CN105271341A - Method for preparing potassium alum by utilization of activated clay production waste water - Google Patents
Method for preparing potassium alum by utilization of activated clay production waste water Download PDFInfo
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- CN105271341A CN105271341A CN201510081845.2A CN201510081845A CN105271341A CN 105271341 A CN105271341 A CN 105271341A CN 201510081845 A CN201510081845 A CN 201510081845A CN 105271341 A CN105271341 A CN 105271341A
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- potassium alum
- activated clay
- production waste
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- clay production
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Abstract
The invention discloses a method for preparing potassium alum by utilization of activated clay production waste water, and belongs to the activated clay waste water processing and inorganic salt preparation technology fields. Sulfuric acid and aluminum sulfate in activated clay production waste water are reacted with aluminum hydroxide and potassium sulfate, and a potassium alum product with a purity of more than 99.5% is prepared after steps of impurity removal, crystallization, press filtration, dewatering and the like. Activated clay waste water can be processed effectively, sulfuric acid and aluminum sulfate in activated clay production waste water can be utilized fully, and purposes of energy saving, emission reduction and changing waste into valuables are achieved. When the method is compared with the prior art, potassium sulfate with a lower price is employed to replace potassium hydroxide, and the production cost is low. centrifuge dewatering is employed to replace heating dewatering, the production efficiency is high, and the cycle is short. Through technology optimization, the purity of potassium alum is high.
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 potassium alum.
[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.
Potassium alum is mainly used as the hardening agent of film and sensitive paper, water purification settling agent, medical astringent matter and hemostatic agent, printing and dyeing mordant, saleratus raw material, papermaking cementing agent, and tanning agent, produces the raw material of high purity aluminium oxide and other aluminium salt, rubber pange agent, foodstuff additive etc.The current main production process of this product obtains Tai-Ace S 150 with vitriolization bauxite, then reacts with potassium 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 potassium hydroxide, filter, evaporate, thick alum, then after purification and impurity removal, dry 7-8 hour purity is the potassium alum finished product of 99%-99.4%.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 potassium alum 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 potassium alum, prepare potassium alum 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, makes the sulfuric acid in activated clay production waste, Tai-Ace S 150 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 potassium sulfate that price is lower to replace potassium hydroxide, make production cost lower, adopts centrifuge dehydration to replace intensification and dewaters, such that production efficiency is higher, the cycle is shorter, by process optimization, makes the purity of potassium alum higher.
For solving above technical problem, the present invention by the following technical solutions:
Utilize activated clay production waste to prepare a method for potassium alum, comprise the following steps:
S1: add aluminium hydroxide to activated clay production waste, stirring and dissolving aluminium hydroxide at temperature is 80-90 DEG C, adds potassium sulfate to above-mentioned solution, makes K in solution
+: Al
3+: SO
4 2-mol ratio be 1-1.08:1:2-2.08, adding potassium hydroxide solution adjust ph 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 potassium alum of filter cake;
S2: thick potassium alum is dropped in water, heat and stirs thick potassium alum 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 potassium alum.
Preferably, the described method utilizing activated clay production waste to prepare potassium alum, in step S1, stirring and dissolving aluminium hydroxide temperature is 85-90 DEG C.
Preferably, the described method utilizing activated clay production waste to prepare potassium alum, K in step S1
+: Al
3+: SO
4 2-mol ratio be 1-1.04:1:2-2.04.
Preferably, the described method utilizing activated clay production waste to prepare potassium alum, in step S1 and step S2, the temperature of crystallisation by cooling is less than 15 DEG C.
Preferably, the described method utilizing activated clay production waste to prepare potassium alum, 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 potassium alum, drops into the water yield and makes concentration of polymer solution be 54%-60% in step S2.
Preferably, the described method utilizing activated clay production waste to prepare potassium alum, 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, makes the sulfuric acid in activated clay production waste, Tai-Ace S 150 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 potassium sulfate that price is lower to replace potassium hydroxide, make production cost lower, adopt centrifuge dehydration to replace intensification and dewater, such that production efficiency is higher, the cycle is shorter, by process optimization, make the purity of potassium alum higher.
[accompanying drawing explanation]
Fig. 1 is the process flow sheet utilizing activated clay production waste to prepare potassium alum.
[embodiment]
Embodiment 1
Utilize activated clay production waste to prepare a method for potassium alum, comprise the following steps:
S1: add aluminium hydroxide to activated clay production waste, stirring and dissolving aluminium hydroxide at temperature is 80 DEG C, adds potassium sulfate to above-mentioned solution, makes K in solution
+: Al
3+: SO
4 2-mol ratio be 1:1:2, adding potassium hydroxide solution adjust ph is 3.2, is crossed by solution while hot and filters impurity, and gained solution cooling temperature is 15 DEG C of crystallizations, and then under pressure is 0.9Mpa, press filtration obtains the thick potassium alum of filter cake;
S2: thick potassium alum is dropped in water, heat and stir thick potassium alum is dissolved completely after make concentration of polymer solution be 54%, again remove impurity while hot, gained solution again cooling temperature is after 15 DEG C of crystallizations, under pressure is 0.9Mpa, press filtration obtains filter cake, gained filter cake being put into rotating speed is remove moisture in 4000r/min whizzer, and the time dewatered is 10min, and namely obtained purity is the potassium alum of 99.6%.
Embodiment 2
Utilize activated clay production waste to prepare a method for potassium alum, comprise the following steps:
S1: add aluminium hydroxide to activated clay production waste, stirring and dissolving aluminium hydroxide at temperature is 90 DEG C, adds potassium sulfate to above-mentioned solution, makes K in solution
+: Al
3+: SO
4 2-mol ratio be 1.08:1:2.08, adding potassium hydroxide solution adjust ph is 3.6, is crossed by solution while hot and filters impurity, and gained solution cooling temperature is 13 DEG C of crystallizations, and then under pressure is 1.0Mpa, press filtration obtains the thick potassium alum of filter cake;
S2: thick potassium alum is dropped in water, heat and stir thick potassium alum is dissolved completely after make concentration of polymer solution be 60%, again remove impurity while hot, gained solution again cooling temperature is after 13 DEG C of crystallizations, under pressure is 0.9Mpa, press filtration obtains filter cake, gained filter cake being put into rotating speed is remove moisture in 5000r/min whizzer, and the time dewatered is 8min, and namely obtained purity is the potassium alum of 99.5%.
Embodiment 3
Utilize activated clay production waste to prepare a method for potassium alum, comprise the following steps:
S1: add aluminium hydroxide to activated clay production waste, stirring and dissolving aluminium hydroxide at temperature is 85 DEG C, adds potassium sulfate to above-mentioned solution, makes K in solution
+: Al
3+: SO
4 2-mol ratio be 1.04:1:2.04, adding potassium hydroxide solution adjust ph is 3.4, is crossed by solution while hot and filters impurity, and gained solution cooling temperature is 12 DEG C of crystallizations, and then under pressure is 0.95Mpa, press filtration obtains the thick potassium alum of filter cake;
S2: thick potassium alum is dropped in water, heat and stir thick potassium alum is dissolved completely after make concentration of polymer solution be 57%, again remove impurity while hot, gained solution again cooling temperature is after 12 DEG C of crystallizations, under pressure is 0.9Mpa, press filtration obtains filter cake, gained filter cake being put into rotating speed is remove moisture in 4500r/min whizzer, and the time dewatered is 9min, and namely obtained purity is the potassium alum of 99.8%.
Embodiment 4
Utilize activated clay production waste to prepare a method for potassium alum, comprise the following steps:
S1: add aluminium hydroxide to activated clay production waste, stirring and dissolving aluminium hydroxide at temperature is 82 DEG C, adds potassium sulfate to above-mentioned solution, makes K in solution
+: Al
3+: SO
4 2-mol ratio be 1.01:1:2.01, adding potassium hydroxide solution adjust ph is 3.2, is crossed by solution while hot and filters impurity, and gained solution cooling temperature is 10 DEG C of crystallizations, and then under pressure is 0.9Mpa, press filtration obtains the thick potassium alum of filter cake;
S2: thick potassium alum is dropped in water, heat and stir thick potassium alum is dissolved completely after make concentration of polymer solution be 55%, again remove impurity while hot, gained solution again cooling temperature is after 10 DEG C of crystallizations, under pressure is 0.9Mpa, press filtration obtains filter cake, gained filter cake being put into rotating speed is remove moisture in 4000r/min whizzer, and the time dewatered is 10min, and namely obtained purity is the potassium alum of 99.5%.
Embodiment 5
Utilize activated clay production waste to prepare a method for potassium alum, comprise the following steps:
S1: add aluminium hydroxide to activated clay production waste, stirring and dissolving aluminium hydroxide at temperature is 83 DEG C, adds potassium sulfate to above-mentioned solution, makes K in solution
+: Al
3+: SO
4 2-mol ratio be 1.02:1:2.02, adding potassium hydroxide solution adjust ph is 3.3, is crossed by solution while hot and filters impurity, and gained solution cooling temperature is 12 DEG C of crystallizations, and then under pressure is 0.92Mpa, press filtration obtains the thick potassium alum of filter cake;
S2: thick potassium alum is dropped in water, heat and stir thick potassium alum is dissolved completely after make concentration of polymer solution be 56%, again remove impurity while hot, gained solution again cooling temperature is after 12 DEG C of crystallizations, under pressure is 0.9Mpa, press filtration obtains filter cake, gained filter cake being put into rotating speed is remove moisture in 5000r/min whizzer, and the time dewatered is 8min, and namely obtained purity is the potassium alum of 99.6%.
Embodiment 6
Utilize activated clay production waste to prepare a method for potassium alum, comprise the following steps:
S1: add aluminium hydroxide to activated clay production waste, stirring and dissolving aluminium hydroxide at temperature is 84 DEG C, adds potassium sulfate to above-mentioned solution, makes K in solution
+: Al
3+: SO
4 2-mol ratio be 1.05:1:2.06, adding potassium hydroxide solution adjust ph is 3.5, is crossed by solution while hot and filters impurity, and gained solution cooling temperature is 15 DEG C of crystallizations, and then under pressure is 1.0Mpa, press filtration obtains the thick potassium alum of filter cake;
S2: thick potassium alum is dropped in water, heat and stir thick potassium alum is dissolved completely after make concentration of polymer solution be 60%, again remove impurity while hot, gained solution again cooling temperature is after 15 DEG C of crystallizations, under pressure is 0.9Mpa, press filtration obtains filter cake, gained filter cake being put into rotating speed is remove moisture in 5000r/min whizzer, and the time dewatered is 8min, and namely obtained purity is the potassium alum of 99.7%.
Embodiment 7
Utilize activated clay production waste to prepare a method for potassium alum, comprise the following steps:
S1: add aluminium hydroxide to activated clay production waste, stirring and dissolving aluminium hydroxide at temperature is 86 DEG C, adds potassium sulfate to above-mentioned solution, makes K in solution
+: Al
3+: SO
4 2-mol ratio be 1.06:1:2.07, adding potassium hydroxide solution adjust ph is 3.6, is crossed by solution while hot and filters impurity, and gained solution cooling temperature is 11 DEG C of crystallizations, and then under pressure is 0.94Mpa, press filtration obtains the thick potassium alum of filter cake;
S2: thick potassium alum is dropped in water, heat and stir thick potassium alum is dissolved completely after make concentration of polymer solution be 57%, again remove impurity while hot, gained solution again cooling temperature is after 11 DEG C of crystallizations, under pressure is 0.9Mpa, press filtration obtains filter cake, gained filter cake being put into rotating speed is remove moisture in 4500r/min whizzer, and the time dewatered is 9min, and namely obtained purity is the potassium alum of 99.6%.
Embodiment 8
Utilize activated clay production waste to prepare a method for potassium alum, comprise the following steps:
S1: add aluminium hydroxide to activated clay production waste, stirring and dissolving aluminium hydroxide at temperature is 88 DEG C, adds potassium sulfate to above-mentioned solution, makes K in solution
+: Al
3+: SO
4 2-mol ratio be 1.08:1:2.07, adding potassium hydroxide solution adjust ph is 3.6, is crossed by solution while hot and filters impurity, and gained solution cooling temperature is 10 DEG C of crystallizations, and then under pressure is 1.0Mpa, press filtration obtains the thick potassium alum of filter cake;
S2: thick potassium alum is dropped in water, heat and stir thick potassium alum is dissolved completely after make concentration of polymer solution be 58%, again remove impurity while hot, gained solution again cooling temperature is after 10 DEG C of crystallizations, under pressure is 0.9Mpa, press filtration obtains filter cake, gained filter cake being put into rotating speed is remove moisture in 5000r/min whizzer, and the time dewatered is 8min, and namely obtained purity is the potassium alum of 99.6%.
Embodiment 9
Utilize activated clay production waste to prepare a method for potassium alum, comprise the following steps:
S1: add aluminium hydroxide to activated clay production waste, stirring and dissolving aluminium hydroxide at temperature is 89 DEG C, adds potassium sulfate to above-mentioned solution, makes K in solution
+: Al
3+: SO
4 2-mol ratio be 1.07:1:2.08, adding potassium hydroxide solution adjust ph is 3.4, is crossed by solution while hot and filters impurity, and gained solution cooling temperature is 12 DEG C of crystallizations, and then under pressure is 0.95Mpa, press filtration obtains the thick potassium alum of filter cake;
S2: thick potassium alum is dropped in water, heat and stir thick potassium alum is dissolved completely after make concentration of polymer solution be 56%, again remove impurity while hot, gained solution again cooling temperature is after 12 DEG C of crystallizations, under pressure is 0.9Mpa, press filtration obtains filter cake, gained filter cake being put into rotating speed is remove moisture in 4500r/min whizzer, and the time dewatered is 9min, and namely obtained purity is the potassium alum 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 (7)
1. utilize activated clay production waste to prepare a method for potassium alum, it is characterized in that: comprise the following steps:
S1: add aluminium hydroxide to activated clay production waste, stirring and dissolving aluminium hydroxide at temperature is 80-90 DEG C, adds potassium sulfate to above-mentioned solution, makes K in solution
+: Al
3+: SO
4 2-mol ratio be 1-1.08:1:2-2.08, adding potassium hydroxide solution adjust ph 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 potassium alum of filter cake;
S2: thick potassium alum is dropped in water, heat and stirs thick potassium alum 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 potassium alum.
2. the method utilizing activated clay production waste to prepare potassium alum according to claim 1, is characterized in that: in step S1, stirring and dissolving aluminium hydroxide temperature is 85-90 DEG C.
3. the method utilizing activated clay production waste to prepare potassium alum according to claim 1, is characterized in that: K in step S1
+: Al
3+: SO
4 2-mol ratio be 1-1.04:1:2-2.04.
4. the method utilizing activated clay production waste to prepare potassium alum according to claim 1, is characterized in that: in step S1 and step S2, the temperature of crystallisation by cooling is less than 15 DEG C.
5. the method utilizing activated clay production waste to prepare potassium alum according to claim 1, is characterized in that: the pressure of press filtration in step S1 and step S2 is 0.9-1.0Mpa.
6. the method utilizing activated clay production waste to prepare potassium alum according to claim 1, is characterized in that: drop into the water yield in step S2 and make concentration of polymer solution be 54%-60%.
7. the method utilizing activated clay production waste to prepare potassium alum 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 (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106277010A (en) * | 2016-08-24 | 2017-01-04 | 淄博市淄川程鹏化工厂 | A kind of Alumen production technology |
| 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 |
| CN106986364A (en) * | 2017-04-13 | 2017-07-28 | 广西隆安瑞丰工贸有限公司 | A kind of activated clay production waste coproduction alum, the method for gypsum |
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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 |
| CN102910660A (en) * | 2012-11-06 | 2013-02-06 | 傅培鑫 | Method for producing alum by utilizing alunite |
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2015
- 2015-02-15 CN CN201510081845.2A patent/CN105271341A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2350564C2 (en) * | 2007-05-04 | 2009-03-27 | Институт химии и технологии редких элементов и минерального сырья им. И.В. Тананаева Кольского научного центра Российской академии наук | Potassium alum production method |
| 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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106277010A (en) * | 2016-08-24 | 2017-01-04 | 淄博市淄川程鹏化工厂 | A kind of Alumen production technology |
| 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 |
| CN106986364A (en) * | 2017-04-13 | 2017-07-28 | 广西隆安瑞丰工贸有限公司 | A kind of activated clay production waste coproduction alum, the method for gypsum |
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Application publication date: 20160127 |