CN1515494A - Production method of crystal alum - Google Patents
Production method of crystal alum Download PDFInfo
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- CN1515494A CN1515494A CNA031126138A CN03112613A CN1515494A CN 1515494 A CN1515494 A CN 1515494A CN A031126138 A CNA031126138 A CN A031126138A CN 03112613 A CN03112613 A CN 03112613A CN 1515494 A CN1515494 A CN 1515494A
- Authority
- CN
- China
- Prior art keywords
- alum
- acid
- potassium
- ammonium
- crystal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000013078 crystal Substances 0.000 title claims abstract description 17
- 229940037003 alum Drugs 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000002253 acid Substances 0.000 claims abstract description 26
- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 claims abstract description 24
- LCQXXBOSCBRNNT-UHFFFAOYSA-K ammonium aluminium sulfate Chemical compound [NH4+].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O LCQXXBOSCBRNNT-UHFFFAOYSA-K 0.000 claims abstract description 20
- 235000011126 aluminium potassium sulphate Nutrition 0.000 claims abstract description 13
- 229940050271 potassium alum Drugs 0.000 claims abstract description 13
- 235000011124 aluminium ammonium sulphate Nutrition 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 229910000343 potassium bisulfate Inorganic materials 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000002893 slag Substances 0.000 claims description 14
- JTNCEQNHURODLX-UHFFFAOYSA-N 2-phenylethanimidamide Chemical compound NC(=N)CC1=CC=CC=C1 JTNCEQNHURODLX-UHFFFAOYSA-N 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 claims description 8
- 239000004576 sand Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 4
- 229940103272 aluminum potassium sulfate Drugs 0.000 claims description 3
- 239000002440 industrial waste Substances 0.000 claims description 3
- HSEYYGFJBLWFGD-UHFFFAOYSA-N 4-methylsulfanyl-2-[(2-methylsulfanylpyridine-3-carbonyl)amino]butanoic acid Chemical compound CSCCC(C(O)=O)NC(=O)C1=CC=CN=C1SC HSEYYGFJBLWFGD-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 abstract description 3
- WWILHZQYNPQALT-UHFFFAOYSA-N 2-methyl-2-morpholin-4-ylpropanal Chemical compound O=CC(C)(C)N1CCOCC1 WWILHZQYNPQALT-UHFFFAOYSA-N 0.000 abstract 1
- CHKVPAROMQMJNQ-UHFFFAOYSA-M potassium bisulfate Chemical compound [K+].OS([O-])(=O)=O CHKVPAROMQMJNQ-UHFFFAOYSA-M 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 6
- 229910052934 alunite Inorganic materials 0.000 description 6
- 239000010424 alunite Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- KPZTWMNLAFDTGF-UHFFFAOYSA-D trialuminum;potassium;hexahydroxide;disulfate Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Al+3].[Al+3].[Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O KPZTWMNLAFDTGF-UHFFFAOYSA-D 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 239000001103 potassium chloride Substances 0.000 description 3
- 235000011164 potassium chloride Nutrition 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 2
- 235000011130 ammonium sulphate Nutrition 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- 235000005273 Canna coccinea Nutrition 0.000 description 1
- 240000008555 Canna flaccida Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- VKUBYCRSYPYMLG-UHFFFAOYSA-M potassium hydrogen sulfate hydrochloride Chemical compound Cl.[K+].OS([O-])(=O)=O VKUBYCRSYPYMLG-UHFFFAOYSA-M 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The production method of crystal alum includes the following steps: placing the roasted alumina-contained raw material into a large-type acid-resisting container, adding sulfuric acid and hydrogen sulfate (when it is used for producing potassium alum, adding potassium hydrogen sulfate and when it is used for producing ammonium alum, adding ammonium hydrogen sulfate), fully reacting to obtain anhydrous potassium aluminium sulfate or anhydrous ammonium aluminium sulfate, adding proper quantity of water to make it be crystallized, introducing steam to heat and dissolve, separating liquid and solid, removing solid residue, recrystallizing, taking crystal potassium alum or ammonium alum, the placing the residual solution into the large-type acid-resistant container for recovery and utilization.
Description
The technical field is as follows:
the invention relates to a method for producing crystal alum, belonging to the field of comprehensive utilization of non-metallic ore and slag.
Background art:
as the workers in China know the technology of alum for a long time, alunite (Alumstone) innature can be classified into potassium alunite (Kalialunite) according to chemical components, which is an important raw material for producing potassium alum (aluminum potassium sulfate) and ammonium alum (aluminum ammonium sulfate). The Anhui Lujiang and Zhejiang canna alum ore has representativeness in China, is produced by a traditional old method for many years, has high consumption, high cost and serious loss, and the discarded slag is not recycled, so that the discarded slag of Anhui Lujiang can reach more than three hundred thousand tons, and can be accumulated like a mountain, thereby becoming a difficult problem of three-waste treatment and comprehensive utilization. Although we have searched for it, no data for solving this problem has been found.
The invention content is as follows:
the technical problem to be solved by the invention is as follows: fully utilizes the alum sand (industrial waste residue) and increases the yield of potassium alum or ammonium alum.
The technical scheme for solving the technical problems is as follows:
a method for producing crystal alum is characterized in that ore or slag is crushed to a diameter less than 10cm, raw materials or industrial waste residues (alum sand) which are roasted at 480-500 ℃ and contain alumina are placed into a large acid-resistant container, hydrogen sulfate is added into the large acid-resistant container, potassium bisulfate is added when producing the potassium alum, sulfuric acid and potassium chloride can be used for reacting in a small acid-resistant container, generated hydrogen chloride gas is absorbed and removed, and then the obtained potassium bisulfate and redundant sulfuric acid are placed into the large acid-resistant container; when the ammonium alum is produced, ammonium bisulfate is added, sulfuric acid and ammonium sulfate can be used for reaction in a smaller acid-resistant container, the obtained ammonium bisulfate and redundant sulfuric acid are placed into a large acid-resistant container, 92-98% of sulfuric acid is added into the large acid-resistant container, all components in the large acid-resistant container are fully reacted to generate anhydrous potassium aluminum sulfate or anhydrous ammonium aluminum sulfate, proper water is added into the large acid-resistant container to crystallize the anhydrous potassium aluminum sulfate or anhydrous ammonium aluminum sulfate, then steam with the temperature of 80-95 ℃ is introduced into the large acid-resistant container to be heated and dissolved, liquid and solid are separated, solid residues are removed, recrystallization is carried out, the crystalline potassium alum or the crystalline ammonium alum can be taken out, and the solution after taking out the crystals is placed into the large acid-resistant container again to be recycled.
The alumina content in the ore is preferably more than 20%; the content of alumina in the slag is preferably more than 10%; the sulfuric acid used in the above step is preferably 95%.
The chemical reaction formula of the potassium sulfate monochloride reaction to generate the potassium bisulfate is as follows:
in the formula, HCL can be absorbed and used as a byproduct. The chemical reaction formula of the reaction of sulfuric acid and ammonium sulfate to generate ammonium bisulfate is as follows:
after potassium bisulfate or ammonium bisulfate is generated, the mixture is placed into a large acid-proof container, and then the mixture can react with alumina at normal temperature in sulfuric acid solution, the reaction product is anhydrous potassium aluminum sulfate or anhydrous ammonium aluminum sulfate, and the chemical reaction formula is as follows:
the product purity can be improved by introducing steam to heat and dissolve the crystals, removing solid residues (mainly silica sand) and recrystallizing. Separating out the crystal after recrystallization, putting the liquid into a large acid-resistant container, and recycling the liquid to improve the yield.
The invention has the following advantages: (a) because the bisulfate is added, the alumina in the ore or the slag can be fully utilized, and the yield and the quality of the potassium alum or the ammonium alum are improved; (b) the slag piled in the mine area like the mountain is treated and converted into potassium alum or ammonium alum, so that the waste is changed into valuable and the comprehensive utilization is realized; (c) the yield and the quality are improved, the cost is reduced, and a batch of closed factories and mines can be saved; (d) reduces waste residue and pollution, and is beneficial to environmental protection.
Detailed description of the preferred embodiments
FIG. 1 is a block diagram of a potassium alum production process
FIG. 2 is a block diagram of the production process of ammonium alum
Example 1
Taking 15 tons of potassium alunite slag with the alumina content of 10 percent, and putting the slag into a large acid-resistant container; adding 2.5 tons of 95 percent sulfuric acid into 2 tons of industrial potassium chloride in a small acid-resistant container, absorbing and removing generated hydrogen chloride gas, putting the obtained potassium bisulfate and redundant sulfuric acid into a large acid-resistant container, supplementing 2.75 tons of 95 percent sulfuric acid, adding a proper amount of water for weathering at normal temperature after the potassium bisulfate is fully reacted to form potassium aluminum sulfate, introducing steam, heating to 95 ℃ for dissolving, separating liquid from solid residues, removing the solid residues, wherein the solid residues are mainly silica sand, recrystallizing the obtained liquid, and taking out the liquid to obtain a crystal potassium alum product. The liquid after taking out the crystal can be put into a large acid-proof container again, so that the recovered liquid can be reused, thereby improving the yield. The whole production process takes about four months.
Example 2
Taking 15 tons of potassium alunite slag with the alumina content of 10 percent, and putting the slag into a large acid-resistant container; taking 2 tons of industrial potassium chloride, adding 2.5 tons of 98 percent sulfuric acid into a small acid-resistant container to generate hydrogen chloride, absorbing and removing, placing the obtained potassium bisulfate and redundant sulfuric acid into a large acid-resistant container, and supplementing 2.75 tons of 98 percent sulfuric acid; after the aluminum potassium sulfate is fully reacted, a proper amount of water is added for weathering at normal temperature, steam is introduced, and the mixture is heated to 98 ℃ for dissolution, and the following steps are the same as the example 1, so that the crystal potassium alum product is obtained.
Example 3
Taking 15 tons of ammonium alunite slag with the alumina content of 10 percent, putting the ammonium alunite slag into a large acid-resistant container, and adding 2.04 tons of 90 percent sulfuric acid; the obtained ammonium bisulfate and the redundant sulfuric acid are also placed into a large acid-resistant container, 2.55 tons of 90 percent sulfuric acid is added, after the ammonium bisulfate is fully reacted to form ammonium aluminum sulfate, a proper amount of water is added for weathering at normal temperature, steam is introduced, and the mixture is heated to 80 ℃ for dissolution, and the following steps are the same as the example 1, so that the crystal ammonium alum product is obtained.
Claims (1)
1. A method for producing crystal alum is characterized in that:
(1) crushing the ore or the slag until the diameter is less than 10 cm;
(2) placing the alumina-containing raw material roasted at 480-500 ℃ or industrial waste residue (alum sand) into a large acid-resistant container;
(3) reacting potassium bisulfate or ammonium bisulfate with sulfuric acid in another smaller acid-proof container, absorbing and removing generated hydrogen chloride, and then putting the obtained potassium bisulfate or ammonium bisulfate and redundant sulfuric acid into a large acid-proof container;
(4) adding 90-98% of sulfuric acid into the large acid-resistant container;
(5) fully reacting the components in the large acid-proof container to generate anhydrous aluminum potassium sulfate or anhydrous aluminum ammonium sulfate;
(6) adding a proper amount of water into the large acid-resistant container to weathered and crystallize the large acid-resistant container;
(7) introducing steam into the large acid-proof container and heating to 80-95 ℃ to dissolve the steam;
(8) separating the liquid from the solid and removing solid residues;
(9) and recrystallizing;
(10) taking out the crystal potassium alum or the crystal ammonium alum;
(11) taking out the solution of the crystal and putting the solution into the large acid-resistant container for recycling;
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031126138A CN1515494A (en) | 2003-01-03 | 2003-01-03 | Production method of crystal alum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031126138A CN1515494A (en) | 2003-01-03 | 2003-01-03 | Production method of crystal alum |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1515494A true CN1515494A (en) | 2004-07-28 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA031126138A Pending CN1515494A (en) | 2003-01-03 | 2003-01-03 | Production method of crystal alum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1515494A (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| RU2421400C1 (en) * | 2009-10-23 | 2011-06-20 | Учреждение Российской академии наук Институт химии и технологии редких элементов и минерального сырья им. И.В. Тананаева Кольского научного центра РАН (ИХТРЭМС КНЦ РАН) | Method of producing alumosilicic coagulant-flocculant |
| CN102351227A (en) * | 2011-09-26 | 2012-02-15 | 西安航天华威化工生物工程有限公司 | Method for extracting aluminum oxide from fly ash by one-step process |
| CN102424391A (en) * | 2011-09-01 | 2012-04-25 | 东北大学 | A method for comprehensive utilization of aluminum-containing materials |
| CN102432052A (en) * | 2011-09-26 | 2012-05-02 | 西安航天华威化工生物工程有限公司 | Method for extracting aluminum oxide from fly ash by using potassium sulfate |
| CN102517461A (en) * | 2011-12-16 | 2012-06-27 | 紫金矿业集团股份有限公司 | Method for recycling gallium in alunite concentrate |
| CN103979592A (en) * | 2014-04-16 | 2014-08-13 | 广西冶金研究院 | Method for recovering aluminum from alumina production waste red mud |
| CN104445330A (en) * | 2014-12-10 | 2015-03-25 | 兴安宸亿工贸有限公司 | Method for producing aluminum ammonium sulfate crystal |
| CN104534452A (en) * | 2014-12-16 | 2015-04-22 | 兴安宸亿工贸有限公司 | Device and method both for recycling steam residual heat in production of alums |
| CN105502455A (en) * | 2015-12-16 | 2016-04-20 | 广西南宁胜祺安科技开发有限公司 | Method for preparing ammonium alum from acid wastewater of kaolin mineral separation |
| CN106892445A (en) * | 2017-05-02 | 2017-06-27 | 常熟理工学院 | The method that the dead catalyst containing aluminium produced in being produced by petroleum chemical enterprise prepares potassium alum |
| CN108342777A (en) * | 2018-03-06 | 2018-07-31 | 宝鸡文理学院 | A kind of preparation method of the crystalline material of sol-gel method synthesis |
-
2003
- 2003-01-03 CN CNA031126138A patent/CN1515494A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| RU2421400C1 (en) * | 2009-10-23 | 2011-06-20 | Учреждение Российской академии наук Институт химии и технологии редких элементов и минерального сырья им. И.В. Тананаева Кольского научного центра РАН (ИХТРЭМС КНЦ РАН) | Method of producing alumosilicic coagulant-flocculant |
| CN102424391A (en) * | 2011-09-01 | 2012-04-25 | 东北大学 | A method for comprehensive utilization of aluminum-containing materials |
| CN102432052B (en) * | 2011-09-26 | 2015-05-13 | 西安航天华威化工生物工程有限公司 | Method for extracting aluminum oxide from pulverized fuel ash by using potassium sulfate |
| CN102351227A (en) * | 2011-09-26 | 2012-02-15 | 西安航天华威化工生物工程有限公司 | Method for extracting aluminum oxide from fly ash by one-step process |
| CN102432052A (en) * | 2011-09-26 | 2012-05-02 | 西安航天华威化工生物工程有限公司 | Method for extracting aluminum oxide from fly ash by using potassium sulfate |
| CN102351227B (en) * | 2011-09-26 | 2013-08-21 | 西安航天华威化工生物工程有限公司 | Method for extracting aluminum oxide from fly ash by one-step process |
| CN102517461A (en) * | 2011-12-16 | 2012-06-27 | 紫金矿业集团股份有限公司 | Method for recycling gallium in alunite concentrate |
| CN103979592A (en) * | 2014-04-16 | 2014-08-13 | 广西冶金研究院 | Method for recovering aluminum from alumina production waste red mud |
| CN103979592B (en) * | 2014-04-16 | 2016-02-10 | 广西冶金研究院 | A kind of method reclaiming aluminium from alumina producing waste red mud |
| CN104445330A (en) * | 2014-12-10 | 2015-03-25 | 兴安宸亿工贸有限公司 | Method for producing aluminum ammonium sulfate crystal |
| CN104445330B (en) * | 2014-12-10 | 2016-05-18 | 兴安宸亿工贸有限公司 | A kind of production method of ammonia-alum |
| CN104534452A (en) * | 2014-12-16 | 2015-04-22 | 兴安宸亿工贸有限公司 | Device and method both for recycling steam residual heat in production of alums |
| CN105502455A (en) * | 2015-12-16 | 2016-04-20 | 广西南宁胜祺安科技开发有限公司 | Method for preparing ammonium alum from acid wastewater of kaolin mineral separation |
| CN106892445A (en) * | 2017-05-02 | 2017-06-27 | 常熟理工学院 | The method that the dead catalyst containing aluminium produced in being produced by petroleum chemical enterprise prepares potassium alum |
| CN108342777A (en) * | 2018-03-06 | 2018-07-31 | 宝鸡文理学院 | A kind of preparation method of the crystalline material of sol-gel method synthesis |
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