CN101279756A - Preparation of polyaluminium sulfate - Google Patents
Preparation of polyaluminium sulfate Download PDFInfo
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- CN101279756A CN101279756A CNA2007100213370A CN200710021337A CN101279756A CN 101279756 A CN101279756 A CN 101279756A CN A2007100213370 A CNA2007100213370 A CN A2007100213370A CN 200710021337 A CN200710021337 A CN 200710021337A CN 101279756 A CN101279756 A CN 101279756A
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- polyaluminium sulfate
- polymerization
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- phosphoric acid
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Abstract
The invention relates to a process for preparing a polymerized aluminum sulfate with high Al2O3 effective content and degree of polymerization and without waste residue in the production process, which is characterized in that the process adopts the mixed reaction of aluminum sulfate, water, phosphoric acid and sodium metaaluminate being present in a weight ratio of 0.8-10.0: 0.00-10.0: 0.01-0.1: 0.10-2.0. Compared with the prior art, the process of the invention has advantages that: the Al2O3 effective content of the prepared product is more than 10 percent, the degree of polymerization is over 45 percent, the product is stable secularly and has no layering, the reaction velocity is fast by using the condensation, the flocculating constituents are compact, the sewage COD and chromaticity removing effects are good and the coagulation effects are superior compared with the polymerized aluminum sulfate, polymerized aluminium chloride and composite polymerized aluminum ferric chloride produced by the prior art. In addition, the process does not adopt basifiers such as a slaked lime and has no three-waste in the production, thereby overcoming the defects of low effective concentration, low degree of polymerization and large amounts of waste residues in the production of the prepared product by adopting the manufacturing technique of the prior art.
Description
Technical field
The present invention relates to a kind of chemistry in water treatment water purification agent polyaluminium sulfate, relate in particular to a kind of Al
2O
3Effective content and polymerization degree height, production process do not have the preparation of polyaluminium sulfate that waste residue produces.
Background technology
Polyaluminium sulfate, it purifies the turbidity removal decolorizing effect and is better than polymerize aluminum chloride and bodied ferric sulfate, is a kind of highly effective inorganic high molecular water purifier.Usually it is synthetic that polyaluminium sulfate production adopted for two steps, earlier prepare Tai-Ace S 150, add basifier (for example white lime, ammonia, carbonate, supercarbonate etc.) again and carry out polymerization and obtain polyaluminium sulfate by aluminum-containing raw material (as bauxitic clay, kaolin, aluminium ash etc.) and sulfuric acid reaction.The polyaluminium sulfate that this method is produced, because of polymerization with not containing effective Al in the basifier
2O
3, effective Al in the gained polyaluminium sulfate like this
2O
3Content is low less than 10%, generally can only reach 5-7%; And the polymerization degree is lower, and the general polymerization degree is below 45%, and product is extremely unstable when the polymerization degree is higher than 45%, hydrolysis reaction takes place easily and layering.Above-mentioned reason causes result of use not ideal enough; Secondly, because of using bauxitic clay, kaolin, aluminium ash, reach raw materials such as white lime in the production, the waste residue generation is big, not only causes environmental pollution, and increases processing cost.
Chinese patent CN91104676.3 discloses a kind of liquid palymeric aluminium sulfate preparation method, with aluminiferous bauxite mine and sulphuric acid soln reaction, prepare certain density aluminum sulfate aqueous solution, under agitation carry out polyreaction with alkaline earth metal compound or ammonia again, polymer material is through solid-liquid separation, remove the vitriol of impurity and alkaline-earth metal, polyaluminium sulfate filtrate.This method is similarly above-mentioned two step method reaction, above-mentioned defective still exists, carry polyaluminium sulfate formation waste residue secretly as the calcium sulfate that main raw material white lime in sulfuric acid insolubles waste residue and the alkaline-earth metal in the bauxitic clay produces, and equally because of not containing Al in alkaline earth metal compound or the ammonia
2O
3Effective constituent, gained polyaluminum sulfate aluminum solutions effective constituents A l
2O
3Percentage composition has only 5-7%.
The disclosed polyaluminium sulfate production technique of Chinese patent CN94116651.1 comprises successively: 1) unslaked lime adds the water reaction, crosses the elimination throw out and gets white lime Ca (OH)
2Slurry, 2) in reactor, add Tai-Ace S 150 and water, be warming up to 60 ℃, stir, all dissolve, make the alum liquor of 30% concentration, 3 until Tai-Ace S 150) with 1) the gained slaked lime slurry adds in the reactor and mixes with Tai-Ace S 150, Ca (OH) wherein
2: Al
2(SO
4)
318H
2O: H
2O (weight)=1: 3: 7 is heated to 60 ℃, and stirring reaction is 1 hour under normal pressure, 4) in above-mentioned reaction solution, add 5 ‰ NaSO of reaction solution gross weight
3, at normal pressure, 50～60 ℃ are stirred after 2～3 hours down and go out still, elimination precipitate colourless transparent liquid polyaluminium sulfate product.Though this technology is by adding NaSO
3Stablizer, instability problem when having overcome high-polymerization degree, but still can't solve the problem that produces waste residue, and obtain the effective constituents A l of product equally
2O
3Percentage composition hangs down at 5-7%.
The disclosed preparation of polyaluminium sulfate of Chinese patent CN200510072367.5 prepares Tai-Ace S 150 with the directly sour molten industrial spent catalyst of sulfuric acid earlier, makes polyaluminium sulfate with Tai-Ace S 150 and aluminium hydroxide polymerization then.This preparation method is to be starting material with the wax catalysis spent catalyst, the source is subjected to great restriction, and waste material produces product foreign matter content height, simultaneously with aluminium hydroxide as polymerizing agent, because the aluminium hydroxide activity is low, so the products obtained therefrom polymerization degree still is lower than 45%.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned prior art, a kind of Al is provided
2O
3The effective content height, polymerization degree height, and do not have the preparation of polyaluminium sulfate that waste residue produces.
The object of the invention realizes that main the improvement is that employing Tai-Ace S 150 is raw material, at phosphoric acid used as stabilizers and sodium metaaluminate polymerization technique, thereby not only can improve Al
2O
3Effective content, and the products obtained therefrom polymerization degree is high and stable, produces no waste residue and produces.Specifically, polyaluminium sulfate preparation of the present invention is characterized in that by Tai-Ace S 150: water: phosphoric acid: sodium metaaluminate, 0.8-10.0: 0.00-10.0: 0.01-0.1 by weight: 0.10-2.0 hybrid reaction.
In the inventive method:
Tai-Ace S 150 mainly provides effective content Al
2O
3, can adopt industrial solid Tai-Ace S 150 or liquid aluminium sulfate, for making it high as far as possible Al is arranged
2O
3Content better is that solid alumina adopts content 〉=15.5%, liquid oxidation aluminium content 〉=7.6%, raw material A l
2O
3The content height helps product A l
2O
3Improve.If adopt liquid aluminium sulfate, then can omit dissolving water.
Phosphoric acid can prevent that as polymerization stabilizer the local excessive polymerization from causing the product instability.In concrete the production, for reducing reaction consumption and reaction volume, a kind of better employing high-concentration phosphoric acid (for example content is more than 85%).
Sodium metaaluminate can improve the polymerization degree mainly as polymerizing agent, contains a certain amount of aluminium because of it simultaneously, can improve effective constituents A l in the products obtained therefrom
2O
3Content.It can adopt commercially available sodium metaaluminate, also can be made by sodium hydroxide and the industrial aluminium hydroxide reaction of sodium al mole ratio 1.05-1.5.The preparation sodium metaaluminate, its naoh concentration better should be more than 30%, and concentration is crossed to hang down and can be caused gained sodium metaaluminate content on the low side, cause the free sodium total content higher, total quantity of alkali consumption is big in can causing producing, and increases cost, and the concentration height also helps and shortens the reaction times.Its content of industrial aluminium hydroxide has no special requirements, but the content height helps improving Al in the sodium metaaluminate
2O
3Content, this is favourable to the present invention.The present invention is a content of effectively controlling free sodium in the sodium metaaluminate, reduces total quantity of alkali consumption, and a kind of being preferably adopted above-mentioned self-control sodium metaaluminate.
Hybrid reaction of the present invention can be carried out in normal temperature, also can suitably heat, and test shows to separate with the interior small piece of land surrounded by water of heating at boiling point and helps accelerating speed of reaction.
The present invention is more preferably a kind of: Tai-Ace S 150: water: phosphoric acid: sodium metaaluminate weight ratio 1.0-8.0: 0.00-8.0: 0.02-0.06: 0.20-1.20.
The inventive method gained polyaluminium sulfate has than prior art: products obtained therefrom effective content height, Al
2O
3Percentage composition is higher than 10%, the polymerization degree height of product, and the polymerization degree is greater than 45%, and long-term stability is not stratified.In addition, the inventive method raw material is easy to get, and because of not adopting basifier such as white lime, no three wastes problem in the production has overcome prior art production technique products obtained therefrom, effective concentration is not high, the polymerization degree is low, produce in the big deficiency of waste residue amount.The inventive method products obtained therefrom has: aggregation speed is fast, and it is closely knit to form flco, and to COD of sewage, chromaticity removing effect is good, and coagulation effect is better than polyaluminium sulfate, polymerize aluminum chloride, the composite polymeric aluminium chloride ferrum that prior art is produced.
Below in conjunction with several embodiments, further specify advantage of the present invention, but can not be interpreted as that the inventive method is restricted by embodiment.
Embodiment
Embodiment 1 (preparation sodium metaaluminate): in reactor, squeeze into 2.0 cubes of water, open and stir, slowly add 1.1 tons of 96% industrial sodium hydroxides again, make dissolution of sodium hydroxide, reactor is warming up to about 75 ℃, progressively add 1.7 tons of 62% industrial aluminium hydroxides again, and open and to be steam heated to about 90 ℃, reaction about 30min that heats up automatically is behind the peak of heating up, again with being steam heated to about 120 ℃, insulation reaction is about 2 hours then, after reaction finishes, opens cooling and is water-cooled to about 90 ℃, through filter press, get 4.8 tons of sodium metaaluminate polymerizing agents.Alumina content is 25.36%, and the sodium al mole ratio is 1.12.
In addition, in above-mentioned sodium al mole ratio 1.05-1.5 scope, the gained sodium metaaluminate can be used for the present invention equally.
Embodiment 2: squeeze into 2 tons of water in reactor, open and stir, slowly add Al
2O
31.7 tons in content 15.8% industrial solid Tai-Ace S 150 makes Tai-Ace S 150 dissolving, adds 40 kilograms of 85% phosphoric acid stabilize agent, open homogenizer again after, be added dropwise to 0.67 ton of embodiment 1 gained sodium metaaluminate polymerizing agent, drip half an hour approximately.Dropwise the back unlatching and be steam heated to about 60 ℃.Digestion is about 2.5 hours under 60 ℃ of temperature, opens cooling again and is water-cooled to about 40 ℃ of blowings.Gained polyaluminium sulfate index is as follows: aluminum oxide 10.54%, the polymerization degree 57.62%, pH3.93, proportion 1.36g/ml.
Embodiment 3: squeeze into 3.7 tons of 7.62% liquid aluminium sulfates in answering still, open homogenizer, 42 kilograms of the phosphoric acid stabilize agent of adding 75% are added dropwise to 0.6 ton of sodium metaaluminate polymerizing agent (sodium metaaluminate of commercial alumina content 38% adds 0.2 ton of dissolving of water for 0.4 ton), drip half an hour approximately.Dropwise the back unlatching and be steam heated to about 70 ℃.Digestion is about 1.5 hours under 70 ℃ of temperature, opens cooling and is water-cooled to about 40 ℃ of blowings.Gained polyaluminium sulfate index is as follows: aluminum oxide 10.21%, the polymerization degree 50.62%, pH3.41, proportion 1.34g/ml.
Embodiment 4: squeeze into 3.7 tons of 7.62% liquid aluminium sulfates in reactor, open homogenizer, add 30 kilograms of 85% phosphoric acid stabilize agent, be added dropwise to 0.55 ton of the sodium metaaluminate polymerizing agent of system among the embodiment 1, drip half an hour approximately.Dropwise the back unlatching and be steam heated to about 80 ℃.Digestion is about 1.0 hours under 80 ℃ of temperature, opens cooling and is water-cooled to about 40 ℃ of blowings.Gained polyaluminium sulfate index is as follows: aluminum oxide 10.35%, the polymerization degree 52.62%, pH3.62, proportion 1.35g/ml.
Comparison test: get behind the former wood pulp biochemistry waste water 1000ml (COD:500,1000 times of colourities) before the dosing, add embodiment 2 gained polyaluminium sulfates respectively, commercially available polyaluminium sulfate, commercially available polymerize aluminum chloride, composite polymeric aluminium chloride ferrum, carry out the coagulation effect simultaneous test, its testing data is seen attached list.From the water outlet effect as can be seen, the removal COD of the inventive method gained polyaluminium sulfate, decoloring ability all is better than other, and it is closely knit than other to form flco.
Use comparative test result
| Sequence number | 1 | 2 | 3 | 4 |
| Name of product | Polyaluminium sulfate of the present invention | Commercially available polyaluminium sulfate | Commercially available polymerize aluminum chloride | The composite polymeric aluminium chloride ferrum |
| Medicament add-on Al 2O 3Meter (mg/L) | 100 | 100 | 100 | 100 |
| Effluent color dilution (doubly) | 52 | 85 | 150 | 90 |
| Water outlet COD (mg/L) | 94 | 111 | 153 | 120 |
| Mud is closely knit | Very closely knit | More closely knit | More closely knit | More closely knit |
| Sludge volume | Few (150ml) | Few (150ml) | In (180ml) | Few (150ml) |
Claims (7)
1. polyaluminium sulfate preparation is characterized in that by Tai-Ace S 150: water: phosphoric acid: sodium metaaluminate, 0.8-10.0: 0.00-10.0: 0.01-0.1 by weight: 0.10-2.0 hybrid reaction.
2. according to the described polyaluminium sulfate preparation of claim 1, it is characterized in that Tai-Ace S 150: water: phosphoric acid: sodium metaaluminate weight ratio 1.0-8.0: 0.00-8.0: 0.02-0.06: 0.20-1.20.
3. according to claim 1 or 2 described polyaluminium sulfate preparations, it is characterized in that said Tai-Ace S 150, solid alumina content 〉=15.5%, liquid oxidation aluminium content 〉=7.6%.
4. according to claim 1 or 2 described polyaluminium sulfate preparations, it is characterized in that said phosphoric acid is the high-concentration phosphoric acid of content 〉=85%.
5. according to claim 1 or 2 described polyaluminium sulfate preparations, it is characterized in that said sodium metaaluminate makes for sodium hydroxide and industrial aluminium hydroxide reaction by sodium al mole ratio 1.05-1.5.
6. according to claim 1 or 2 described polyaluminium sulfate preparations, it is characterized in that hybrid reaction is for heating 40-100 ℃, digestion 0.5-8.0 hour.
7. according to the described polyaluminium sulfate preparation of claim 6, it is characterized in that the digestion temperature is 55-85 ℃, the digestion time is 0.5-3.0 hour.
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|---|---|---|---|
| CN2007100213370A CN101279756B (en) | 2007-04-05 | 2007-04-05 | Preparation of polyaluminium sulfate |
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|---|---|---|---|
| CN2007100213370A CN101279756B (en) | 2007-04-05 | 2007-04-05 | Preparation of polyaluminium sulfate |
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| CN101279756A true CN101279756A (en) | 2008-10-08 |
| CN101279756B CN101279756B (en) | 2012-07-04 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344157A (en) * | 2010-07-30 | 2012-02-08 | 浙江师范大学 | Method for preparing aluminium polychlorid with high content of Al13 |
| CN105712387A (en) * | 2016-03-15 | 2016-06-29 | 北京世纪地和控股有限公司 | Method for preparing aluminum hydroxide sulfate |
| CN106395875A (en) * | 2016-09-14 | 2017-02-15 | 重庆中昆铝业有限公司 | Method for producing polyaluminium sulfate from aluminum profile machining waste liquid |
| CN109224365A (en) * | 2018-08-20 | 2019-01-18 | 长安大学 | A kind of aluminium shape surface processing controlling waste residue method |
| EP3564187A2 (en) | 2018-04-03 | 2019-11-06 | Nikolaos Dailianis | Method and equipment for the recycling of alkaline wastes from aluminum extrusion industries for the production of useful coagulants |
| CN110451844A (en) * | 2019-08-20 | 2019-11-15 | 重庆腾治科技有限公司 | A kind of alkali-free liquid accelerator and preparation method thereof |
| CN112142085A (en) * | 2020-08-04 | 2020-12-29 | 广西锋华环保科技有限公司 | Method for producing polyaluminum sulfate by using aluminum ash |
-
2007
- 2007-04-05 CN CN2007100213370A patent/CN101279756B/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344157A (en) * | 2010-07-30 | 2012-02-08 | 浙江师范大学 | Method for preparing aluminium polychlorid with high content of Al13 |
| CN102344157B (en) * | 2010-07-30 | 2013-11-13 | 浙江师范大学 | Method for preparing aluminium polychlorid with high content of Al13 |
| CN105712387A (en) * | 2016-03-15 | 2016-06-29 | 北京世纪地和控股有限公司 | Method for preparing aluminum hydroxide sulfate |
| CN106395875A (en) * | 2016-09-14 | 2017-02-15 | 重庆中昆铝业有限公司 | Method for producing polyaluminium sulfate from aluminum profile machining waste liquid |
| EP3564187A2 (en) | 2018-04-03 | 2019-11-06 | Nikolaos Dailianis | Method and equipment for the recycling of alkaline wastes from aluminum extrusion industries for the production of useful coagulants |
| CN109224365A (en) * | 2018-08-20 | 2019-01-18 | 长安大学 | A kind of aluminium shape surface processing controlling waste residue method |
| CN110451844A (en) * | 2019-08-20 | 2019-11-15 | 重庆腾治科技有限公司 | A kind of alkali-free liquid accelerator and preparation method thereof |
| CN112142085A (en) * | 2020-08-04 | 2020-12-29 | 广西锋华环保科技有限公司 | Method for producing polyaluminum sulfate by using aluminum ash |
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|---|---|
| CN101279756B (en) | 2012-07-04 |
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Application publication date: 20081008 Assignee: JIANGSU YIJING WATER TREATMENT CHEMICAL CO., LTD. Assignor: Yijing Environment Protection Co., Ltd, Jiangsu Contract record no.: 2015320000410 Denomination of invention: Method for preparing polyaluminum sulfate Granted publication date: 20120704 License type: Exclusive License Record date: 20150610 |
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Effective date of registration: 20160120 Address after: Xu Yifeng village in Yixing City, Jiangsu province 214241 Patentee after: JIANGSU YIJING WATER TREATMENT CHEMICAL CO., LTD. Address before: 214205 Nanyue village, ring garden, Yixing, Jiangsu Patentee before: Yijing Environment Protection Co., Ltd, Jiangsu |
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Effective date of registration: 20181212 Address after: 221000 Xuzhou Industrial Park, Xuzhou City, Jiangsu Province, south of Mid-latitude Road and west of Tunshidagou Patentee after: Xuzhou Murray Circle Environmental Technology Co. Ltd. Address before: 214241 Yifeng Village, Xushe Town, Yixing City, Jiangsu Province Patentee before: JIANGSU YIJING WATER TREATMENT CHEMICAL CO., LTD. |