CN1275874C - Preparation method of polyaluminum chloride water purifying agent - Google Patents
Preparation method of polyaluminum chloride water purifying agent Download PDFInfo
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- CN1275874C CN1275874C CNB2003101104353A CN200310110435A CN1275874C CN 1275874 C CN1275874 C CN 1275874C CN B2003101104353 A CNB2003101104353 A CN B2003101104353A CN 200310110435 A CN200310110435 A CN 200310110435A CN 1275874 C CN1275874 C CN 1275874C
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- purifying agent
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 7
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000012629 purifying agent Substances 0.000 title abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 33
- 239000012535 impurity Substances 0.000 claims abstract description 25
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 21
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 21
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000006229 carbon black Substances 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 9
- 239000007791 liquid phase Substances 0.000 claims abstract description 9
- 239000007790 solid phase Substances 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 25
- 238000000746 purification Methods 0.000 claims description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 24
- 235000011167 hydrochloric acid Nutrition 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 14
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- 238000000137 annealing Methods 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 235000006408 oxalic acid Nutrition 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 8
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 8
- 239000008399 tap water Substances 0.000 claims description 8
- 235000020679 tap water Nutrition 0.000 claims description 8
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 239000000376 reactant Substances 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 238000000605 extraction Methods 0.000 abstract description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 4
- 239000011707 mineral Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000010802 sludge Substances 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 2
- 239000000945 filler Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 239000000706 filtrate Substances 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 1
- 238000001694 spray drying Methods 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000004411 aluminium Substances 0.000 description 4
- 239000003245 coal Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
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- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention relates to a method for preparing a polyaluminium chloride water purifying agent by using kaolin minerals. The method is characterized in that firstly, kaolin crude ore is dried; then carrying out calcination treatment: calcining at 650-700 deg.c and adding water to compound slurry; then aging for 2 hours, centrifugally separating, and reacting for 3 hours at 90-95 ℃ in a reaction vessel; next, the reaction was centrifuged again: concentrating the filtrate to obtain liquid phase purifying agent or spray drying to obtain solid phase purifying agent; and removing impurities from the filter residue for the second time, centrifuging and drying to obtain the white carbon black. The polymerized aluminum oxide water purifying agent prepared by the invention has the aluminum extraction rate of 95 percent; the average particle size of the water purifying agent is less than 40 nm; the water purifying agent has obvious water treatment effect, the average dosage is reduced by 40 percent, and the sludge settling rate is improved by more than 50 percent; the byproduct white carbon black is used as high-quality filler; the preparation method is simple, convenient and effective, low in production cost and wide in market prospect.
Description
Technical field:
The present invention relates to the environment functional material field, is to utilize kaolin mineral to prepare the method for polyaluminium chloride water purification agent specifically.
Background technology:
Nonmetalliferous ores such as present domestic main employing coal gangue are the feedstock production polyaluminium chloride water purification agent, but the extraction yield of aluminium is low, the clean water treatment weak effect, and the flocculation time of response is long, and the sewage settling time reaches 3～4 hours.
Summary of the invention:
The objective of the invention is to overcome the weak point of prior art, and providing a kind of kaolin mineral that utilizes high yield to prepare the method for polyaluminium chloride water purification agent, this method is not only simple and effective, and the extraction yield height of aluminium, use this water purification agent obvious to the water treatment effect, sludge settling speed improves.
Technical scheme of the present invention is:
At first the kaolin raw ore is carried out drying treatment: drying temperature is 200 ℃, 2 hours time of drying;
Carry out calcination processing then: 650 ℃～700 ℃ of calcining temperatures, 1～2 hour after annealing time of calcining;
Join slurry again: take by weighing the kaolin raw ore and place in the reacting appliance for 200 kilograms, add 200 liters～240 liters tap water and be made into slurries;
Then use 36～50 gram Sodium hexametaphosphate 99s to carry out dispersion treatment, carry out the removing impurities by oxidation processing with the oxalic acid of 60 grams and the concentrated hydrochloric acid of 32 grams, reducing removal of impurities with the V-Brite Bs of 100 grams as vat powder handles, it is fully stirred 20 minutes after-filtration, add the 240 premium on currency pulp that stirs again;
And then ageing was handled 2 hours, after the centrifugation, added 200 premium on currency in filter residue, 215～218 kilograms of concentrated hydrochloric acids, and 90～95 ℃ were reacted 3 hours down in reaction vessel;
Next, centrifugal treating reactant again: concentrating filter liquor after half liquid phase water purification agent or the spray-dried solid phase water purification agent that obtains; Filter residue is white carbon black then through the secondary removal of impurities after centrifugal treating and the drying.
The preparation method of polymerization oxidation aluminium water purifying agent of the present invention, its advantage and positively effect are embodied in:
The extraction rate reached to 95% of aluminium; The mean particle size of water purification agent is less than 40nm; Water purification agent is better than national standard after adjusting basicity; Use this water purification agent obvious to the water treatment effect, average consumption reduces 40%, and sludge settling speed improves more than 50%; Its byproduct white carbon black has fully been realized the comprehensive utilization of resource then as high quality filler; This preparation method is simple and effective, makes full use of the kaolin mineral of high yield, and production cost is low, and market outlook are wide.
Embodiment:
Be described further below in conjunction with embodiment.
Embodiment one:
At first adopt loft drier to carry out drying treatment to the kaolin raw ore, drying temperature is 200 ℃, and be 2 hours time of drying; Adopt muffle furnace to carry out calcination processing at 650 ℃ then, annealing time is 1 hour; Take by weighing the kaolin raw ore of handling well again and place in the reacting appliance for 200 kilograms, add 240 liters of tap water and be made into slurries; Then use 36 gram Sodium hexametaphosphate 99s to carry out dispersion treatment, carry out the removing impurities by oxidation processing with the oxalic acid of 60 grams and the concentrated hydrochloric acid of 32 grams, reduce removal of impurities with the V-Brite Bs of 100 grams as vat powder and handle, mixture stirs 20 minutes after-filtration, adds the 240L water pulp that stirs again; And then ageing was handled 2 hours, after the centrifugation, added 200 premium on currency, 218 kilograms of concentrated hydrochloric acids in filter residue, and 90 ℃ were reacted 3 hours in reaction vessel; Recentrifuge processing reaction thing: concentrating filter liquor after half liquid phase water purification agent or spray-dried solid phase water purification agent; Filter residue is white carbon black after secondary removal of impurities, centrifugal treating and drying.
Embodiment two:
At first adopt loft drier to carry out drying treatment to the kaolin raw ore, drying temperature is 200 ℃, and be 2 hours time of drying; Adopt muffle furnace to carry out calcination processing at 650 ℃ then, annealing time is 2 hours; Take by weighing the kaolin raw ore of handling well again and place in the reacting appliance for 200 kilograms, add 240 liters of tap water and be made into slurries; Then use 36 gram Sodium hexametaphosphate 99s to carry out dispersion treatment, carry out the removing impurities by oxidation processing with the oxalic acid of 60 grams and the concentrated hydrochloric acid of 32 grams, reduce removal of impurities with the V-Brite Bs of 100 grams as vat powder and handle, mixture stirs 20 minutes after-filtration, adds the 240L water pulp that stirs again; And then ageing was handled 2 hours, after the centrifugation, added 200 premium on currency, 218 kilograms of concentrated hydrochloric acids in filter residue, and 90 ℃ were reacted 3 hours in reaction vessel; Recentrifuge processing reaction thing: concentrating filter liquor after half liquid phase water purification agent or spray-dried solid phase water purification agent; Filter residue is white carbon black after secondary removal of impurities, centrifugal treating and drying.
Embodiment three:
At first adopt loft drier to carry out drying treatment to the kaolin raw ore, drying temperature is 200 ℃, and be 2 hours time of drying, adopts muffle furnace to carry out calcination processing at 700 ℃ then, and annealing time is 2 hours; Take by weighing the kaolin raw ore of handling well again and place in the reacting appliance for 200 kilograms, add 240 liters of tap water and be made into slurries; Then use 36 gram Sodium hexametaphosphate 99s to carry out dispersion treatment, carry out the removing impurities by oxidation processing with the oxalic acid of 60 grams and the concentrated hydrochloric acid of 32 grams, reduce removal of impurities with the V-Brite Bs of 100 grams as vat powder and handle, mixture stirs 20 minutes after-filtration, adds the 240L water pulp that stirs again; And then ageing was handled 2 hours, after the centrifugation, added 200 premium on currency, 218 kilograms of concentrated hydrochloric acids in filter residue, and 90 ℃ were reacted 3 hours in reaction vessel; Recentrifuge processing reaction thing: concentrating filter liquor after half liquid phase water purification agent or spray-dried solid phase water purification agent; Filter residue is white carbon black after secondary removal of impurities, centrifugal treating and drying.
Embodiment four:
At first adopt loft drier to carry out drying treatment to the kaolin raw ore, drying temperature is 200 ℃, and be 2 hours time of drying; Adopt muffle furnace to carry out calcination processing at 650 ℃ then, annealing time is 1 hour; Then take by weighing the kaolin raw ore of handling well and place in the reacting appliance for 200 kilograms, add 240 liters of tap water and be made into slurries; Then use 50 gram Sodium hexametaphosphate 99s to carry out dispersion treatment, carry out the removing impurities by oxidation processing with the oxalic acid of 60 grams and the concentrated hydrochloric acid of 32 grams, reduce removal of impurities with the V-Brite Bs of 100 grams as vat powder and handle, mixture stirs 20 minutes after-filtration, adds the 240L water pulp that stirs again; And then ageing was handled 2 hours, after the centrifugation, added 200 premium on currency, 218 kilograms of concentrated hydrochloric acids in filter residue, and 90 ℃ were reacted 3 hours in reaction vessel; Recentrifuge processing reaction thing: concentrating filter liquor after half liquid phase water purification agent or spray-dried solid phase water purification agent; Filter residue is white carbon black after secondary removal of impurities, centrifugal treating and drying.
Embodiment five:
At first adopt loft drier to carry out drying treatment to the kaolin raw ore, drying temperature is 200 ℃, and be 2 hours time of drying; Adopt muffle furnace to carry out calcination processing at 650 ℃ then, annealing time is 1 hour; Take by weighing the kaolin raw ore of handling well again and place in the reacting appliance for 200 kilograms, add 240 liters of tap water and be made into slurries; Then use 36 gram Sodium hexametaphosphate 99s to carry out dispersion treatment, carry out the removing impurities by oxidation processing with the oxalic acid of 60 grams and the concentrated hydrochloric acid of 32 grams, reduce removal of impurities with the V-Brite Bs of 100 grams as vat powder and handle, mixture stirs 20 minutes after-filtration, adds the 240L water pulp that stirs again; And then ageing was handled 2 hours, after the centrifugation, added 200 premium on currency, 218 kilograms of concentrated hydrochloric acids in filter residue, and 95 ℃ were reacted 3 hours in reaction vessel; Recentrifuge processing reaction thing: concentrating filter liquor after half liquid phase water purification agent or spray-dried solid phase water purification agent; Filter residue is white carbon black after secondary removal of impurities, centrifugal treating and drying.
Embodiment six:
At first adopt loft drier to carry out drying treatment to the kaolin raw ore, drying temperature is 200 ℃, and be 2 hours time of drying; Adopt muffle furnace to carry out calcination processing at 650 ℃ then, annealing time is 1 hour; Take by weighing the kaolin raw ore of handling well again and place in the reacting appliance for 200 kilograms, add 240 liters of tap water and be made into slurries; Then use 36 gram Sodium hexametaphosphate 99s to carry out dispersion treatment, carry out the removing impurities by oxidation processing with the oxalic acid of 60 grams and the concentrated hydrochloric acid of 32 grams, reduce removal of impurities with the V-Brite Bs of 100 grams as vat powder and handle, mixture stirs 20 minutes after-filtration, adds the 240L water pulp that stirs again; And then ageing was handled 2 hours, after the centrifugation, added 200 premium on currency, 218 kilograms of concentrated hydrochloric acids in filter residue, and 90 ℃ were reacted 3 hours in 50 kPas pressurized vessel; Recentrifuge processing reaction thing: concentrating filter liquor after half liquid phase water purification agent or spray-dried solid phase water purification agent; Filter residue is white carbon black after secondary removal of impurities, centrifugal treating and drying.
Claims (1)
1. the preparation method of a polyaluminium chloride water purification agent is characterized in that:
At first the kaolin raw ore is carried out drying treatment: drying temperature is 200 ℃, 2 hours time of drying;
Carry out calcination processing then: 650 ℃～700 ℃ of calcining temperatures, 1～2 hour after annealing time of calcining;
Join slurry again: take by weighing the kaolin raw ore and place in the reacting appliance for 200 kilograms, add 200 liters～240 liters tap water and be made into slurries;
Then use 36～50 gram Sodium hexametaphosphate 99s to carry out dispersion treatment, carry out the removing impurities by oxidation processing with the oxalic acid of 60 grams and the concentrated hydrochloric acid of 32 grams, reducing removal of impurities with the V-Brite Bs of 100 grams as vat powder handles, it is fully stirred 20 minutes after-filtration, add the 240 premium on currency pulp that stirs again;
And then ageing was handled 2 hours, after the centrifugation, added 200 premium on currency in filter residue, 215～218 kilograms of concentrated hydrochloric acids, and 90～95 ℃ were reacted 3 hours down in reaction vessel;
Next, centrifugal treating reactant again: concentrating filter liquor after half liquid phase water purification agent or the spray-dried solid phase water purification agent that obtains; Filter residue is white carbon black then through the secondary removal of impurities after centrifugal treating and the drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101104353A CN1275874C (en) | 2003-10-21 | 2003-10-21 | Preparation method of polyaluminum chloride water purifying agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101104353A CN1275874C (en) | 2003-10-21 | 2003-10-21 | Preparation method of polyaluminum chloride water purifying agent |
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| Publication Number | Publication Date |
|---|---|
| CN1609012A CN1609012A (en) | 2005-04-27 |
| CN1275874C true CN1275874C (en) | 2006-09-20 |
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| CNB2003101104353A Expired - Fee Related CN1275874C (en) | 2003-10-21 | 2003-10-21 | Preparation method of polyaluminum chloride water purifying agent |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1313387C (en) * | 2005-09-15 | 2007-05-02 | 丁杰 | Polymeric bisgallic acid alumnium and its preparation method |
| CN101905898B (en) * | 2010-08-03 | 2012-06-27 | 常州友邦净水材料有限公司 | Utilization method for polymeric aluminium reaction residues |
| CN102198956B (en) * | 2011-04-07 | 2013-01-23 | 付克明 | New process for producing aluminum and silicon chemical products by low-grade bauxite or kaolin raw material based on alkaline method |
| CN103482666A (en) * | 2013-09-07 | 2014-01-01 | 郴州四方立投资有限公司 | Method for preparing polyalumnium chloride water purifying agent by using low-grade kaolin |
| CN105883992A (en) * | 2014-08-29 | 2016-08-24 | 枣庄民兴化工有限公司 | Method for preparing polyaluminum chloride water purifier by utilization of kaolinite |
| CN105129945B (en) * | 2015-09-07 | 2017-05-10 | 广西师范学院 | Production technology for activated soil product for water treatment |
| CN106277007A (en) * | 2016-08-29 | 2017-01-04 | 太仓市新星轻工助剂厂 | A kind of preparation method of aluminium polychlorid |
| CN112250154A (en) * | 2020-10-27 | 2021-01-22 | 马鞍山健鼎化工有限公司 | Preparation method of polyaluminum chloride with high flocculation effect |
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2003
- 2003-10-21 CN CNB2003101104353A patent/CN1275874C/en not_active Expired - Fee Related
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| CN1609012A (en) | 2005-04-27 |
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