CN107117638A - A kind of method that activated clay production spent acid prepares alum - Google Patents
A kind of method that activated clay production spent acid prepares alum Download PDFInfo
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- CN107117638A CN107117638A CN201710241434.4A CN201710241434A CN107117638A CN 107117638 A CN107117638 A CN 107117638A CN 201710241434 A CN201710241434 A CN 201710241434A CN 107117638 A CN107117638 A CN 107117638A
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- Prior art keywords
- alum
- spent acid
- activated clay
- sulfate
- clay production
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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
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/68—Aluminium compounds containing sulfur
- C01F7/74—Sulfates
- C01F7/76—Double salts, i.e. compounds containing, besides aluminium and sulfate ions, only other cations, e.g. alums
- C01F7/762—Ammonium or alkali metal aluminium sulfates
- C01F7/765—Ammonium aluminium sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of method that activated clay production spent acid prepares alum, belong to activated clay production waste processing and inorganic salts preparing technical field.The present invention is repeatedly circulated with bentonite using activated clay production spent acid, is made to be dissolved in aluminum sulfate therein and is reached saturation, then is reacted with ammonium sulfate (potassium sulfate or sodium sulphate), through flocculation, crystallizes pure alum is made twice.The present invention uses polyaluminium sulfate as flocculant, pass through further optimize technique simultaneously, so that the alum purity obtained by the method for the present invention reaches more than 99.85%, increase rate must be measured and reach more than 16.89%, " a kind of utilization atlapulgite spent acid mother liquor prepares the method (publication number of alum than prior art:CN105271342A it is) " high.
Description
【Technical field】
The present invention relates to activated clay production waste processing and inorganic salts preparing technical field, and in particular to a kind of activity is white
The method that autochthonal production spent acid prepares alum.
【Background technology】
Atlapulgite is mainly used in the decolorizing and refining of mineral oil, vegetable oil and animal fat, is a kind of important oil
Work and daily-use chemical industry raw material.Atlapulgite is, using bentonite as raw material, mainly to be processed using wet method acidification technique.It is produced
Process includes:Bentonite aquation plus sulfuric acid activated, washing, dry, crushing., need to be through washing repeatedly just because its product acid content is big
Acid content can be made to be less than 0.2%, to reach the requirement of HG/T2569-94 product standards.It is different according to method, what water-washing process was produced
Wastewater flow rate has different, but the wastewater flow rate that production 1t atlapulgites are produced typically is no less than 30-40t.Mainly contain in the waste water
There are aluminum sulfate and unreacted sulfuric acid that bentonite acidification reaction is produced etc., if directly discharging, not only waste substantial amounts of resource,
And serious pollution can be caused to environment.
In recent years, the improvement and recycling for activated clay production waste have pointed out certain methods, and such as lime is neutralized
Method, carbide slag neutralisation, time acid activation method, and china clay is decomposed with process industry water treatment agent aluminum sulfate with it, dissolve iron filings
Manufacture green vitriol etc..These methods, what is had preferably solves the governing problem of activated clay production waste, and such as lime neutralisation is led to
Crossing addition lime can be neutralized the acidity in waste water, make the formation such as sulfate ion, aluminium ion and iron ion calcium sulfate, hydrogen
Aluminum oxide, iron hydroxide etc. are precipitated and removed, but these sediments turn into new solid waste because that can not be utilized;What is had is preferable
Ground solves the problems, such as the recycling of resource in activated clay production waste, such as decomposes china clay with it with process industry water process
The method of agent aluminum sulfate is exactly to decompose china clay using the sulfuric acid in waste water, and the aluminium in china clay is leached to solution, then passes through
Purification and impurity removal, evaporative crystallization, separation drying, crushing packing obtain aluminum sulfate, and the method is although efficiently utilize activated clay production
Resources such as sulfuric acid, aluminum sulfate in waste water, but because the impurity such as iron ion can influence the quality of product aluminum sulfate, thus must be through
Purification and impurity removal process is removed.At present frequently with activated manganese dioxide method except iron is, it is necessary to which expensive manganese salt, causes processing
Cost is higher.
Alum is generally comprised:Ammonia-alum (AlNH4(SO4)2·12H2O), potassium alum (AlK (SO4)2·12H2) and sodium is bright O
Alum (AlNa (SO4)2·12H2O)。
Ammonia-alum is mainly used in the purification of water, plating, the post processing of paper industry, tanning and the processing of fur, aluminum oxide
And the production of corundum, printing and dyeing industry is used as mordant, pharmaceutically as astringent, diuretics, emetic and cathartic, food addition
Agent etc..The current main production process of the product is that aluminum sulfate is made with sulfuric acid treatment bauxite, is then reacted with ammonium sulfate, then pass through
Purification, evaporation, crystallisation by cooling, filtering, drying and obtain.
Potassium alum is mainly used as the hardener of film and sensitive paper, water purification settling agent, medical astringent and styptic, printing and dyeing matchmaker
Stain, ferment powder raw material, papermaking cementing agent, tanning extracts, the raw material of production high purity aluminium oxide and other aluminium salts, rubber pange agent,
Food additives etc..The current main production process of the product is that aluminum sulfate is made with sulfuric acid treatment bauxite, then with potassium sulfate
Reaction, then purified, evaporation, crystallisation by cooling, filtering, drying and obtain.
Soda alum chemical name aluminum sodium sulfate, is white particulate or powdery.Met generation carbon dioxide with sodium acid carbonate, so
Food additives yeast powder is commonly used for, mordant, waterproofing agent are used as in textile industry, ceramics, tanning is may be additionally used for, makes
The industries such as paper, match, ink, purified water, refined sugar.The current main production process of the product is made with sulfuric acid treatment bauxite
Aluminum sulfate, then with sodium sulphate react, then purified, evaporation, crystallisation by cooling, filtering, drying and obtain.
" a kind of utilization atlapulgite spent acid mother liquor prepares the method (publication number of alum to patent:CN105271342A) ", it is public
Open a kind of method for preparing alum of knowing clearly, but this method is the problem of have purity and relatively low yield.
【The content of the invention】
The technical problem to be solved in the present invention is to provide a kind of method that activated clay production spent acid prepares alum, to solve
Atlapulgite spent acid mother liquor prepares the problem of alum has purity and relatively low yield in the prior art.The present invention uses polymerised sulphur
Sour aluminium is as flocculant, while passing through further optimize technique so that the alum purity obtained by method of the invention reaches
More than 99.85%, the amount of obtaining increase rate reaches more than 16.89%, and than prior art, " one kind utilizes atlapulgite spent acid mother liquor system
Method (the publication number of standby alum:CN105271342A it is) " high.
To solve above technical problem, the present invention uses following technical scheme:
A kind of method that activated clay production spent acid prepares alum, comprises the following steps:
S1:Mixed using activated clay production spent acid with bentonite, the aluminum sulfate in bentonite is dissolved in production spent acid
In, then by increase the activated clay production spent acid circulation of sulfuric acid aluminum concentration with newly plus bentonite mix, up to being dissolved in production
The aluminum sulfate of spent acid reaches saturation;
S2:Aluminum sulfate made from step S1 is reached into the production spent acid temperature control of saturation at 86-89 DEG C, pH value control exists
4.2-4.5, adds ammonium sulfate or potassium sulfate, then or sodium sulphate reaction generation alum;
S3:Added into step S2 alum solution after flocculant, coacervation alum, be then filtered to remove impurity, gained is clear
Liquid crystallisation by cooling, then press filtration obtains the thick alum of filter cake;
S4:By in thick alum input water made from step S3, it is heated up to 86-89 DEG C and stirring is completely dissolved thick alum
Afterwards, flocculant is added, after coacervation alum, impurity is then removed again, to gained clear liquid crystallisation by cooling again, then press filtration is obtained
Alum;
S5:Alum made from step S4 is put into centrifuge and removes moisture, that is, pure alum is made.
Preferably, the number of times that spent acid is recycled in step S1 is 3-4, and the temperature for controlling to dissolve aluminum sulfate is 96-99 DEG C.
Preferably, activated clay production spent acid temperature control is at 87 DEG C in step S2, and pH value is controlled 4.4.
Preferably, the method that pH value is controlled in step S2 is:Ammonium hydrogen carbonate is added when pH value is less than 4.2;When pH value is big
The activated clay production spent acid that pH value is less than 2.5 is added when 4.5.
Preferably, in step S2, when adding ammonium sulfate, the amount of the ammonium sulfate is to make NH in alum4 +:Al3+:SO4 2-'s
Molar concentration rate is 1-1.03:1:2.01-2.04;When adding potassium sulfate, the amount of the potassium sulfate is to make K in alum+:Al3+:
SO4 2-Molar concentration rate be 1.01-1.02:1:2.02-2.03;When adding sodium sulphate, the amount of the sodium sulphate is to make in alum
Na+:Al3+:SO4 2--Molar concentration rate be 1.02-1.04:1:2.01-2.03.
Preferably, flocculant described in step S2 and S4 is polyaluminium sulfate.
Preferably, the temperature of clear liquid crystallisation by cooling is less than 10 DEG C in step S3 and S4.
Preferably, the pressure of press filtration is 0.8-0.95MPa in step S3 and S4, and alum is depressed into moisture content for 46%-50%.
Preferably, amount of water is equal to the weight of thick alum in step S4.
Preferably, the rotating speed of centrifuge is 4000-5000r/min in step S5.
The invention has the advantages that:
The present invention uses polyaluminium sulfate as flocculant, and polyaluminium sulfate is composite polymer polymer, molecule knot
Structure is huge, high adsorption capacity, and the floccule body formed after input water is big, and settling velocity is fast, and activity is high, and filterability is good, passes through simultaneously
Further optimize technique so that the alum purity obtained by method of the invention reaches more than 99.85%, and the amount of obtaining increase rate reaches
More than 16.89%, than prior art, " a kind of utilization atlapulgite spent acid mother liquor prepares the method (publication number of alum:
CN105271342A it is) " high.
【Brief description of the drawings】
Fig. 1 is that activated clay production spent acid of the present invention prepares alum process chart.
【Embodiment】
For ease of more fully understanding the present invention, it is illustrated by following examples, these embodiments belong to the present invention's
Protection domain, but do not limit the scope of the invention.
In embodiment, the method that the activated clay production spent acid prepares alum comprises the following steps:
S1:Mixed using activated clay production spent acid with bentonite, control the temperature of solution to make for 96-99 DEG C in bentonite
Aluminum sulfate be dissolved in production spent acid in, then will increase sulfuric acid aluminum concentration activated clay production spent acid circulation with newly plus swelling
Soil mixing, is according to said method circulated 3-4 times, until the aluminum sulfate for being dissolved in production spent acid reaches saturation;
S2:Aluminum sulfate made from step S1 is reached into the production spent acid temperature control of saturation at 86-89 DEG C, to above-mentioned spent acid
Addition ammonium hydrogen carbonate or activated clay production spent acid make pH value be 4.2-4.5, add ammonium sulfate, and the amount of the ammonium sulfate is bright to make
NH in alum4 +:Al3+:SO4 2-Molar concentration rate be 1-1.03:1:2.01-2.04;When adding potassium sulfate, the amount of the potassium sulfate
To make K in alum+:Al3+:SO4 2-Molar concentration rate be 1.01-1.02:1:2.02-2.03;When adding sodium sulphate, the sulphur
The amount of sour sodium is to make Na in alum+:Al3+:SO4 2--Molar concentration rate be 1.02-1.04:1:2.01-2.03;
S3:Added into step S2 alum solution after polyaluminium sulfate, coacervation alum, be then filtered to remove impurity, institute
Obtain clear liquid and be cooled to less than 10 DEG C, then in the case where pressure is 0.8-0.95MPa, alum is depressed into moisture content for 46%-50%, obtained
To the thick alum of filter cake;
S4:By in the water of the weight such as thick alum input made from step S3, it is heated up to 86-89 DEG C and stirring makes thick alum complete
After fully dissolved, add after polyaluminium sulfate, coacervation alum, impurity then removed again, less than 10 DEG C are cooled to gained clear liquid,
Then in the case where pressure is 0.8-0.95MPa, alum is depressed into moisture content for 46%-50%, alum is obtained;
S5:Alum made from step S4 is put into the centrifuge that rotating speed is 4000-5000r/min and removes moisture, that is, is made
Obtain pure alum.
Embodiment 1
A kind of method that activated clay production spent acid prepares ammonia-alum, comprises the following steps:
S1:Mixed using activated clay production spent acid with bentonite, control the temperature of solution to make for 98 DEG C in bentonite
Aluminum sulfate is dissolved in production spent acid, then the bentonite that will increase the activated clay production spent acid circulation of sulfuric acid aluminum concentration and newly add
Mixing, is according to said method circulated 3 times, until the aluminum sulfate for being dissolved in production spent acid reaches saturation;
S2:The production spent acid temperature control that aluminum sulfate made from step S1 is reached into saturation adds at 87 DEG C to above-mentioned spent acid
Plus ammonium hydrogen carbonate or activated clay production spent acid make pH value be 4.4, ammonium sulfate is added, the amount of the ammonium sulfate is to make in alum
NH4 +:Al3+:SO4 2-Molar concentration rate be 1.01:1:2.01;
S3:Add after polyaluminium sulfate, coacervation ammonia-alum, be then filtered to remove miscellaneous into step S2 ammonia-alum solution
Matter, gained clear liquid is cooled to 8 DEG C, then in the case where pressure is 0.894MPa, and it is 48% that ammonia-alum is depressed into moisture content, obtains filter cake
Thick ammonia-alum;
S4:By in the water of the weight such as thick ammonia-alum input made from step S3, it is heated up to 87 DEG C and stirs make thick ammonia-alum
After being completely dissolved, add after polyaluminium sulfate, coacervation ammonia-alum, impurity then removed again, 9 DEG C are cooled to gained clear liquid,
Then in the case where pressure is 0.95MPa, it is 48% that ammonia-alum is depressed into moisture content, obtains ammonia-alum;
S5:Ammonia-alum made from step S4 is put into the centrifuge that rotating speed is 5000r/min and removes moisture, that is, is made pure
Net ammonia-alum.
Embodiment 2
A kind of method that activated clay production spent acid prepares potassium alum, comprises the following steps:
S1:Mixed using activated clay production spent acid with bentonite, control the temperature of solution to make for 97 DEG C in bentonite
Aluminum sulfate is dissolved in production spent acid, then the bentonite that will increase the activated clay production spent acid circulation of sulfuric acid aluminum concentration and newly add
Mixing, is according to said method circulated 4 times, until the aluminum sulfate for being dissolved in production spent acid reaches saturation;
S2:The production spent acid temperature control that aluminum sulfate made from step S1 is reached into saturation adds at 89 DEG C to above-mentioned spent acid
Plus ammonium hydrogen carbonate or activated clay production spent acid make pH value be 4.2, potassium sulfate is added, the amount of the potassium sulfate is to make K in alum+:Al3+:SO4 2-Molar concentration rate be 1.02:1:2.02;
S3:Add after polyaluminium sulfate, coacervation potassium alum, be then filtered to remove miscellaneous into step S2 potassium alum solution
Matter, gained clear liquid is cooled to 10 DEG C, then in the case where pressure is 0.8MPa, and it is 46% that potassium alum is depressed into moisture content, obtains filter cake
Thick potassium alum;
S4:By in the water of the weight such as thick potassium alum input made from step S3, it is heated up to 89 DEG C and stirs make thick potassium alum
After being completely dissolved, add after polyaluminium sulfate, coacervation potassium alum, impurity then removed again, 10 DEG C are cooled to gained clear liquid,
Then in the case where pressure is 0.8MPa, it is 46% that potassium alum is depressed into moisture content, obtains potassium alum;
S5:Potassium alum made from step S4 is put into the centrifuge that rotating speed is 4000r/min and removes moisture, that is, is made pure
Net potassium alum.
Embodiment 3
A kind of method that activated clay production spent acid prepares soda alum, comprises the following steps:
S1:Mixed using activated clay production spent acid with bentonite, control the temperature of solution to make for 99 DEG C in bentonite
Aluminum sulfate is dissolved in production spent acid, then the bentonite that will increase the activated clay production spent acid circulation of sulfuric acid aluminum concentration and newly add
Mixing, is according to said method circulated 3 times, until the aluminum sulfate for being dissolved in production spent acid reaches saturation;
S2:The production spent acid temperature control that aluminum sulfate made from step S1 is reached into saturation adds at 86 DEG C to above-mentioned spent acid
Plus ammonium hydrogen carbonate or activated clay production spent acid make pH value be 4.5, sodium sulphate is added, the amount of the sodium sulphate is to make Na in alum+:Al3+:SO4 2--Molar concentration rate be 1.04:1:2.03;
S3:Add after polyaluminium sulfate, coacervation soda alum, be then filtered to remove miscellaneous into step S2 soda alum solution
Matter, gained clear liquid is cooled to 7 DEG C, then in the case where pressure is 0.86MPa, and it is 50% that soda alum is depressed into moisture content, obtains filter cake
Thick soda alum;
S4:By in the water of the weight such as thick soda alum input made from step S3, it is heated up to 86 DEG C and stirs make thick soda alum
After being completely dissolved, add after polyaluminium sulfate, coacervation soda alum, impurity then removed again, 7 DEG C are cooled to gained clear liquid,
Then in the case where pressure is 0.86MPa, it is 50% that soda alum is depressed into moisture content, obtains soda alum;
S5:Soda alum made from step S4 is put into the centrifuge that rotating speed is 4500r/min and removes moisture, that is, is made pure
Net soda alum.
Comparative example 1-3, using " a kind of utilization atlapulgite spent acid mother liquor prepares the method (publication number of alum:
CN105271342A the embodiment 1-3 methods in) " prepare alum.
Alum purity in embodiment and comparative example, it increase rate result must be measured see the table below, be obtained wherein setting in comparative example by alum
It is 0 to measure increase rate, and other must measure increase rate in contrast.
As seen from the above table, the alum purity that activated clay production spent acid of the present invention is prepared obtained by the method for alum reaches
More than 99.85%, the amount of obtaining increase rate reaches more than 16.89%, higher than prior art, it is seen that alum made from present invention process
Not only purity is high and yield is also high.
Embodiments of the invention are the foregoing is only, are not intended to limit the invention, it is all in the spirit and principles in the present invention
Interior made any modification, equivalent substitution and improvements etc., should be included in the scope of the protection.
Claims (10)
1. a kind of method that activated clay production spent acid prepares alum, it is characterised in that:Comprise the following steps:
S1:Mixed using activated clay production spent acid with bentonite, the aluminum sulfate in bentonite is dissolved in production spent acid, then
The activated clay production spent acid circulation for increasing sulfuric acid aluminum concentration is mixed with the bentonite newly added, until being dissolved in production spent acid
Aluminum sulfate reaches saturation;
S2:Aluminum sulfate made from step S1 is reached into the production spent acid temperature control of saturation at 86-89 DEG C, pH value is controlled in 4.2-
4.5, add ammonium sulfate or potassium sulfate, then or sodium sulphate reaction generation alum;
S3:Added into step S2 alum solution after flocculant, coacervation alum, be then filtered to remove impurity, gained clear liquid is cold
But crystallize, then press filtration obtains the thick alum of filter cake;
S4:86-89 DEG C will be heated up to and stirred to make after thick alum is completely dissolved in thick alum input water made from step S3, plus
Enter after flocculant, coacervation alum, impurity is then removed again, to gained clear liquid crystallisation by cooling again, then press filtration obtains alum;
S5:Alum made from step S4 is put into centrifuge and removes moisture, that is, pure alum is made.
2. the method that activated clay production spent acid according to claim 1 prepares alum, it is characterised in that followed in step S1
Ring is 3-4 using the number of times of spent acid, and the temperature for controlling to dissolve aluminum sulfate is 96-99 DEG C.
3. the method that activated clay production spent acid according to claim 1 prepares alum, it is characterised in that living in step S2
Property carclazyte produce spent acid temperature control at 87 DEG C, pH value control 4.4.
4. the method that activated clay production spent acid according to claim 1 prepares alum, it is characterised in that pH in step S2
The method that value is controlled is:Ammonium hydrogen carbonate is added when pH value is less than 4.2;When pH value is more than 4.5, addition pH value is less than 2.5 work
Property carclazyte production spent acid.
5. the method that activated clay production spent acid according to claim 1 prepares alum, it is characterised in that in step S2,
When adding ammonium sulfate, the amount of the ammonium sulfate is to make NH in alum4 +:Al3+:SO4 2-Molar concentration rate be 1-1.03:1:
2.01-2.04;When adding potassium sulfate, the amount of the potassium sulfate is to make K in alum+:Al3+:SO4 2-Molar concentration rate be 1.01-
1.02:1:2.02-2.03;When adding sodium sulphate, the amount of the sodium sulphate is to make Na in alum+:Al3+:SO4 2--Molar concentration
Than for 1.02-1.04:1:2.01-2.03.
6. the method that activated clay production spent acid according to claim 1 prepares alum, it is characterised in that step S3 and S4
Described in flocculant be polyaluminium sulfate.
7. the method that activated clay production spent acid according to claim 1 prepares alum, it is characterised in that step S3 and S4
The temperature of middle clear liquid crystallisation by cooling is less than 10 DEG C.
8. the method that activated clay production spent acid according to claim 1 prepares alum, it is characterised in that step S3 and S4
The pressure of middle press filtration is 0.8-0.95MPa, and alum is depressed into moisture content for 46%-50%.
9. the method that activated clay production spent acid according to claim 1 prepares alum, it is characterised in that add in step S4
Water is equal to the weight of thick alum.
10. the method that activated clay production spent acid according to claim 1 prepares alum, it is characterised in that in step S5
The rotating speed of centrifuge is 4000-5000r/min.
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CN109279636A (en) * | 2018-10-30 | 2019-01-29 | 黄山市白岳活性白土有限公司 | A kind of production method of aluminum sulfate |
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CN104477960A (en) * | 2014-12-10 | 2015-04-01 | 兴安宸亿工贸有限公司 | Method for producing potassium alum |
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