2: thick tschermigite is dropped in water, the thick tschermigite of heating for dissolving, be configured to the solution that mass concentration is 60%, again remove impurity while hot, it is that after 16 DEG C of crystallizations, under pressure is 1.0Mpa, press filtration obtains filter cake that gained solution is cooled to temperature again, gained filter cake being put into rotating speed is remove moisture in the whizzer of 5000r/min, and the time dewatered is 8min, and namely obtained purity is the tschermigite of 99.6%.
Embodiment 8
Utilize activated clay production waste to prepare a method for tschermigite, 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 to above-mentioned solution the ammoniacal liquor that concentration is 30%, make NH in solution
4 +: Al
3+: SO
4 2-mol ratio be 1.06:1:2.06, and pH value is 3.4, is crossed by solution while hot and filters impurity, and it is 16 DEG C of crystallizations that gained solution is cooled to temperature, and then under pressure is 0.95Mpa, press filtration obtains the thick tschermigite of filter cake;
S2: thick tschermigite is dropped in water, the thick tschermigite of heating for dissolving, be configured to the solution that mass concentration is 60%, again remove impurity while hot, it is that after 16 DEG C of crystallizations, under pressure is 1.0Mpa, press filtration obtains filter cake that gained solution is cooled to temperature again, gained filter cake being put into rotating speed is remove moisture in the whizzer of 5000r/min, and the time dewatered is 8min, and namely obtained purity is the tschermigite of 99.7%.
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 (8)
1. utilize activated clay production waste to prepare a method for tschermigite, 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 ammoniacal liquor to above-mentioned solution, makes NH in solution
4 +: Al
3+: SO
4 2-mol ratio be 1-1.06:1:2-2.06, and pH value is 3.2-3.6, is crossed by solution while hot and filters impurity, gained solution crystallisation by cooling, and then press filtration obtains the thick tschermigite of filter cake;
S2: thick tschermigite is dropped in water, heat and stirs thick tschermigite is dissolved completely after again remove impurity while hot, gained solution again after crystallisation by cooling press filtration obtain filter cake, gained filter cake is put in whizzer and removes moisture, namely obtain pure tschermigite.
2. the method utilizing activated clay production waste to prepare tschermigite according to claim 1, is characterized in that: in step S1, stirring and dissolving Tai-Ace S 150 temperature is 80-85 DEG C.
3. the method utilizing activated clay production waste to prepare tschermigite according to claim 1, is characterized in that: in step S1, the concentration of ammoniacal liquor is 28%-32%.
4. the method utilizing activated clay production waste to prepare tschermigite according to claim 1, is characterized in that: NH in step S1
4 +: Al
3+: SO
4 2-mol ratio be 1-1.03:1:2-2.03.
5. the method utilizing activated clay production waste to prepare tschermigite according to claim 1, is characterized in that: in step S1 and step S2, the temperature of crystallisation by cooling is less than 16 DEG C.
6. the method utilizing activated clay production waste to prepare tschermigite according to claim 1, is characterized in that: the pressure of press filtration in step S1 and step S2 is 0.9-1.0Mpa.
7. the method utilizing activated clay production waste to prepare tschermigite according to claim 1, is characterized in that: drop into the water yield in step S2 and make concentration of polymer solution be 56%-60%.
8. the method utilizing activated clay production waste to prepare tschermigite according to claim 1, it is characterized in that: in step S2, the dewatered rotating speed of whizzer is 4000-5000r/min, the time dewatered is 8-10min.
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Cited By (5)
| 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 |
| CN106986367A (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 soda 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 |
| CN107512731A (en) * | 2017-10-25 | 2017-12-26 | 徐州轩辕铝业有限公司 | A kind of recovery and treatment method of high-purity sulphuric acid aluminium |
| CN111573703A (en) * | 2020-05-29 | 2020-08-25 | 贵州锂电新能源科技有限公司 | Method for preparing ammonium alum by using sulfuric acid method lithium extraction leaching solution |
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| CN103787396A (en) * | 2014-01-27 | 2014-05-14 | 紫金矿业集团股份有限公司 | Method for preparing high-purity potassium alum and aluminum sulfate from alunite ore |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| 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 |
| CN107512731A (en) * | 2017-10-25 | 2017-12-26 | 徐州轩辕铝业有限公司 | A kind of recovery and treatment method of high-purity sulphuric acid aluminium |
| CN111573703A (en) * | 2020-05-29 | 2020-08-25 | 贵州锂电新能源科技有限公司 | Method for preparing ammonium alum by using sulfuric acid method lithium extraction leaching solution |
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Application publication date: 20160203 |