CN104445330A - Method for producing aluminum ammonium sulfate crystal - Google Patents
Method for producing aluminum ammonium sulfate crystal Download PDFInfo
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- CN104445330A CN104445330A CN201410755557.6A CN201410755557A CN104445330A CN 104445330 A CN104445330 A CN 104445330A CN 201410755557 A CN201410755557 A CN 201410755557A CN 104445330 A CN104445330 A CN 104445330A
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- Prior art keywords
- aluminum
- ammonium sulfate
- tschermigite
- gained
- tai
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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
Abstract
The invention discloses a method for producing an aluminum ammonium sulfate crystal from an industrial waste (aluminum residue). The method for producing the aluminum ammonium sulfate from aluminum residue comprises the following steps: (1) preparing an aluminum residue slurry from aluminum residue; (2) enabling the aluminum residue slurry to react with concentrated sulfuric acid to generate a crude aluminum sulfate solution; (3) precipitating to separate the crude aluminum sulfate solution; (4) enabling aluminum sulfate to react with aluminum sulfate to generate a crude aluminum ammonium sulfate solution; (5) cooling to crystallize the crude aluminum ammonium sulfate solution; and (6) washing the aluminum ammonium sulfate crystal with water, airing, and packaging to obtain the finished product of aluminum ammonium sulfate. Because aluminum residue is used as the raw material to produce the aluminum ammonium sulfate crystal, the production cost can be reduced. A small amount of aluminum residue is used, but an additional benefit can be achieved. The wastewater can be recycled. The process for producing the aluminum ammonium sulfate crystal is simple, is convenient to operate, is highly safe, is low in production cost, consumes less energy and is suitable of large-scale production.
Description
Technical field
The present invention relates to a kind of production method of tschermigite, specifically, refer to by industrial waste---aluminum dross prepares the method for tschermigite, belongs to chemical technology field.
Background technology
Tschermigite, i.e. Monoaluminum monoammonium disulfate Dodecahydrate, be again aluminium ammonium alum, ammonium alum and jewel alum, and molecular formula is NH
4al (SO
4)
212H
2o, be colourless crystallization, white particle or powder, taste is micro-sweet and puckery; 120 DEG C time, lose 10 molecular crystal water, 250 DEG C time, slough crystal water becomes white powder, i.e. exsiccated alum, more than 280 DEG C decomposition, and discharges ammonia; Water soluble, diluted acid, glycerine, be insoluble to ethanol; Density 1.64g/cm
3, fusing point 94.5 DEG C, refractive index 1.459.
The purposes of tschermigite widely, buffer reagent, the raising agent of food grade products can be used as, the flocculation agent of sewage purification, the aluminum tanning agent of tanning industry and the post-treatment agent of hide tannage, the reserving agent of dyestuffs industries, the upper stain of paper industry paper sizing, the tinting material of glass industry yellow glass, sword agent received by medicine, and printing and dyeing mordant, also can be used for the industrial circles such as pigment, plating, starch.
The production method of tschermigite mainly contains:
(1) reacted by alum liquor and ammoniumsulphate soln, and obtained through crystallisation by cooling, centrifugation, washing and drying, and chemical equation is:
Al
2(SO
4)
3+(NH
4)
2SO
4+12H
2O→2NH
4Al(SO
4)
2·12H
2O
(2) bauxitic clay method: generate alum liquor with sulfuric acid decomposition bauxite ore, then add ammonium sulfate reaction, through concentrated, crystallisation by cooling, separating, washing, get product, chemical equation is:
Al
2O
3+3H
2SO
4→Al
2(SO
4)
3+3H
2O
Al
2(SO
4)
3+(NH
4)
2SO
4+24H
2O→2NH
4Al(SO
4)
2·12H
2O
(3) aluminium hydroxide method: aluminium hydroxide and sulfuric acid reaction generate Tai-Ace S 150, then react with ammonium sulfate, through concentrated, crystallisation by cooling, drying, get product, chemical equation is:
2Al(OH)
3+3H
2SO
4→Al
2(SO
4)
3+6H
2O
Al
2(SO
4)
3+(NH
4)
2SO
4+24H
2O→2NH
4Al(SO
4)
2·12H
2O
(4) under 400 DEG C of high temperature, aluminum oxide and the reaction of sulphur ammonium can generate exsiccated ammonium alum, and chemical equation is:
Al
2O
3+4(NH
4)
2SO
4→2NH
4Al(SO
4)
2+6NH
3+3H
20
Above-mentioned 4 kinds of production methods, method (1) adopts finished product sulfuric acid aluminium to be raw material, and price is higher, and cause production cost higher, the market competitiveness is little, adopts the producer of this method considerably less; Method (2) is because most of enterprise all adopts bauxitic clay to produce all the year round, China's aluminum current alumina raw is caused to reduce, raw materials quality generally declines, and in production process, a large amount of acid waste residue waste water can be produced, the manpower and materials of at substantial, cause the production cost of product high, labour intensity is large; Method (3) is because aluminium hydroxide cost of material used is higher, and cause production cost to increase, benefit is low, and Jin You minority producer adopts this method; Method (4) adopts finished product aluminum oxide and ammonium sulfate, and price is higher, and desired reaction temperature is higher, causes production cost to increase.
Aluminum dross is the solid waste produced in aluminum profile extrusion pretreatment process, and China all will produce the aluminum dross of thousands of tons of every year.Although aluminum dross is through concentrated, water ratio is still very high, not only takies a large amount of places, and its transudate also can polluted underground water body, works the mischief to environment.Containing a large amount of effective constituent---aluminum oxide in aluminum dross, it is good industrial raw material source.At present for the mineral wealth relative shortage such as high-quality bauxite, kaolin of aluminium metallurgy, and this kind of mineral wealth also exist the drawback that smelting is difficult, solubility rate is low, energy consumption is high; And the aluminum dross that Aluminiferous waste slag, particularly aluminum profile extrusion produce does not exist the problem of stripping difficulty, and raw material sources are refuse, both can save raw materials cost, can save waste treatment expense again.
Summary of the invention
Technical problem to be solved by this invention is not enough for prior art, provides a kind of by industrial waste---aluminium slag prepares the production method of tschermigite, and present method technique is simple, with low cost, be easy to heavy industrialization application.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of production method of tschermigite, comprises following processing step:
(1) pulping process: get aluminum dross raw material, after pulverizing, add water stirring, obtained aluminium dreg slurry;
(2) the thick liquid preparation section of Tai-Ace S 150: first the aluminium dreg slurry that step (1) is obtained is pumped in reactor, again the vitriol oil pumping into high-order bucket is joined in reactor, closed reactor, stir, when reacting kettle inner pressure is 0.3 ~ 0.4MPa, stop stirring, leave standstill, the obtained thick liquid of Tai-Ace S 150; When reacting kettle inner pressure is 0.1MPa, by the obtained thick liquid discharging of Tai-Ace S 150 to settling vat;
(3) the settlement separate operation of the thick liquid of Tai-Ace S 150:
A, bottom settling vat, pass into pressurized air, blown to boiling by the mixed solution of thick for Tai-Ace S 150 liquid and washing end slag gained washings, add polymeric flocculant and produce alumen ustum to described mixed solution, adjust ph scope is 1.5 ~ 2.5, leave standstill, obtain supernatant liquor and end slag;
B, supernatant liquor is delivered to pressure filter, after press filtration, obtain filtrate and filter cake; Filtrate delivers to hold-up vessel, is aluminum sulfate mother liquor; Filter cake is delivered to cement mill and is done tankage; Rinse the filter cloth of pressure filter with clear water, obtain scavenging solution;
C, by end slag with step b gained scavenging solution and from crystallisation by cooling operation gained crystalline mother solution washing, obtain washings, deliver to subordinate's settling vat;
(4) the thick liquid preparation section of exsiccated ammonium alum: by step (3) gained aluminum sulfate mother liquor, delivers in exsiccated ammonium alum reaction concentration tank, heating, and adds ammonium sulfate, stir, after ammonium sulfate dissolves completely, stop stirring, obtain the thick liquid of exsiccated ammonium alum;
(5) crystallisation by cooling operation: by the thick liquid of step (4) gained exsiccated ammonium alum, deliver to crystallizing pond, naturally cooling dries, and obtains ammonium aluminum sulfate crystal and crystalline mother solution; By gained crystalline mother solution, return step (3), as the bath water of end slag;
(6) wash, dry, packaging process: by step (5) gained ammonium aluminum sulfate crystal, wash decon with water, more naturally dry, packaging, obtain tschermigite finished product; After water lotion adds limestone vegetation, as plant area's greening water.
On the basis of technique scheme, the present invention can also do following improvement.
Further, in step (1) described aluminum dross, the content of aluminum oxide is 20 ~ 60%, and described aluminum dross powder particle diameter is >=80 orders, and the concentration of described aluminium dreg slurry is 30 ~ 40 degree Beaume.
Further, the massfraction of step (2) the described vitriol oil is 98%, and the additional proportion of the described vitriol oil is: the weight ratio of aluminium dreg slurry and the vitriol oil is 1:1, and the speed of described stirring is 20 ~ 25 revs/min, time is 5 ~ 35 minutes, and the described standing time is 2 ~ 4 hours.
Further, the described compressed-air actuated flow of step (3) is 2.5MPa, and described polymeric flocculant is polyacrylamide, and described time of repose is 2 ~ 3 hours, and described pressure filter is plate and frame(type)filter press, and described washing times is 1 time.
Further, (the NH in step (4) described ammonium sulfate
4)
2sO
4contents on dry basis>=21%, the additional proportion of described ammonium sulfate is: the weight ratio of Tai-Ace S 150 and ammonium sulfate is 8:1.
Further, the time that step (5) described naturally cooling dries is 2 ~ 4 days.
Further, step (6) the described time of naturally drying is 1 ~ 2 day, the NH of described tschermigite finished product
4al (SO
4)
2contents on dry basis>=99.2%.
The invention has the beneficial effects as follows:
(1) saving production cost: the present invention is with industrial waste---aluminum dross is raw material production tschermigite, the a small amount of waste residue produced in production process also can be delivered to cement mill and do tankage, the cycling utilization of wastewater produced, achieve effective utilization of refuse, both decrease environmental pollution, again save production cost.
(2) energy is saved: the present invention's aluminum dross, sulfuric acid produce Tai-Ace S 150, utilize exothermic heat of reaction, without the need to external heat source, and the vitriol oil enters reactor from high-order bucket, under gravity, sink with acceleration, speed of response is accelerated, enhances productivity.
(3) labor intensity of operating staff is reduced: aluminium dreg slurry of the present invention adopts pumping, achieves semi-automation, avoids operator and come and go eminence to reacting aluminum sulfate still Manual material feeding, alleviate the labour intensity of operator; The vitriol oil is that automatic gauge adds reactor, and operator, without the need to directly contacting the vitriol oil, decrease the possibility that vitriol oil corrosion risk accident occurs.
(4) reduce waste sludge discharge: the settlement separate operation of traditional with bauxite is raw material, waste residue output is up to 40 ~ 50%, and gained waste residue content≤5% of the present invention, this also substantially increases the concentration of subsequent sulphuric acid aluminium mother liquor.
(5) present invention process is simple, and easy to operate, security is high, consuming little energy, and waste residue amount is few and can bring add on yield, waste water reusable edible, and production cost is low, is suitable for large-scale production.
Accompanying drawing explanation
Fig. 1 is the production technological process of tschermigite of the present invention.
Embodiment
Be described principle of the present invention and feature below in conjunction with specific embodiment, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1:
A production method for tschermigite, comprises following processing step:
(1) pulping process: the content getting aluminum oxide is the aluminum dross raw material of 20 ~ 60%, after being ground into 80 order particle diameters, being placed in stock tank, stirs while add waterside, the aluminium dreg slurry of obtained 30 ~ 40 degree Beaume;
(2) the thick liquid preparation section of Tai-Ace S 150: first the aluminium dreg slurry that step (1) is obtained is pumped in reactor, the vitriol oil being 98% by the massfraction pumping into high-order bucket again joins in reactor, the weight ratio of aluminium dreg slurry and the vitriol oil is 1:1, closed reactor, starts agitator and stirs, the speed stirred is 25 revs/min, time is 5 minutes, when reacting kettle inner pressure is 0.3 ~ 0.4MPa, stops stirring, leave standstill 2 hours, the obtained thick liquid of Tai-Ace S 150; When reacting kettle inner pressure is 0.1MPa, by the obtained thick liquid discharging of Tai-Ace S 150 to settling vat;
(3) the settlement separate operation of the thick liquid of Tai-Ace S 150:
A, bottom settling vat, pass into the pressurized air that flow is 2.5MPa, the mixed solution of thick for Tai-Ace S 150 liquid and washing end slag gained washings is blown to boiling, add polyacrylamide and produce alumen ustum to described mixed solution, adjust ph scope is 1.5 ~ 2.5, leave standstill 2 ~ 3 hours, obtain supernatant liquor and end slag;
B, supernatant liquor is delivered to plate and frame(type)filter press, after press filtration, obtain filtrate and filter cake; Filtrate delivers to hold-up vessel, is aluminum sulfate mother liquor; Filter cake is delivered to cement mill and is done tankage; Rinse the filter cloth of pressure filter with clear water, obtain scavenging solution;
C, by end slag with step b gained scavenging solution and from crystallisation by cooling operation gained crystalline mother solution washing, obtain washings, deliver to subordinate's settling vat;
(4) the thick liquid preparation section of exsiccated ammonium alum: by step (3) gained aluminum sulfate mother liquor, delivers in exsiccated ammonium alum reaction concentration tank, heating, and adds ammonium sulfate in proportion, (the NH in ammonium sulfate
4)
2sO
4contents on dry basis>=21%, the weight amount of Tai-Ace S 150 and ammonium sulfate, than being 8:1, stirs, and after ammonium sulfate dissolves completely, stops stirring, obtains the thick liquid of exsiccated ammonium alum;
(5) crystallisation by cooling operation: by the thick liquid of step (4) gained exsiccated ammonium alum, deliver to crystallizing pond, naturally cooling dries 2 days, obtains ammonium aluminum sulfate crystal and crystalline mother solution; By gained crystalline mother solution, return step (3), as the bath water of end slag;
(6) wash, dry, packaging process: by step (5) gained ammonium aluminum sulfate crystal, wash decon with water, more naturally dry 1 ~ 2 day, packaging, obtain tschermigite finished product, its NH
4al (SO
4)
2contents on dry basis be 99.2%; After water lotion adds limestone vegetation, as plant area's greening water.
Embodiment 2:
A production method for tschermigite, comprises following processing step:
(1) pulping process: the content getting aluminum oxide is the aluminum dross raw material of 20 ~ 60%, after being ground into 100 order particle diameters, being placed in stock tank, stirs while add waterside, the aluminium dreg slurry of obtained 30 ~ 40 degree Beaume;
(2) the thick liquid preparation section of Tai-Ace S 150: first the aluminium dreg slurry that step (1) is obtained is pumped in reactor, the vitriol oil being 98% by the massfraction pumping into high-order bucket again joins in reactor, the weight ratio of aluminium dreg slurry and the vitriol oil is 1:1, closed reactor, starts agitator and stirs, the speed stirred is 20 revs/min, time is 35 minutes, when reacting kettle inner pressure is 0.3 ~ 0.4MPa, stops stirring, leave standstill 2 hours, the obtained thick liquid of Tai-Ace S 150; When reacting kettle inner pressure is 0.1MPa, by the obtained thick liquid discharging of Tai-Ace S 150 to settling vat;
(3) the settlement separate operation of the thick liquid of Tai-Ace S 150:
A, bottom settling vat, pass into the pressurized air that flow is 2.5MPa, thick for Tai-Ace S 150 liquid and washing end slag gained washings are blown to boiling, add polyacrylamide and produce alumen ustum to described mixed solution, adjust ph scope is 1.5 ~ 2.5, leave standstill 2 ~ 3 little, obtain supernatant liquor and end slag;
B, supernatant liquor is delivered to plate and frame(type)filter press, after press filtration, obtain filtrate and filter cake; Filtrate delivers to hold-up vessel, is aluminum sulfate mother liquor; Filter cake is delivered to cement mill and is done tankage; Rinse the filter cloth of pressure filter with clear water, obtain scavenging solution;
C, by end slag with step b gained scavenging solution and from crystallisation by cooling operation gained crystalline mother solution washing, obtain washings, deliver to subordinate's settling vat;
(4) the thick liquid preparation section of exsiccated ammonium alum: by step (3) gained aluminum sulfate mother liquor, delivers in exsiccated ammonium alum reaction concentration tank, heating, and adds ammonium sulfate in proportion, (the NH in ammonium sulfate
4)
2sO
4contents on dry basis>=21%, the weight amount of Tai-Ace S 150 and ammonium sulfate, than being 8:1, stirs, and after ammonium sulfate dissolves completely, stops stirring, obtains the thick liquid of exsiccated ammonium alum;
(5) crystallisation by cooling operation: by the thick liquid of step (4) gained exsiccated ammonium alum, deliver to crystallizing pond, naturally cooling dries 4 days, obtains ammonium aluminum sulfate crystal and crystalline mother solution; By gained crystalline mother solution, return step (3), as the bath water of end slag;
(6) wash, dry, packaging process: by step (5) gained ammonium aluminum sulfate crystal, wash decon with water, more naturally dry 1 ~ 2 day, packaging, obtain tschermigite finished product, its NH
4al (SO
4)
2contents on dry basis be 99.8%; After water lotion adds limestone vegetation, as plant area's greening water.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. a production method for tschermigite, is characterized in that, comprises following processing step:
(1) pulping process: get aluminum dross raw material, after pulverizing, add water stirring, obtained aluminium dreg slurry;
(2) the thick liquid preparation section of Tai-Ace S 150: first the aluminium dreg slurry that step (1) is obtained is pumped in reactor, again the vitriol oil pumping into high-order bucket is joined in reactor, closed reactor, stir, when reacting kettle inner pressure is 0.3 ~ 0.4MPa, stop stirring, leave standstill, the obtained thick liquid of Tai-Ace S 150; When reacting kettle inner pressure is 0.1MPa, by the obtained thick liquid discharging of Tai-Ace S 150 to settling vat;
(3) the settlement separate operation of the thick liquid of Tai-Ace S 150:
A, bottom settling vat, pass into pressurized air, blown to boiling by the mixed solution of thick for Tai-Ace S 150 liquid and washing end slag gained washings, add polymeric flocculant and produce alumen ustum to described mixed solution, adjust ph scope is 1.5 ~ 2.5, leave standstill, obtain supernatant liquor and end slag;
B, supernatant liquor is delivered to pressure filter, after press filtration, obtain filtrate and filter cake; Filtrate delivers to hold-up vessel, is aluminum sulfate mother liquor; Filter cake is delivered to cement mill and is done tankage; Rinse the filter cloth of pressure filter with clear water, obtain scavenging solution;
C, by end slag with step b gained scavenging solution and from crystallisation by cooling operation gained crystalline mother solution washing, obtain washings, deliver to subordinate's settling vat;
(4) the thick liquid preparation section of exsiccated ammonium alum: by step (3) gained aluminum sulfate mother liquor, delivers in exsiccated ammonium alum reaction concentration tank, heating, and adds ammonium sulfate, stir, after ammonium sulfate dissolves completely, stop stirring, obtain the thick liquid of exsiccated ammonium alum;
(5) crystallisation by cooling operation: by the thick liquid of step (4) gained exsiccated ammonium alum, deliver to crystallizing pond, naturally cooling dries, and obtains ammonium aluminum sulfate crystal and crystalline mother solution; By gained crystalline mother solution, return step (3), as the bath water of end slag;
(6) wash, dry, packaging process: by step (5) gained ammonium aluminum sulfate crystal, wash decon with water, more naturally dry, packaging, obtain tschermigite finished product; After water lotion adds limestone vegetation, as plant area's greening water.
2. the production method of a kind of tschermigite according to claim 1, it is characterized in that, in step (1) described aluminum dross, the content of aluminum oxide is 20 ~ 60%, and described aluminum dross powder particle diameter is >=80 orders, and the concentration of described aluminium dreg slurry is 30 ~ 40 degree Beaume.
3. the production method of a kind of tschermigite according to claim 1, it is characterized in that, the massfraction of step (2) the described vitriol oil is 98%, the additional proportion of the described vitriol oil is: the weight ratio of aluminium dreg slurry and the vitriol oil is 1:1, the speed of described stirring is 20 ~ 25 revs/min, time is 5 ~ 35 minutes, and the described standing time is 2 ~ 4 hours.
4. the production method of a kind of tschermigite according to claim 1, it is characterized in that, the described compressed-air actuated flow of step (3) is 2.5MPa, described polymeric flocculant is polyacrylamide, described time of repose is 2 ~ 3 hours, described pressure filter is plate and frame(type)filter press, and described washing times is 1 time.
5. the production method of a kind of tschermigite according to claim 1, is characterized in that, (the NH in step (4) described ammonium sulfate
4)
2sO
4contents on dry basis>=21%, the additional proportion of described ammonium sulfate is: the weight ratio of Tai-Ace S 150 and ammonium sulfate is 8:1.
6. the production method of a kind of tschermigite according to any one of claim 1 to 5, is characterized in that, the time that step (5) described naturally cooling dries is 2 ~ 4 days.
7. the production method of a kind of tschermigite according to any one of claim 1 to 5, is characterized in that, step (6) the described time of naturally drying is 1 ~ 2 day, the NH of described tschermigite finished product
4al (SO
4)
2contents on dry basis>=99.2%.
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|---|---|---|---|
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|---|---|---|---|
| CN201410755557.6A CN104445330B (en) | 2014-12-10 | 2014-12-10 | A kind of production method of ammonia-alum |
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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 |
| CN107117638A (en) * | 2017-04-13 | 2017-09-01 | 广西隆安瑞丰工贸有限公司 | A kind of method that activated clay production spent acid prepares alum |
| CN107487952A (en) * | 2017-09-22 | 2017-12-19 | 中南大学 | A kind of combination treatment method of the residual beneficiation wastewater containing xanthate |
| CN114317979A (en) * | 2021-12-29 | 2022-04-12 | 五矿稀土江华有限公司 | Method for recovering aluminum from ionic rare earth impurity removal slag |
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Cited By (5)
| 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 |
| CN107117638A (en) * | 2017-04-13 | 2017-09-01 | 广西隆安瑞丰工贸有限公司 | A kind of method that activated clay production spent acid prepares alum |
| CN107487952A (en) * | 2017-09-22 | 2017-12-19 | 中南大学 | A kind of combination treatment method of the residual beneficiation wastewater containing xanthate |
| CN107487952B (en) * | 2017-09-22 | 2020-09-29 | 长沙华时捷环保科技发展股份有限公司 | Combined treatment method for beneficiation wastewater containing xanthate residues |
| CN114317979A (en) * | 2021-12-29 | 2022-04-12 | 五矿稀土江华有限公司 | Method for recovering aluminum from ionic rare earth impurity removal slag |
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| Publication number | Publication date |
|---|---|
| CN104445330B (en) | 2016-05-18 |
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