CN105502456A - Method for recycling and preparing aluminum ammonium sulfate from activated clay production wastewater - Google Patents
Method for recycling and preparing aluminum ammonium sulfate from activated clay production wastewater Download PDFInfo
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- CN105502456A CN105502456A CN201510960344.1A CN201510960344A CN105502456A CN 105502456 A CN105502456 A CN 105502456A CN 201510960344 A CN201510960344 A CN 201510960344A CN 105502456 A CN105502456 A CN 105502456A
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- tschermigite
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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
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Abstract
The invention discloses a method for recycling and preparing aluminum ammonium sulfate from activated clay production wastewater, and belongs to the technical field of wastewater treatment and inorganic salt preparation. Activated clay production wastewater and bentonite are recycled repeatedly, aluminum sulfate dissolved into the activated clay production wastewater is saturated and subjected to a reaction with ammonium bisulfate, and aluminum ammonium sulfate with the purity being 99.86-99.92% is obtained through two times of crystallization. According to the method, activated clay production wastewater can be effectively treated, aluminum elements in the activated clay production wastewater are sufficiently utilized, and the purposes of energy conservation, emission reduction and waste material recycling are achieved.
Description
Technical field
The present invention relates to wastewater treatment and inorganic salt preparing technical field, be specifically related to a kind ofly from activated clay production waste, reclaim the method for tschermigite produced.
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.
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 strong aqua (potassium hydroxide), filter, evaporate, thick alum, then obtain through purification and impurity removal the alum finished product that purity is greater than 99%.This invention solves Problems existing in the improvement of activated clay production waste and recoverying and utilizing method, has recycled alum, but the method also also exists shortcomings such as production cost is high, the production cycle is long.
Summary of the invention
The technical problem to be solved in the present invention is to provide and a kind ofly from activated clay production waste, reclaims the method for tschermigite produced, to solve the problem that existing activated clay production waste processing mode causes aluminium element significant wastage.The present invention effectively can process activated clay production waste, the aluminium element in activated clay production waste 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:
From activated clay production waste, reclaim the method producing tschermigite, comprise the following steps:
S1: adopt activated clay production waste to mix with wilkinite, bentonitic aluminium sesquioxide is made to be dissolved in activated clay production waste, again the activated clay production waste circulation increasing Tai-Ace S 150 concentration is mixed with the wilkinite newly increased, with such processing step cyclical operation, until the Tai-Ace S 150 being dissolved in activated clay production waste reaches capacity;
S2: the activated clay production waste 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: tschermigite obtained for step S4 is adopted hot air dries, namely obtained pure tschermigite.
Preferably, in step S1, bentonitic aluminium sesquioxide is dissolved in the temperature of activated clay production waste is 90-94 DEG C, and the activated clay production waste circulation increasing Tai-Ace S 150 concentration is 2-5 time with the wilkinite mixed cycle operation steps newly increased.
Preferably, the temperature that the activated clay production waste that in step S2, Tai-Ace S 150 reaches capacity controls is 86-88 DEG C, and pH value is 4.1-4.3.
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 1.01-1.04:1:2.01-2.06.
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 tschermigite is depressed into water ratio≤40%.
Preferably, in step S4, amount of water is weight 1.1-1.3 times of thick tschermigite.
Preferably, warm air described in step S5 is that flue-gas and air heat exchange obtain.
More preferably, described flue-gas temperature is 860-900 DEG C, and described air themperature is 8-35 DEG C, and described hot air temperature is 300-400 DEG C.
Preferably, in step S5, tschermigite is dried 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) the present invention effectively make use of the energy of soot waste gas, dries tschermigite at a higher temperature, makes the production cycle of the present invention shorter than prior art;
(3) not only purity is high for the tschermigite prepared of the present invention, reaches 99.86%-99.92%, and steady quality;
(4) the present invention can aluminium element in effective recycling activated clay production waste, and does not increase new element in activated clay production waste, reaches the object of comprehensive utilization, energy-saving and emission-reduction.
Accompanying drawing explanation
Fig. 1 is that the present invention reclaims the process flow diagram producing tschermigite from activated clay production waste.
Embodiment
Embodiment 1
From activated clay production waste, reclaim the method producing tschermigite, comprise the following steps:
S1: adopt activated clay production waste to mix with wilkinite at temperature is 90 DEG C, bentonitic aluminium sesquioxide is made to be dissolved in activated clay production waste, again the activated clay production waste circulation increasing Tai-Ace S 150 concentration is mixed with the wilkinite newly increased, the Tai-Ace S 150 being dissolved in activated clay production waste is reached capacity;
S2: the activated clay production waste 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 4.1 times, and the amount of added monoammonium sulfate is for making NH in tschermigite
4 +: Al
3+: SO
4 2-molar concentration rate be 1.01:1:2.02, 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: it is remove moisture further under the warm air of 300 DEG C that the tschermigite that obtained by step S4 adopts temperature to be the flue-gas of 860 DEG C and temperature to be the air heat exchange of 35 DEG C to obtain temperature is till 0.8% until tschermigite water ratio, namely obtained pure tschermigite.
Embodiment 2
From activated clay production waste, reclaim the method producing tschermigite, comprise the following steps:
S1: adopt activated clay production waste to mix with wilkinite at temperature is 94 DEG C, bentonitic aluminium sesquioxide is made to be dissolved in activated clay production waste, again the activated clay production waste circulation increasing Tai-Ace S 150 concentration is mixed with the wilkinite newly increased, with such processing step cyclical operation 5 times, until the Tai-Ace S 150 being dissolved in activated clay production waste reaches capacity;
S2: the activated clay production waste 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 4.2 times, and the amount of added monoammonium sulfate is for making NH in tschermigite
4 +: Al
3+: SO
4 2-molar concentration rate be 1.02:1:2.01, 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 1.3 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: it is remove moisture further under the warm air of 350 DEG C that the tschermigite that obtained by step S4 adopts temperature to be the flue-gas of 900 DEG C and temperature to be the air heat exchange of 8 DEG C to obtain temperature is till 0.9% until tschermigite water ratio, namely obtained pure tschermigite.
Embodiment 3
From activated clay production waste, reclaim the method producing tschermigite, comprise the following steps:
S1: adopt activated clay production waste to mix with wilkinite at temperature is 92 DEG C, bentonitic aluminium sesquioxide is made to be dissolved in activated clay production waste, again the activated clay production waste circulation increasing Tai-Ace S 150 concentration is mixed with the wilkinite newly increased, with such processing step cyclical operation 3 times, until the Tai-Ace S 150 being dissolved in activated clay production waste reaches capacity;
S2: the activated clay production waste 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 4.3 times, and the amount of added monoammonium sulfate is for making NH in tschermigite
4 +: Al
3+: SO
4 2-molar concentration rate be 1.04:1:2.06, 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: it is remove moisture further under the warm air of 400 DEG C that the tschermigite that obtained by step S4 adopts temperature to be the flue-gas of 900 DEG C and temperature to be the air heat exchange of 35 DEG C to obtain temperature is till 0.6% until tschermigite water ratio, namely obtained pure tschermigite.
Embodiment 4
From activated clay production waste, reclaim the method producing tschermigite, comprise the following steps:
S1: adopt activated clay production waste to mix with wilkinite at temperature is 93 DEG C, bentonitic aluminium sesquioxide is made to be dissolved in activated clay production waste, again the activated clay production waste circulation increasing Tai-Ace S 150 concentration is mixed with the wilkinite newly increased, with such processing step cyclical operation 4 times, until the Tai-Ace S 150 being dissolved in activated clay production waste reaches capacity;
S2: the activated clay production waste 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 4.1 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 1.3 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: it is remove moisture further under the warm air of 360 DEG C that the tschermigite that obtained by step S4 adopts temperature to be the flue-gas of 880 DEG C and temperature to be the air heat exchange of 20 DEG C to obtain temperature, till tschermigite water ratio≤0.7%, namely obtained pure tschermigite.
Embodiment 5
From activated clay production waste, reclaim the method producing tschermigite, comprise the following steps:
S1: adopt activated clay production waste to mix with wilkinite at temperature is 92 DEG C, bentonitic aluminium sesquioxide is made to be dissolved in activated clay production waste, again the activated clay production waste circulation increasing Tai-Ace S 150 concentration is mixed with the wilkinite newly increased, with such processing step cyclical operation 4 times, until the Tai-Ace S 150 being dissolved in activated clay production waste reaches capacity;
S2: the activated clay production waste 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 4.3 times, and the amount of added monoammonium sulfate is for making NH in tschermigite
4 +: Al
3+: SO
4 2-molar concentration rate be 1.04:1:2.05, 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 1.3 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: it is remove moisture further under the warm air of 380 DEG C that the tschermigite that obtained by step S4 adopts temperature to be the flue-gas of 870 DEG C and temperature to be the air heat exchange of 30 DEG C to obtain temperature is till 0.9% until tschermigite water ratio, namely obtained pure tschermigite.
Embodiment 6
From activated clay production waste, reclaim the method producing tschermigite, comprise the following steps:
S1: adopt activated clay production waste to mix with wilkinite at temperature is 94 DEG C, bentonitic aluminium sesquioxide is made to be dissolved in activated clay production waste, again the activated clay production waste circulation increasing Tai-Ace S 150 concentration is mixed with the wilkinite newly increased, with such processing step cyclical operation 5 times, until the Tai-Ace S 150 being dissolved in activated clay production waste reaches capacity;
S2: the activated clay production waste 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 4.2 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: it is remove moisture further under the warm air of 320 DEG C that the tschermigite that obtained by step S4 adopts temperature to be the flue-gas of 890 DEG C and temperature to be the air heat exchange of 25 DEG C to obtain temperature is till 0.6% 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.
As seen from the above table, the tschermigite purity (butt meter) that the present invention reclaims the method gained producing tschermigite from activated clay production waste is 99.86%-99.92%, 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 (10)
1. from activated clay production waste, reclaim the method producing tschermigite, it is characterized in that: comprise the following steps:
S1: adopt activated clay production waste to mix with wilkinite, bentonitic aluminium sesquioxide is made to be dissolved in activated clay production waste, again the activated clay production waste circulation increasing Tai-Ace S 150 concentration is mixed with the wilkinite newly increased, with such processing step cyclical operation, until the Tai-Ace S 150 being dissolved in activated clay production waste reaches capacity;
S2: the activated clay production waste 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: tschermigite obtained for step S4 is adopted hot air dries, namely obtained pure tschermigite.
2. according to claim 1ly from activated clay production waste, reclaim the method for tschermigite produced, it is characterized in that, in step S1, bentonitic aluminium sesquioxide is dissolved in the temperature of activated clay production waste is 90-94 DEG C, and the activated clay production waste circulation increasing Tai-Ace S 150 concentration is 2-5 time with the wilkinite mixed cycle operation steps newly increased.
3. according to claim 1ly from activated clay production waste, reclaim the method for tschermigite produced, it is characterized in that, the temperature that the activated clay production waste that in step S2, Tai-Ace S 150 reaches capacity controls is 86-88 DEG C, and pH value is 4.1-4.3.
4. according to claim 1ly from activated clay production waste, reclaim the method for tschermigite produced, it 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 1.01-1.04:1:2.01-2.06.
5. according to claim 1ly from activated clay production waste, reclaim the method for tschermigite produced, it is characterized in that, temperature≤12 DEG C of clear liquid crystallisation by cooling in step S3 and S4.
6. according to claim 1ly from activated clay production waste, reclaim the method for tschermigite produced, 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. according to claim 1ly from activated clay production waste, reclaim the method for tschermigite produced, it is characterized in that, in step S4 amount of water be the weight 1.1-1.3 of thick tschermigite doubly.
8. according to claim 1ly from activated clay production waste, reclaim the method for tschermigite produced, it is characterized in that, warm air described in step S5 is that flue-gas and air heat exchange obtain.
9. according to claim 8ly from activated clay production waste, reclaim the method for tschermigite produced, it is characterized in that, described flue-gas temperature is 860-900 DEG C, and described air themperature is 8-35 DEG C, and described hot air temperature is 300-400 DEG C.
10. according to claim 1ly from activated clay production waste, reclaim the method for tschermigite produced, it is characterized in that, in step S5, tschermigite is dried to water ratio≤0.9%.
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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 |
| 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 |
| 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 |
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Application publication date: 20160420 |