CN105399123A - Method for preparing sodium alum by using kaolin mineral processing wastewater - Google Patents
Method for preparing sodium alum by using kaolin mineral processing wastewater Download PDFInfo
- Publication number
- CN105399123A CN105399123A CN201510936939.3A CN201510936939A CN105399123A CN 105399123 A CN105399123 A CN 105399123A CN 201510936939 A CN201510936939 A CN 201510936939A CN 105399123 A CN105399123 A CN 105399123A
- Authority
- CN
- China
- Prior art keywords
- sodium alum
- kaolin
- water
- waster water
- sodium
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Classifications
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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
-
- 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
- C01P2006/82—Compositional purity water content
Abstract
The invention discloses a method for preparing sodium alum by using kaolin mineral processing wastewater, and belongs to the technical fields of wastewater treatment and inorganic salt preparation. The kaolin mineral processing wastewater and kaolin are mixed circularly for multiple times, aluminum sulfate dissolved in the wastewater is allowed to reach saturation, then the wastewater is subjected to a reaction with sodium sulfate, crystallization is carried out for two times to obtain the sodium alum with the purity reaching 99.84% or more. The method can effectively treat the kaolin mineral processing wastewater, so that aluminum elements in the kaolin mineral processing wastewater are fully utilized, and the purposes of saving energy, reducing emission, and turning waste to 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 processing waster water to prepare sodium alum.
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 processing waster water pH value is generally about 3, and the SO containing high density
4 2-, Al
3+.The domestic process to kaolin processing waster 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 processing waster water is processed and is recycled Al
3+the document preparing sodium alum 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 processing waster water to prepare sodium alum, to solve the problem that existing kaolin processing waster water processing mode causes aluminium element significant wastage.The present invention effectively can process kaolin processing waster water, the aluminium element in kaolin processing waster 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 processing waster water to prepare a method for sodium alum, comprise the following steps:
S1: adopt kaolin processing waster water to mix with kaolin, kaolinic aluminium sesquioxide is made to be dissolved in kaolin processing waster water, again the kaolin processing waster 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 processing waster water reaches capacity;
S2: the kaolin processing waster water that the Tai-Ace S 150 obtained by step S1 reaches capacity adds sodium sulfate reaction and generates sodium alum after control temperature and pH value;
S3: the sodium alum solution removing impurity that step S2 reaction is generated, gained clear liquid crystallisation by cooling, gained crystallization press filtration obtains the thick sodium alum of filter cake;
S4: thick sodium alum obtained for step S3 is dropped in water, stir after thick sodium alum is dissolved completely and again remove impurity, gained clear liquid crystallisation by cooling again, gained crystallization press filtration obtains sodium alum;
S5: the sodium alum that step S4 is obtained removes moisture further, namely obtained pure sodium alum.
Preferably, in step S1, kaolinic aluminium sesquioxide is dissolved in the temperature of kaolin processing waster water is 92-94 DEG C, and the kaolin processing waster water circulation increasing Tai-Ace S 150 concentration is 3-5 time with the kaolin mixed cycle operation steps newly increased,
Preferably, the temperature that the kaolin processing waster 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 sodium sulfate, the amount of described sodium sulfate is for making Na in sodium alum
+: Al
3+: SO
4 2-molar concentration rate be 1.02-1.04:1:2.03-2.06.
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 sodium alum is depressed into water ratio≤40%.
Preferably, in step S4, amount of water is weight 1.1-1.3 times of thick sodium alum.
Preferably, remove moisture and carry out under whizzer process in step S5, the rotating speed of whizzer is 4000-5000r/min, and sodium alum removing moisture is to water ratio≤0.9%.
The present invention has following beneficial effect:
(1) compared with the sodium alum produced by sodium alum 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 sodium alum prepared of the present invention, reaches more than 99.84%, and steady quality;
(3) the present invention can aluminium element in effective recycling kaolin processing waster water, and does not increase new element in kaolin processing waster water, reaches the object of comprehensive utilization, energy-saving and emission-reduction.
Accompanying drawing explanation
Fig. 1 is that the present invention utilizes kaolin processing waster water to prepare the process flow diagram of sodium alum.
Embodiment
Embodiment 1
Utilize kaolin processing waster water to prepare a method for sodium alum, comprise the following steps:
S1: adopt kaolin processing waster water to mix with kaolin at temperature is 92 DEG C, kaolinic aluminium sesquioxide is made to be dissolved in kaolin processing waster water, again the kaolin processing waster water circulation increasing Tai-Ace S 150 concentration is mixed with the kaolin newly increased, the Tai-Ace S 150 being dissolved in kaolin processing waster water is reached capacity;
S2: the kaolin processing waster water that the Tai-Ace S 150 obtained by step S1 reaches capacity is 85 DEG C through control temperature, pH value is add sodium sulfate 3.3 times, and the amount of added sodium sulfate is for making Na in sodium alum
+: Al
3+: SO
4 2-molar concentration rate be 1.02:1:2.03, reaction generate sodium alum;
S3: the sodium alum 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 sodium alum of filter cake that water ratio is 40%;
S4: thick sodium alum obtained for step S3 is dropped in water, institute's amount of water is the weight 1.1 times of thick sodium alum, stir at temperature is 86 DEG C after thick sodium alum 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 sodium alum that water ratio is 40%;
S5: the sodium alum obtained by step S4 removes moisture further under the rotating speed of whizzer is 5000r/min is till 0.9% until sodium alum water ratio, namely obtained pure sodium alum.
Embodiment 2
Utilize kaolin processing waster water to prepare a method for sodium alum, comprise the following steps:
S1: adopt kaolin processing waster water to mix with kaolin at temperature is 94 DEG C, kaolinic aluminium sesquioxide is made to be dissolved in kaolin processing waster water, again the kaolin processing waster water circulation increasing Tai-Ace S 150 concentration is mixed with the kaolin newly increased, with such processing step cyclical operation 5 times, until the Tai-Ace S 150 being dissolved in kaolin processing waster water reaches capacity;
S2: the kaolin processing waster water that the Tai-Ace S 150 obtained by step S1 reaches capacity is 88 DEG C through control temperature, pH value is add sodium sulfate 3.4 times, and the amount of added sodium sulfate is for making Na in sodium alum
+: Al
3+: SO
4 2-molar concentration rate be 1.02:1:2.02, reaction generate sodium alum;
S3: the sodium alum 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 sodium alum of filter cake that water ratio is 36%;
S4: thick sodium alum obtained for step S3 is dropped in water, institute's amount of water is the weight 1.3 times of thick sodium alum, stir at temperature is 88 DEG C after thick sodium alum 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 sodium alum that water ratio is 35%;
S5: the sodium alum obtained by step S4 removes moisture further under the rotating speed of whizzer is 4000r/min is till 0.8% until sodium alum water ratio, namely obtained pure sodium alum.
Embodiment 3
Utilize kaolin processing waster water to prepare a method for sodium alum, comprise the following steps:
S1: adopt kaolin processing waster water to mix with kaolin at temperature is 92 DEG C, kaolinic aluminium sesquioxide is made to be dissolved in kaolin processing waster water, again the kaolin processing waster water circulation increasing Tai-Ace S 150 concentration is mixed with the kaolin newly increased, with such processing step cyclical operation 5 times, until the Tai-Ace S 150 being dissolved in kaolin processing waster water reaches capacity;
S2: the kaolin processing waster water that the Tai-Ace S 150 obtained by step S1 reaches capacity is 87 DEG C through control temperature, pH value is add sodium sulfate 3.5 times, and the amount of added sodium sulfate is for making Na in sodium alum
+: Al
3+: SO
4 2-molar concentration rate be 1.04:1:2.06, reaction generate sodium alum;
S3: the sodium alum 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 sodium alum of filter cake that water ratio is 30%;
S4: thick sodium alum obtained for step S3 is dropped in water, institute's amount of water is the weight 1.2 times of thick sodium alum, stir at temperature is 87 DEG C after thick sodium alum 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 sodium alum that water ratio is 32%;
S5: the sodium alum obtained by step S4 removes moisture further under the rotating speed of whizzer is 4500r/min is till 0.7% until sodium alum water ratio, namely obtained pure sodium alum.
Embodiment 4
Utilize kaolin processing waster water to prepare a method for sodium alum, comprise the following steps:
S1: adopt kaolin processing waster water to mix with kaolin at temperature is 92 DEG C, kaolinic aluminium sesquioxide is made to be dissolved in kaolin processing waster water, again the kaolin processing waster 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 processing waster water reaches capacity;
S2: the kaolin processing waster water that the Tai-Ace S 150 obtained by step S1 reaches capacity is 88 DEG C through control temperature, pH value is add sodium sulfate 3.3 times, and the amount of added sodium sulfate is for making Na in sodium alum
+: Al
3+: SO
4 2-molar concentration rate be 1.03:1:2.05, reaction generate sodium alum;
S3: the sodium alum 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 .0MPa obtains the thick sodium alum of filter cake that water ratio is 40%;
S4: thick sodium alum obtained for step S3 is dropped in water, institute's amount of water is the weight 1.3 times of thick sodium alum, stir at temperature is 86 DEG C after thick sodium alum 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 sodium alum that water ratio is 36%;
S5: the sodium alum obtained by step S4 removes moisture further under the rotating speed of whizzer is 5000r/min is till 0.9% until sodium alum water ratio, namely obtained pure sodium alum.
Embodiment 5
Utilize kaolin processing waster water to prepare a method for sodium alum, comprise the following steps:
S1: adopt kaolin processing waster water to mix with kaolin at temperature is 92 DEG C, kaolinic aluminium sesquioxide is made to be dissolved in kaolin processing waster water, again the kaolin processing waster 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 processing waster water reaches capacity;
S2: the kaolin processing waster water that the Tai-Ace S 150 obtained by step S1 reaches capacity is 89 DEG C through control temperature, pH value is add sodium sulfate 3.5 times, and the amount of added sodium sulfate is for making Na in sodium alum
+: Al
3+: SO
4 2-molar concentration rate be 1.04:1:2.05, reaction generate sodium alum;
S3: the sodium alum 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 sodium alum of filter cake that water ratio is 35%;
S4: thick sodium alum obtained for step S3 is dropped in water, institute's amount of water is the weight 1.3 times of thick sodium alum, stir at temperature is 86 DEG C after thick sodium alum 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 sodium alum that water ratio is 30%;
S5: the sodium alum obtained by step S4 removes moisture further under the rotating speed of whizzer is 4000r/min is till 0.8% until sodium alum water ratio, namely obtained pure sodium alum.
Embodiment 6
Utilize kaolin processing waster water to prepare a method for sodium alum, comprise the following steps:
S1: adopt kaolin processing waster water to mix with kaolin at temperature is 91 DEG C, kaolinic aluminium sesquioxide is made to be dissolved in kaolin processing waster water, again the kaolin processing waster water circulation increasing Tai-Ace S 150 concentration is mixed with the kaolin newly increased, with such processing step cyclical operation 5 times, until the Tai-Ace S 150 being dissolved in kaolin processing waster water reaches capacity;
S2: the kaolin processing waster water that the Tai-Ace S 150 obtained by step S1 reaches capacity is 86 DEG C through control temperature, pH value is add sodium sulfate 3.5 times, and the amount of added sodium sulfate is for making Na in sodium alum
+: Al
3+: SO
4 2-molar concentration rate be 1.03:1:2.03, reaction generate sodium alum;
S3: the sodium alum 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 sodium alum of filter cake that water ratio is 40%;
S4: thick sodium alum obtained for step S3 is dropped in water, institute's amount of water is the weight 1.2 times of thick sodium alum, stir at temperature is 88 DEG C after thick sodium alum 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 sodium alum that water ratio is 40%;
S5: the sodium alum obtained by step S4 removes moisture further under the rotating speed of whizzer is 5000r/min is till 0.9% until sodium alum water ratio, namely obtained pure sodium alum.
Measure sodium alum purity in embodiment (butt meter), measuring method adopts foodstuff additive sodium alum GB standard to carry out, and analytical results sees the following form.
| Embodiment | Sodium alum purity (%) | Sodium alum purity (%) | Sodium alum purity (%) | Sodium alum purity (%) | Sodium alum purity (%) | Sodium alum purity (%) |
| 1 | 99.88 | |||||
| 2 | 99.84 | |||||
| 3 | 99.92 | |||||
| 4 | 99.87 | |||||
| 5 | 99.9 | |||||
| 6 | 99.89 |
As seen from the above table, the sodium alum purity (butt meter) that the present invention utilizes kaolin processing waster water to prepare the method gained of sodium alum reaches more than 99.84%, and the sodium alum 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 processing waster water to prepare a method for sodium alum, it is characterized in that: comprise the following steps:
S1: adopt kaolin processing waster water to mix with kaolin, kaolinic aluminium sesquioxide is made to be dissolved in kaolin processing waster water, again the kaolin processing waster 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 processing waster water reaches capacity;
S2: the kaolin processing waster water that the Tai-Ace S 150 obtained by step S1 reaches capacity adds sodium sulfate reaction and generates sodium alum after control temperature and pH value;
S3: the sodium alum solution removing impurity that step S2 reaction is generated, gained clear liquid crystallisation by cooling, gained crystallization press filtration obtains the thick sodium alum of filter cake;
S4: thick sodium alum obtained for step S3 is dropped in water, stir after thick sodium alum is dissolved completely and again remove impurity, gained clear liquid crystallisation by cooling again, gained crystallization press filtration obtains sodium alum;
S5: the sodium alum that step S4 is obtained removes moisture further, namely obtained pure sodium alum.
2. the method utilizing kaolin processing waster water to prepare sodium alum according to claim 1, it is characterized in that, in step S1, kaolinic aluminium sesquioxide is dissolved in the temperature of kaolin processing waster water is 92-94 DEG C, and the kaolin processing waster water circulation increasing Tai-Ace S 150 concentration is 3-5 time with the kaolin mixed cycle operation steps newly increased.
3. the method utilizing kaolin processing waster water to prepare sodium alum according to claim 1, is characterized in that, the temperature that the kaolin processing waster 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 processing waster water to prepare sodium alum according to claim 1, is characterized in that, in step S2, when adding sodium sulfate, the amount of described sodium sulfate is for making Na in sodium alum
+: Al
3+: SO
4 2-molar concentration rate be 1.02-1.04:1:2.03-2.06.
5. the method utilizing kaolin processing waster water to prepare sodium alum 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 processing waster water to prepare sodium alum according to claim 1, is characterized in that, the pressure of press filtration in step S3 and S4 is 0.9-1.0MPa, and sodium alum is depressed into water ratio≤40%.
7. the method utilizing kaolin processing waster water to prepare sodium alum according to claim 1, is characterized in that, in step S4, amount of water is weight 1.1-1.3 times of thick sodium alum.
8. the method utilizing kaolin processing waster water to prepare sodium alum 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 sodium alum removing moisture is to water ratio≤0.9%.
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| CN201510936939.3A CN105399123A (en) | 2015-12-16 | 2015-12-16 | Method for preparing sodium alum by using kaolin mineral processing wastewater |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1037363A (en) * | 1988-05-07 | 1989-11-22 | 山西师范大学 | The method of comprehensive utilization of low-grade aluminium ore |
| 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 |
| CN103073126A (en) * | 2013-01-24 | 2013-05-01 | 中国高岭土有限公司 | Treatment method of kaolin mineral processing waste water |
| CN105129830A (en) * | 2015-02-15 | 2015-12-09 | 广西隆安瑞丰工贸有限公司 | Method for preparation of potassium alum from activated clay production mother liquor |
-
2015
- 2015-12-16 CN CN201510936939.3A patent/CN105399123A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1037363A (en) * | 1988-05-07 | 1989-11-22 | 山西师范大学 | The method of comprehensive utilization of low-grade aluminium ore |
| 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 |
| CN103073126A (en) * | 2013-01-24 | 2013-05-01 | 中国高岭土有限公司 | Treatment method of kaolin mineral processing waste water |
| CN105129830A (en) * | 2015-02-15 | 2015-12-09 | 广西隆安瑞丰工贸有限公司 | Method for preparation of potassium alum from activated clay production mother liquor |
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Application publication date: 20160316 |