CN101306827B - Process for preparing polymerized aluminum by burnt waste slag of sludge - Google Patents
Process for preparing polymerized aluminum by burnt waste slag of sludge Download PDFInfo
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- CN101306827B CN101306827B CN2008101147436A CN200810114743A CN101306827B CN 101306827 B CN101306827 B CN 101306827B CN 2008101147436 A CN2008101147436 A CN 2008101147436A CN 200810114743 A CN200810114743 A CN 200810114743A CN 101306827 B CN101306827 B CN 101306827B
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- sludge
- aluminum
- waste slag
- burnt waste
- hydrochloric acid
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Abstract
The invention relates to a method for preparing polyaluminium chloride from sludge incineration waste residues, which comprises the steps of adding the sludge incineration waste residues into 10-30% hydrochloric acid in accordance with the equivalence ratio of alumina and hydrochloric acid 1.0:(1.0-1.5), stirring at room temperature, allowing reaction for 2-10 hours, and performing solid-liquid separation; and adding calcium oxide powder into the obtained aluminum chloride-containing acid solution in accordance with the weight ratio of aluminum chloride and calcium oxide 1.0:(0.3-0.6), and stirring at room temperature for 2-24 hours to obtain polyaluminium solution. The inventive method can be used for pyrolysis and incineration waste residues resource treatment of sludge formed by aluminum salt flocculation agent for sewage treatment; can realize recovery and cyclic utilization of the aluminum salt flocculation agent added in sewage treatment process, and reduce pollutant emission and aluminum resource consumption; and is helpful for clean production and resource saving of sewage treatment system.
Description
Technical field
The present invention relates to a kind of method for preparing polymeric aluminum with burnt waste slag of sludge, this method is applicable to process water, sewage-farms such as industrial sewage such as oil field, refinery and urban domestic wastewater carry out purifying treatment with aluminium salt flocculation medicament and mud concentrates the mud that forms, its waste slag of aluminum that contains through burn forming, or reclaim and utilize again through the aluminium salt that contains waste slag of aluminum of calcination decarburization again through the residue of pyrolysis processing.
Background technology
Polymeric aluminum has another name called aluminium chlorohydroxide or aluminium chlorohydroxide.It has that coagulability is strong, consumption is few, water purification usefulness height, characteristics that adaptive faculty is strong, is widely used in printing and dyeing, the process water and the wastewater treatment of industry such as process hides, medicine, oil, papermaking, makeup.Its water purification is can force rate Tai-Ace S 150 high 8～10 times, and it is fast and particle is big to form the speed of floss during cohesion.Polymeric aluminum is a kind of efficient flocculant that the scientist of states such as moral, Japan and the United States found in the thirties, and the later stage sixties forms scale production in developed country, and the output surge seventies is called as epoch-making inorganic polymer flocculation seventies medicament.China develops this product since the seventies, is subjected to the influence of aluminium deep processing, and the aluminium ash is collected difficulty and limited development, and the eighties, the poly-aluminium of the explained hereafter that has nothing in common with each other is adopted according to its cheap bauxite resource advantage in various places.
At present, domestic production polymeric aluminum is mainly based in acid-soluble one-step, the acidleach and two-step approach, gel method, thermal decomposition method etc.Raw material commonly used mainly contains pure aluminum (various aluminium processing fents such as aluminium ingot, aluminium ash, aluminium bits), aluminum-containing mineral (as bauxite, clay, kaolin, alunite, coal gangue etc.), aluminium salt compound (as aluminum chloride, Tai-Ace S 150 etc.), flyash etc.
Polymeric aluminum is at process water, is extensive use of during industrial sewage such as oil field, refinery and urban domestic wastewater purifying treatment and mud concentrate, and belongs to disposable running stores, finally enters environment with the mud that forms or the waste residue of its burning or pyrolysis processing.Through the aluminium of the general sewage disposal pyrolyzing sludge of research and appraisal residue (with Al
2O
3Meter) content can reach more than 20%, and Gao Zheke reaches 50% to 60%, and higher aluminium content is arranged, if not to its recycling, it had both wasted bauxite resource, also has environmental pollution simultaneously.Adopt burnt waste slag of sludge to prepare polymeric aluminum, all be of great practical significance from the aspects such as useless improvement, resources conservation and economic benefit admittedly in sewage-farm so that it obtains certain utilization.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing polymeric aluminum with burnt waste slag of sludge, solution contains that aluminium solid waste is innoxious, minimizing and resource utilization problem, and emphasis is to solve a large amount of aluminium salt flocculation medicaments to be used for a large amount of mud that form after the sewage disposal and the innoxious and resource recycling of burning or pyrolysis processing waste residue thereof.
The inventive method is achieved in that burnt waste slag of sludge is placed closed reactor, presses aluminum oxide (Al contained in the burnt waste slag of sludge
2O
3) with the equivalence ratio of hydrochloric acid be that 1.0: 1.0～1.5 to add concentration be 10～30% aqueous hydrochloric acid, stir at normal temperatures and carry out sour molten reaction, sour molten reaction 2～10 hours; The solidliquid mixture that forms is carried out solid-liquid separation, must contain the chlorination aluminum solutions; Contain aluminum chloride (AlCl in the acid solution that separation is obtained then
3) weight ratio of weight and calcium oxide is 1.0: 0.3～0.6 to add lime powder, stirs at normal temperatures and carries out polyreaction, polymerization reaction time is 2-24 hour, get final product polymeric aluminum solution.
Concrete processing parameter and condition are done following description:
1, burnt waste slag of sludge is to carry out the sewage purification processing with aluminium salt flocculation medicament to concentrate the mud that forms with mud, through burning the waste residue of formation, or through the residue of pyrolysis processing again through the waste residue of calcination decarburization, the aluminum oxide (Al of burnt waste slag
2O
3) content is 10～60%, the best is 30～60%.
2, the used acid of sour molten reaction is hydrochloric acid, and the hydrochloric acid consumption is 1.0: 1.0～1.2 by equivalence ratio the best of the salic and hydrochloric acid of burnt waste slag of sludge; Concentration of hydrochloric acid the best is 20～30%; The molten reaction times the best of acid is 2～5 hours.
What 3, described solid-liquid separation adopted is separating centrifuge, is the best with the horizontal helical type separating centrifuge wherein.Also can adopt sedimentation method to isolate and contain the chlorination aluminum solutions.
4, the weight ratio that contains aluminum chloride weight contained in the chlorination aluminum solutions and calcium oxide that obtains by separation is 1.0: 0.4～0.5; The polyreaction churning time is 5-10 hour the best.Get polymeric aluminum solution.
The invention has the beneficial effects as follows: the method for preparing polymeric aluminum with burnt waste slag of sludge is used for the mud that purifying treatment and the concentrated formation of mud are carried out with aluminium salt flocculation medicament in sewage-farms such as oil field, refinery, urban industry and sanitary wastewater, it is through burning the waste slag of aluminum that contains that forms, or through the residue of pyrolysis processing again through the recycling treatment that contains waste slag of aluminum of calcination decarburization, can realize the recycle and reuse of the aluminium salt flocculation medicament that sewage treatment process adds, reduce pollutant emission and bauxite resource consumption, help Sewage treatment systems cleaner production and resources conservation.
Description of drawings
Fig. 1 is the present invention prepares the method for polymeric aluminum with burnt waste slag of sludge a process flow sheet.
Embodiment
Embodiment 1: consult Fig. 1.
1. take by weighing 228g oilfield sewage burnt waste slag of sludge, the aluminum oxide (Al in the burnt waste slag of sludge
2O
3) content is 30%.
2. press the equivalence ratio 1: 1.17 of aluminum oxide contained in the burnt waste slag of sludge and hydrochloric acid, adding concentration is 30% aqueous hydrochloric acid 508ml in the 2L Erlenmeyer flask, under magnetic agitation, slowly add above-mentioned burnt waste slag, add the airtight stirring in back after 2 hours 30 minutes, adopt the horizontal helical type separating centrifuge to isolate and contain aluminum chloride (AlCl
3) solution;
3. under powerful stirring condition, by containing aluminum chloride (AlCl contained in the chlorination aluminum solutions
3) with the weight ratio of calcium oxide be 1: 0.52, containing of going out slowly add lime powder 60g in the aluminic acid liquid to centrifugation, stirred 3 hours, obtain the liquid product polymeric aluminum, its aluminium (is pressed Al
2O
3Meter) content is 10.52%, and basicity is 61.24%.
Embodiment 2: consult Fig. 1.
1. take by weighing 450g oil refining sewerage burnt waste slag of sludge, the aluminum oxide (Al that contains in the burnt waste slag of sludge
2O
3) be 45%.
2. press the equivalence ratio 1: 1.08 of aluminum oxide contained in the burnt waste slag of sludge and hydrochloric acid, add the aqueous hydrochloric acid 1383ml of concentration at the 2L Erlenmeyer flask for adding 30%, under magnetic agitation, slowly add above-mentioned roasting residue, add the airtight stirring in back after 3 hours, adopt the centrifugal settling method to isolate and contain aluminum chloride (AlCl
3) solution;
3. under powerful stirring condition, the weight ratio of contained aluminum chloride and calcium oxide is 1: 0.43 in the chlorination aluminum solutions by containing, and containing of going out slowly adds lime powder 140g in the chlorination aluminic acid liquid to centrifugation, stirs 3 hours, obtain the liquid product polymeric aluminum, its aluminium (is pressed Al
2O
3Meter) content is 10.34%, and basicity is 69.82%.
Claims (6)
1. one kind prepares the method for polymeric aluminum with burnt waste slag of sludge, it is characterized in that:
Burnt waste slag of sludge is done following processing:
A, burnt waste slag of sludge is placed closed reactor, equivalence ratio by aluminum oxide contained in the burnt waste slag of sludge and hydrochloric acid is 1.0: 1.0～1.5, adding concentration is 10～30% aqueous hydrochloric acid, stirs at normal temperatures and carries out sour molten reaction, sour molten reaction 2～10 hours;
B, the solidliquid mixture that forms is carried out solid-liquid separation, must contain the chlorination aluminum solutions;
C, the weight ratio that contains aluminum chloride weight contained in the chlorination aluminum solutions and calcium oxide that obtains by separation are 1.0: 0.3～0.6 adding lime powder, stir at normal temperatures and carry out polyreaction, and polymerization reaction time is 2-24 hour, gets polymeric aluminum solution.
2. a kind ofly prepare the method for polymeric aluminum with burnt waste slag of sludge according to claim 1 is described, it is characterized in that: the alumina content of burnt waste slag of sludge is 10-60%.
3. a kind ofly prepare the method for polymeric aluminum with burnt waste slag of sludge according to claim 1 is described, it is characterized in that: the alumina content of burnt waste slag of sludge is 30-60%.
4. describedly a kind ofly prepare the method for polymeric aluminum with burnt waste slag of sludge according to claim 1 or 2 or 3, it is characterized in that: the used acid of sour molten reaction is hydrochloric acid, and the aluminum oxide that the hydrochloric acid consumption contains by burnt waste slag of sludge and the equivalence ratio of hydrochloric acid are 1.0: 1.0～1.2; Concentration of hydrochloric acid is 20-30%; The molten reaction times of acid is 2-5 hour.
5. a kind ofly prepare the method for polymeric aluminum with burnt waste slag of sludge according to claim 1 is described, it is characterized in that: described solid-liquid separation is centrifugation, and the separating device of use is the horizontal helical type separating centrifuge.
6. a kind ofly prepare the method for polymeric aluminum with burnt waste slag of sludge according to claim 1 is described, it is characterized in that: the lime powder amount that polyreaction adds is 1.0: 0.4～0.5 by the weight ratio that contains aluminum chloride weight contained in the chlorination aluminum solutions and calcium oxide; The polyreaction churning time is 5-10 hour.
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| CN2008101147436A CN101306827B (en) | 2008-06-11 | 2008-06-11 | Process for preparing polymerized aluminum by burnt waste slag of sludge |
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| CN2008101147436A CN101306827B (en) | 2008-06-11 | 2008-06-11 | Process for preparing polymerized aluminum by burnt waste slag of sludge |
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| CN101306827A CN101306827A (en) | 2008-11-19 |
| CN101306827B true CN101306827B (en) | 2010-07-28 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103121779B (en) * | 2013-02-04 | 2014-06-18 | 刘进龙 | Cyclic regeneration method and application of town sewage treatment medicament |
| CN107285355B (en) * | 2017-08-01 | 2019-01-04 | 广西新晶科技有限公司 | A method of aluminium polychloride is prepared using discarded anthraquinone regenerative agent |
| CN110963662A (en) * | 2019-12-09 | 2020-04-07 | 上海净屹环保科技有限公司 | Method for recovering aluminum salt coagulant from aluminum-containing sludge |
| CN114804315B (en) * | 2022-06-06 | 2023-07-14 | 中国铁工投资建设集团有限公司 | Polyaluminium ferric chloride prepared from municipal sludge drying pyrolysis residues and composite flocculant |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2626567A1 (en) * | 1988-01-29 | 1989-08-04 | Atochem | ALUMINUM BASIC CHLOROSULFATE, METHOD FOR PRODUCING THE SAME, USE THEREOF AS FLOCCULANT AGENT |
| CN1106766A (en) * | 1994-02-08 | 1995-08-16 | 董正康 | Process for production of aluminium polychloride |
| CN1718543A (en) * | 2004-07-09 | 2006-01-11 | 中国石油天然气股份有限公司 | Preparation method of polymerized aluminium chloride having high aluminium content |
| CN101113067A (en) * | 2006-07-28 | 2008-01-30 | 中国石油天然气股份有限公司 | Resource treating method for oil-containing sludge |
-
2008
- 2008-06-11 CN CN2008101147436A patent/CN101306827B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2626567A1 (en) * | 1988-01-29 | 1989-08-04 | Atochem | ALUMINUM BASIC CHLOROSULFATE, METHOD FOR PRODUCING THE SAME, USE THEREOF AS FLOCCULANT AGENT |
| CN1106766A (en) * | 1994-02-08 | 1995-08-16 | 董正康 | Process for production of aluminium polychloride |
| CN1718543A (en) * | 2004-07-09 | 2006-01-11 | 中国石油天然气股份有限公司 | Preparation method of polymerized aluminium chloride having high aluminium content |
| CN101113067A (en) * | 2006-07-28 | 2008-01-30 | 中国石油天然气股份有限公司 | Resource treating method for oil-containing sludge |
Non-Patent Citations (2)
| Title |
|---|
| 王莉娜.含油废水处理剂的合成与应用研究.中国优秀博硕士学位论文全文数据库(硕士) 工程科技I辑 8.2006,(8),第15页"2.1.1 实验研究内容","2.1.2 试验研究技术路线"、图2-1. |
| 王莉娜.含油废水处理剂的合成与应用研究.中国优秀博硕士学位论文全文数据库(硕士) 工程科技I辑 8.2006,(8),第15页"2.1.1 实验研究内容","2.1.2 试验研究技术路线"、图2-1. * |
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