CN105502455A - Method for preparing ammonium alum from acid wastewater of kaolin mineral separation - Google Patents
Method for preparing ammonium alum from acid wastewater of kaolin mineral separation Download PDFInfo
- Publication number
- CN105502455A CN105502455A CN201510937738.5A CN201510937738A CN105502455A CN 105502455 A CN105502455 A CN 105502455A CN 201510937738 A CN201510937738 A CN 201510937738A CN 105502455 A CN105502455 A CN 105502455A
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- China
- Prior art keywords
- tschermigite
- waste water
- ore dressing
- acid waste
- kaolin
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/68—Aluminium compounds containing sulfur
- C01F7/74—Sulfates
- C01F7/76—Double salts, i.e. compounds containing, besides aluminium and sulfate ions, only other cations, e.g. alums
- C01F7/762—Ammonium or alkali metal aluminium sulfates
- C01F7/765—Ammonium aluminium sulfates
-
- C—CHEMISTRY; METALLURGY
- 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
Abstract
The invention discloses a method for preparing ammonium alum from acid wastewater of kaolin mineral separation, and belongs to the technical field of wastewater processing and inorganic salt preparation. Acid wastewater of kaolin mineral separation and kaolin are circulated multiple times so that aluminum sulfate dissolved in acid wastewater and kaolin can reach saturation, aluminum sulfate then reacts with ammonium bisulfate, and ammonium alum with the purity of 99.82% or above is prepared through two times of crystallization. By means of the method, acid wastewater of kaolin mineral separation can be effectively processed, the element aluminum in acid wastewater of kaolin mineral separation is fully utilized, and the aims of saving energy, reducing emission and turning wealth into treasure are achieved.
Description
Technical field
The present invention relates to wastewater treatment and inorganic salt preparing technical field, be specifically related to a kind of method utilizing kaolin ore dressing acid waste water to prepare tschermigite.
Background technology
Chinese kaolin is widely distributed, spreads all over the north and southern region, but Relatively centralized, southern kaolin reserves are more, the ground such as such as Guangdong, Fujian, Jiangxi, Jiangsu.Carrying out producing beneficiation wastewater in kaolin ore dressing process, kaolin ore dressing acid waste water pH value is generally about 3, and the SO containing high density
4 2-, Al
3+.The domestic process to kaolin ore dressing acid waste water is mostly simply add alkali to carry out pH value neutralization, and a lot of little source mill does not even process directly discharges beneficiation wastewater, causes great destruction to environment; Some larger kaolin enterprise, beneficiation wastewater process has been carried out under the pressure of government's pressure, but do not have specialized personnel to go research and design, beneficiation wastewater processing cost is caused to remain high, water after processing can only be discharged, recycle can not be accomplished or to wherein efficient resource recycling, cause water resources and Al
3+deng active substance significant wastage, kaolin ore dressing acid waste water is processed and is recycled Al
3+the document preparing tschermigite is not reported so far.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method utilizing kaolin ore dressing acid waste water to prepare tschermigite, to solve the problem that existing kaolin ore dressing acid waste water processing mode causes aluminium element significant wastage.The present invention effectively can process kaolin ore dressing acid waste water, the aluminium element in kaolin ore dressing acid waste water is fully used, the object reach energy-saving and emission-reduction, turning waste into wealth.
For solving above technical problem, the present invention by the following technical solutions:
Utilize kaolin ore dressing acid waste water to prepare a method for tschermigite, comprise the following steps:
S1: adopt kaolin ore dressing acid waste water to mix with kaolin, kaolinic aluminium sesquioxide is made to be dissolved in kaolin ore dressing acid waste water, again the kaolin ore dressing acid waste water circulation increasing Tai-Ace S 150 concentration is mixed with the kaolin newly increased, with such processing step cyclical operation, until the Tai-Ace S 150 being dissolved in kaolin ore dressing acid waste water reaches capacity;
S2: the kaolin ore dressing acid waste water that the Tai-Ace S 150 obtained by step S1 reaches capacity adds monoammonium sulfate reaction and generates tschermigite after control temperature and pH value;
S3: the tschermigite solution removing impurity that step S2 reaction is generated, gained clear liquid crystallisation by cooling, gained crystallization press filtration obtains the thick tschermigite of filter cake;
S4: thick tschermigite obtained for step S3 is dropped in water, stir after thick tschermigite is dissolved completely and again remove impurity, gained clear liquid crystallisation by cooling again, gained crystallization press filtration obtains tschermigite;
S5: the tschermigite that step S4 is obtained removes moisture further, namely obtained pure tschermigite.
Preferably, in step S1, kaolinic aluminium sesquioxide is dissolved in the temperature of kaolin ore dressing acid waste water is 92-94 DEG C, and the kaolin ore dressing acid waste water circulation increasing Tai-Ace S 150 concentration is 3-4 time with the kaolin mixed cycle operation steps newly increased,
Preferably, the temperature that the kaolin ore dressing acid waste water that in step S2, Tai-Ace S 150 reaches capacity controls is 85-88 DEG C, and pH value is 3.3-3.5.
Preferably, in step S2, when adding monoammonium sulfate, the amount of described monoammonium sulfate is for making NH in tschermigite
4 +: Al
3+: SO
4 2-molar concentration rate be 1.02-1.05:1:2.03-2.08.
Preferably, temperature≤12 DEG C of clear liquid crystallisation by cooling in step S3 and S4.
Preferably, the pressure of press filtration in step S3 and S4 is 0.9-1.0MPa, and tschermigite is depressed into water ratio≤40%.
Preferably, in step S4, amount of water is weight 1.1-1.2 times of thick tschermigite.
Preferably, remove moisture and carry out under whizzer process in step S5, the rotating speed of whizzer is 4000-5000r/min, and tschermigite removing moisture is to water ratio≤0.9%.
The present invention has following beneficial effect:
(1) compared with the tschermigite produced by tschermigite and the prior art of industrial raw material production, production cost of the present invention is lower;
(2) not only purity is high for the tschermigite prepared of the present invention, reaches more than 99.82%, and steady quality;
(3) the present invention can aluminium element in effective recycling kaolin ore dressing acid waste water, and does not increase new element in kaolin ore dressing acid waste water, reaches the object of comprehensive utilization, energy-saving and emission-reduction.
Accompanying drawing explanation
Fig. 1 is that the present invention utilizes kaolin ore dressing acid waste water to prepare the process flow diagram of tschermigite.
Embodiment
Embodiment 1
Utilize kaolin ore dressing acid waste water to prepare a method for tschermigite, comprise the following steps:
S1: adopt kaolin ore dressing acid waste water to mix with kaolin at temperature is 92 DEG C, kaolinic aluminium sesquioxide is made to be dissolved in kaolin ore dressing acid waste water, again the kaolin ore dressing acid waste water circulation increasing Tai-Ace S 150 concentration is mixed with the kaolin newly increased, the Tai-Ace S 150 being dissolved in kaolin ore dressing acid waste water is reached capacity;
S2: the kaolin ore dressing acid waste water that the Tai-Ace S 150 obtained by step S1 reaches capacity is 85 DEG C through control temperature, pH value is add monoammonium sulfate 3.3 times, and the amount of added monoammonium sulfate is for making NH in tschermigite
4 +: Al
3+: SO
4 2-molar concentration rate be 1.02:1:2.03, reaction generate tschermigite;
S3: the tschermigite solution removing impurity that step S2 reaction is generated, gained clear liquid is crystallisation by cooling at temperature is 12 DEG C, and gained crystallization press filtration under pressure is 0.9MPa obtains the thick tschermigite of filter cake that water ratio is 40%;
S4: thick tschermigite obtained for step S3 is dropped in water, institute's amount of water is the weight 1.1 times of thick tschermigite, stir at temperature is 86 DEG C after thick tschermigite is dissolved completely and again remove impurity, gained clear liquid crystallisation by cooling again at temperature is 12 DEG C, gained crystallization press filtration obtains the tschermigite that water ratio is 40%;
S5: the tschermigite obtained by step S4 removes moisture further under the rotating speed of whizzer is 5000r/min is till 0.9% until tschermigite water ratio, namely obtained pure tschermigite.
Embodiment 2
Utilize kaolin ore dressing acid waste water to prepare a method for tschermigite, comprise the following steps:
S1: adopt kaolin ore dressing acid waste water to mix with kaolin at temperature is 94 DEG C, kaolinic aluminium sesquioxide is made to be dissolved in kaolin ore dressing acid waste water, again the kaolin ore dressing acid waste water circulation increasing Tai-Ace S 150 concentration is mixed with the kaolin newly increased, with such processing step cyclical operation 4 times, until the Tai-Ace S 150 being dissolved in kaolin ore dressing acid waste water reaches capacity;
S2: the kaolin ore dressing acid waste water that the Tai-Ace S 150 obtained by step S1 reaches capacity is 88 DEG C through control temperature, pH value is add monoammonium sulfate 3.4 times, and the amount of added monoammonium sulfate is for making NH in tschermigite
4 +: Al
3+: SO
4 2-molar concentration rate be 1.05:1:2.08, reaction generate tschermigite;
S3: the tschermigite solution removing impurity that step S2 reaction is generated, gained clear liquid is crystallisation by cooling at temperature is 10 DEG C, and gained crystallization press filtration under pressure is 1.0MPa obtains the thick tschermigite of filter cake that water ratio is 36%;
S4: thick tschermigite obtained for step S3 is dropped in water, institute's amount of water is the weight 1.2 times of thick tschermigite, stir at temperature is 88 DEG C after thick tschermigite is dissolved completely and again remove impurity, gained clear liquid crystallisation by cooling again at temperature is 10 DEG C, gained crystallization press filtration obtains the tschermigite that water ratio is 35%;
S5: the tschermigite obtained by step S4 removes moisture further under the rotating speed of whizzer is 4000r/min is till 0.8% until tschermigite water ratio, namely obtained pure tschermigite.
Embodiment 3
Utilize kaolin ore dressing acid waste water to prepare a method for tschermigite, comprise the following steps:
S1: adopt kaolin ore dressing acid waste water to mix with kaolin at temperature is 92 DEG C, kaolinic aluminium sesquioxide is made to be dissolved in kaolin ore dressing acid waste water, again the kaolin ore dressing acid waste water circulation increasing Tai-Ace S 150 concentration is mixed with the kaolin newly increased, with such processing step cyclical operation 4 times, until the Tai-Ace S 150 being dissolved in kaolin ore dressing acid waste water reaches capacity;
S2: the kaolin ore dressing acid waste water that the Tai-Ace S 150 obtained by step S1 reaches capacity is 87 DEG C through control temperature, pH value is add monoammonium sulfate 3.5 times, and the amount of added monoammonium sulfate is for making NH in tschermigite
4 +: Al
3+: SO
4 2-molar concentration rate be 1.04:1:2.06, reaction generate tschermigite;
S3: the tschermigite solution removing impurity that step S2 reaction is generated, gained clear liquid is crystallisation by cooling at temperature is 8 DEG C, and gained crystallization press filtration under pressure is 0.9MPa obtains the thick tschermigite of filter cake that water ratio is 30%;
S4: thick tschermigite obtained for step S3 is dropped in water, institute's amount of water is the weight 1.2 times of thick tschermigite, stir at temperature is 87 DEG C after thick tschermigite is dissolved completely and again remove impurity, gained clear liquid crystallisation by cooling again at temperature is 10 DEG C, gained crystallization press filtration obtains the tschermigite that water ratio is 32%;
S5: the tschermigite obtained by step S4 removes moisture further under the rotating speed of whizzer is 4500r/min is till 0.7% until tschermigite water ratio, namely obtained pure tschermigite.
Embodiment 4
Utilize kaolin ore dressing acid waste water to prepare a method for tschermigite, comprise the following steps:
S1: adopt kaolin ore dressing acid waste water to mix with kaolin at temperature is 92 DEG C, kaolinic aluminium sesquioxide is made to be dissolved in kaolin ore dressing acid waste water, again the kaolin ore dressing acid waste water circulation increasing Tai-Ace S 150 concentration is mixed with the kaolin newly increased, with such processing step cyclical operation 4 times, until the Tai-Ace S 150 being dissolved in kaolin ore dressing acid waste water reaches capacity;
S2: the kaolin ore dressing acid waste water that the Tai-Ace S 150 obtained by step S1 reaches capacity is 88 DEG C through control temperature, pH value is add monoammonium sulfate 3.3 times, and the amount of added monoammonium sulfate is for making NH in tschermigite
4 +: Al
3+: SO
4 2-molar concentration rate be 1.03:1:2.05, reaction generate tschermigite;
S3: the tschermigite solution removing impurity that step S2 reaction is generated, gained clear liquid is crystallisation by cooling at temperature is 12 DEG C, and gained crystallization press filtration under pressure is 1.0MPa obtains the thick tschermigite of filter cake that water ratio is 40%;
S4: thick tschermigite obtained for step S3 is dropped in water, institute's amount of water is the weight 1.2 times of thick tschermigite, stir at temperature is 86 DEG C after thick tschermigite is dissolved completely and again remove impurity, gained clear liquid crystallisation by cooling again at temperature is 10 DEG C, gained crystallization press filtration obtains the tschermigite that water ratio is 36%;
S5: the tschermigite obtained by step S4 removes moisture further under the rotating speed of whizzer is 5000r/min is till 0.9% until tschermigite water ratio, namely obtained pure tschermigite.
Embodiment 5
Utilize kaolin ore dressing acid waste water to prepare a method for tschermigite, comprise the following steps:
S1: adopt kaolin ore dressing acid waste water to mix with kaolin at temperature is 92 DEG C, kaolinic aluminium sesquioxide is made to be dissolved in kaolin ore dressing acid waste water, again the kaolin ore dressing acid waste water circulation increasing Tai-Ace S 150 concentration is mixed with the kaolin newly increased, with such processing step cyclical operation 4 times, until the Tai-Ace S 150 being dissolved in kaolin ore dressing acid waste water reaches capacity;
S2: the kaolin ore dressing acid waste water that the Tai-Ace S 150 obtained by step S1 reaches capacity is 89 DEG C through control temperature, pH value is add monoammonium sulfate 3.5 times, and the amount of added monoammonium sulfate is for making NH in tschermigite
4 +: Al
3+: SO
4 2-molar concentration rate be 1.04:1:2.05, reaction generate tschermigite;
S3: the tschermigite solution removing impurity that step S2 reaction is generated, gained clear liquid is crystallisation by cooling at temperature is 10 DEG C, and gained crystallization press filtration under pressure is 0.9MPa obtains the thick tschermigite of filter cake that water ratio is 35%;
S4: thick tschermigite obtained for step S3 is dropped in water, institute's amount of water is the weight 1.1 times of thick tschermigite, stir at temperature is 86 DEG C after thick tschermigite is dissolved completely and again remove impurity, gained clear liquid crystallisation by cooling again at temperature is 12 DEG C, gained crystallization press filtration obtains the tschermigite that water ratio is 30%;
S5: the tschermigite obtained by step S4 removes moisture further under the rotating speed of whizzer is 4000r/min is till 0.8% until tschermigite water ratio, namely obtained pure tschermigite.
Embodiment 6
Utilize kaolin ore dressing acid waste water to prepare a method for tschermigite, comprise the following steps:
S1: adopt kaolin ore dressing acid waste water to mix with kaolin at temperature is 91 DEG C, kaolinic aluminium sesquioxide is made to be dissolved in kaolin ore dressing acid waste water, again the kaolin ore dressing acid waste water circulation increasing Tai-Ace S 150 concentration is mixed with the kaolin newly increased, with such processing step cyclical operation 3 times, until the Tai-Ace S 150 being dissolved in kaolin ore dressing acid waste water reaches capacity;
S2: the kaolin ore dressing acid waste water that the Tai-Ace S 150 obtained by step S1 reaches capacity is 86 DEG C through control temperature, pH value is add monoammonium sulfate 3.5 times, and the amount of added monoammonium sulfate is for making NH in tschermigite
4 +: Al
3+: SO
4 2-molar concentration rate be 1.03:1:2.03, reaction generate tschermigite;
S3: the tschermigite solution removing impurity that step S2 reaction is generated, gained clear liquid is crystallisation by cooling at temperature is 12 DEG C, and gained crystallization press filtration under pressure is 1.0MPa obtains the thick tschermigite of filter cake that water ratio is 40%;
S4: thick tschermigite obtained for step S3 is dropped in water, institute's amount of water is the weight 1.2 times of thick tschermigite, stir at temperature is 88 DEG C after thick tschermigite is dissolved completely and again remove impurity, gained clear liquid crystallisation by cooling again at temperature is 12 DEG C, gained crystallization press filtration obtains the tschermigite that water ratio is 40%;
S5: the tschermigite obtained by step S4 removes moisture further under the rotating speed of whizzer is 5000r/min is till 0.9% until tschermigite water ratio, namely obtained pure tschermigite.
Measure tschermigite purity in embodiment (butt meter), measuring method adopts foodstuff additive tschermigite GB standard to carry out, and analytical results sees the following form.
| Embodiment | Tschermigite purity (%) | Tschermigite purity (%) | Tschermigite purity (%) | Tschermigite purity (%) | Tschermigite purity (%) | Tschermigite purity (%) |
| 1 | 99.82 | |||||
| 2 | 99.86 | |||||
| 3 | 99.88 | |||||
| 4 | 99.9 | |||||
| 5 | 99.89 | |||||
| 6 | 99.85 |
As seen from the above table, the tschermigite purity (butt meter) that the present invention utilizes kaolin ore dressing acid waste water to prepare the method gained of tschermigite reaches more than 99.82%, and the tschermigite that visible the present invention obtains not only purity is high and stable.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to the scope of patent protection that the present invention is determined by submitted to claims.
Claims (8)
1. utilize kaolin ore dressing acid waste water to prepare a method for tschermigite, it is characterized in that: comprise the following steps:
S1: adopt kaolin ore dressing acid waste water to mix with kaolin, kaolinic aluminium sesquioxide is made to be dissolved in kaolin ore dressing acid waste water, again the kaolin ore dressing acid waste water circulation increasing Tai-Ace S 150 concentration is mixed with the kaolin newly increased, with such processing step cyclical operation, until the Tai-Ace S 150 being dissolved in kaolin ore dressing acid waste water reaches capacity;
S2: the kaolin ore dressing acid waste water that the Tai-Ace S 150 obtained by step S1 reaches capacity adds monoammonium sulfate reaction and generates tschermigite after control temperature and pH value;
S3: the tschermigite solution removing impurity that step S2 reaction is generated, gained clear liquid crystallisation by cooling, gained crystallization press filtration obtains the thick tschermigite of filter cake;
S4: thick tschermigite obtained for step S3 is dropped in water, stir after thick tschermigite is dissolved completely and again remove impurity, gained clear liquid crystallisation by cooling again, gained crystallization press filtration obtains tschermigite;
S5: the tschermigite that step S4 is obtained removes moisture further, namely obtained pure tschermigite.
2. the method utilizing kaolin ore dressing acid waste water to prepare tschermigite according to claim 1, it is characterized in that, in step S1, kaolinic aluminium sesquioxide is dissolved in the temperature of kaolin ore dressing acid waste water is 92-94 DEG C, and the kaolin ore dressing acid waste water circulation increasing Tai-Ace S 150 concentration is 3-4 time with the kaolin mixed cycle operation steps newly increased.
3. the method utilizing kaolin ore dressing acid waste water to prepare tschermigite according to claim 1, is characterized in that, the temperature that the kaolin ore dressing acid waste water that in step S2, Tai-Ace S 150 reaches capacity controls is 85-88 DEG C, and pH value is 3.3-3.5.
4. the method utilizing kaolin ore dressing acid waste water to prepare tschermigite according to claim 1, is characterized in that, in step S2, when adding monoammonium sulfate, the amount of described monoammonium sulfate is for making NH in tschermigite
4 +: Al
3+: SO
4 2-molar concentration rate be 1.02-1.05:1:2.03-2.08.
5. the method utilizing kaolin ore dressing acid waste water to prepare tschermigite according to claim 1, is characterized in that, temperature≤12 DEG C of clear liquid crystallisation by cooling in step S3 and S4.
6. the method utilizing kaolin ore dressing acid waste water to prepare tschermigite according to claim 1, it is characterized in that, the pressure of press filtration in step S3 and S4 is 0.9-1.0MPa, and tschermigite is depressed into water ratio≤40%.
7. the method utilizing kaolin ore dressing acid waste water to prepare tschermigite according to claim 1, is characterized in that, in step S4, amount of water is weight 1.1-1.2 times of thick tschermigite.
8. the method utilizing kaolin ore dressing acid waste water to prepare tschermigite according to claim 1, it is characterized in that, remove moisture in step S5 to carry out under whizzer process, the rotating speed of whizzer is 4000-5000r/min, and tschermigite removing moisture is to water ratio≤0.9%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510937738.5A CN105502455B (en) | 2015-12-16 | 2015-12-16 | A kind of method that utilization kaolin ore dressing acid waste water prepares ammonia-alum |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510937738.5A CN105502455B (en) | 2015-12-16 | 2015-12-16 | A kind of method that utilization kaolin ore dressing acid waste water prepares ammonia-alum |
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| Publication Number | Publication Date |
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| CN105502455A true CN105502455A (en) | 2016-04-20 |
| CN105502455B CN105502455B (en) | 2017-06-06 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1515494A (en) * | 2003-01-03 | 2004-07-28 | 王如声 | Production method of crystal alum |
| 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 |
| CN102815737A (en) * | 2012-08-14 | 2012-12-12 | 衡阳市建衡实业有限公司 | New method for producing potassium alum |
-
2015
- 2015-12-16 CN CN201510937738.5A patent/CN105502455B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1515494A (en) * | 2003-01-03 | 2004-07-28 | 王如声 | Production method of crystal alum |
| 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 |
| CN102815737A (en) * | 2012-08-14 | 2012-12-12 | 衡阳市建衡实业有限公司 | New method for producing potassium alum |
Non-Patent Citations (2)
| Title |
|---|
| 李斌: ""铝铵矾的合成与精制"", 《四川化工》 * |
| 赵锡武等: ""利用高岭土生产无机化工产品"", 《化工科技市场》 * |
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