CN1483675A - Process for synthesizing aluminium polychhoride by evaporating residue using ethyl acetate - Google Patents
Process for synthesizing aluminium polychhoride by evaporating residue using ethyl acetate Download PDFInfo
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- CN1483675A CN1483675A CNA03132469XA CN03132469A CN1483675A CN 1483675 A CN1483675 A CN 1483675A CN A03132469X A CNA03132469X A CN A03132469XA CN 03132469 A CN03132469 A CN 03132469A CN 1483675 A CN1483675 A CN 1483675A
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Abstract
A process for preparing a liquid aluminum polychloride from acetic ether residual having a component of 5-20% law boiling point organic, 60-80% aluminum hydroxide, 10-15% aluminum chloride and a small amount of zinc chloride, includes reacting the residual with 10-25% hydrochloric acid, at a ratio of 1:1-5 and a temperature of 60-130 deg.C, and a time of 3-6 hours, and then settling and filtering. The aluminum polychloride obtained contains Al2O3 10-12%; and has salinity, 50-65; PH 3.5-5.
Description
The technical field is as follows:
the invention relates to a method for synthesizing polyaluminium chloride by producing ethyl acetate evaporation residues through an acetaldehyde condensation method.
Background art:
polyaluminium chloride, also known as basic aluminium chloride, is an inorganic high molecular aluminium salt with good water purification performance. The general formula is [ Al2(OH)nCl6-n]m, wherein n is more than or equal to 1 and less than or equal to 5, and m is less than or equal to 10. Compared with the traditional water purifying agents such as aluminum sulfate and ferric chloride, the water purifying agent has the advantages of high purification efficiency, more obvious effect when being used for treating high-turbidity raw water, fast floc formation, high precipitation speed, wide application range, small corrosivity and the like, and is more and more emphasized by drinking water and sewage treatment departments. In addition, the polyaluminium chloride can be used for paper making, pharmacy,Sugar manufacturing, precision casting, oil well sand prevention, concrete rapid hardening, high-grade tanning, bonding of refractory aluminum-silicon fiber cotton and the like.
A great deal of work is done by technical workers at home and abroad on the manufacturing method of the polyaluminium chloride, and a lot of innovations are provided from the selection of raw materials to the simplification of the process. The production process of the acid-soluble one-step method is developed by using aluminum ash as a raw material in 1971 in China, and polyaluminium chloride is produced in a large scale for the first time. And many manufacturers in China turn the attention to the production of polyaluminium chloride by using cheap and rich clay ore, bauxite, kaolin, coal gangue and the like as raw materials, and aim to use mineral resources with relatively low cost and wide sources to reduce the cost.
At present, the production process routes of polyaluminium chloride are various, and the following main processes are adopted for realizing industrialization: a coal gangue hydrochloric acid method; boiling pyrolysis method; aluminum hydroxide hydrochloric acid method; one-step and two-step methods of aluminum scrap hydrochloric acid and the like. Most of the methods are prepared by carrying out secondary polymerization on raw materials containing aluminum or aluminum ash, pure aluminum scraps and industrial concentrated hydrochloric acid under the conditions of high temperature and high pressure (or low pressure). The common disadvantages are long reaction time and high energy consumption. Particularly, concentrated hydrochloric acid has serious corrosion to equipment under high temperature and high pressure, the equipment is frequently overhauled, and a lot of troubles are brought to production. The method for synthesizing the polyaluminium chloride by using mineral resources such as coal gangue, bauxite, kaolin and the like as raw materials has the defects that the raw materials are roasted at a high temperature of 700-800 ℃, and treatment steps such as uniformly mixing, screening, drying, crushing and the like are required after sintering, so that the reaction energy consumption is high, the production process is long, and the production cost is increased. The study on the current state and progress of the preparation technology of polyaluminium chloride published by Lifancui et al in 2002, volume 92, pages 33-36 can be seen.
Aluminum ethoxide is used as a catalyst in the process of producing ethyl acetate by an acetaldehyde condensation method, and water is needed to be added to destroy the aluminum ethoxide after the reaction is finished, so that a large amount of evaporation residues are generated in the evaporation process, and 8-12 kg of residues can be generated when 1 ton of ethyl acetate is produced. The evaporation residue contains about 5-20% (mass fraction, the same below) of low boiling point organic matter, 60-80% of aluminum hydroxide, 10-15% of aluminum trichloride and a small amount of zinc chloride. The evaporation residues are generally treated by underground deep burying or stacking in the open air. This not only wastes aluminum resource but also pollutes environment.
The invention content is as follows:
the invention provides a method for synthesizing polyaluminium chloride by using evaporation residues of ethyl acetate, and the polyaluminium chloride can be used as a flocculating agent of industrial wastewater, so that wastes are treated by wastes, the environmental pollution is reduced, and aluminum resources are fully utilized. The method of the invention not only reduces the production cost of the polyaluminium chloride, but also fundamentally solves the problem of discharge of waste residue in the production of the ethyl acetate, which finds a way for recycling resources and controlling the pollution of wastes to the environment, and has remarkable economic and social benefits.
The present invention synthesizes polyaluminium chloride with the evaporating residue of ethyl acetate produced through acetaldehyde condensation process, and the evaporating residue consists of low boiling point organic matter 5-20 wt%, aluminum hydroxide 60-80 wt%, aluminum trichloride 10-15 wt% and small amount of zinc chloride. The synthesis steps of the polyaluminium chloride are as follows: firstly, the evaporation residue reacts with hydrochloric acid, and liquid polyaluminium chloride is obtained through polymerization, sedimentation and filtration, wherein the reaction equation is as follows:
the mass ratio of the evaporation residue to the hydrochloric acid is 1: 1-5, the concentration of the hydrochloric acid is 10% -25%, the reaction time is 3-6 hours, the reaction temperature is 60-130 ℃, and Al of liquid polyaluminium chloride is2O3The content is 10-12%, the basicity is 50-65, and the pH is 3.5-5. The hydrochloric acid used can be industrial grade hydrochloric acid or hydrochloric acid which is a byproduct in the chemical production process.
The specific implementation mode is as follows:
adding 50g of evaporation residue into 95.5g of 20% HCl, heating in water bath, stirring, and controlling reaction temperatureWhen the reaction was carried out at 80 ℃ for 2.5 hours, 85ml of water was added under stirring, the reaction was continued for 3 hours, pH was measured to be 4.0, the reaction was terminated, the reaction mixture was cooled to room temperature, and filtration was carried out to obtain Al2O3Polyaluminum chloride with a content of 10.9% and a basicity of 53.
Therefore, the polyaluminium chloride synthesized by the method has the advantages of low production cost, simple process, reutilization of waste, reduction of environmental pollution and remarkable economic and social benefits.
Claims (2)
1. The invention relates to a method for synthesizing polyaluminium chloride by using ethyl acetate evaporation residues, which comprises 5-20% of low-boiling-point organic matters, 60-80% of aluminum hydroxide, 10-15% of aluminum trichloride and a small amount of zinc chloride, and is characterized in that the evaporation residues are reacted with hydrochloric acid at the mass ratio of 1: 1-5, the mass fraction of the hydrochloric acid is 10-25%, the reaction time is 3-6 hours, the reaction temperature is 60-130 ℃, and liquid polyaluminium chloride is obtained by polymerization, sedimentation and filtration.
2. The method for synthesizing polyaluminum chloride from residues of evaporation of ethyl acetate as claimed in claim 1, wherein said hydrochloric acid can be industrial-grade hydrochloric acid or hydrochloric acid as byproduct of chemical production.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB03132469XA CN100337923C (en) | 2003-06-30 | 2003-06-30 | Process for synthesizing aluminium polychhoride by evaporating residue using ethyl acetate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB03132469XA CN100337923C (en) | 2003-06-30 | 2003-06-30 | Process for synthesizing aluminium polychhoride by evaporating residue using ethyl acetate |
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| Publication Number | Publication Date |
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| CN1483675A true CN1483675A (en) | 2004-03-24 |
| CN100337923C CN100337923C (en) | 2007-09-19 |
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| CNB03132469XA Expired - Fee Related CN100337923C (en) | 2003-06-30 | 2003-06-30 | Process for synthesizing aluminium polychhoride by evaporating residue using ethyl acetate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100460328C (en) * | 2007-04-28 | 2009-02-11 | 王军 | Technical process for producing chloride aluminum |
| CN104761030A (en) * | 2015-03-20 | 2015-07-08 | 杭州萧山三江净水剂有限公司 | Special efficient polyaluminum chloride for printing and dyeing wastewater, and preparation method thereof |
| CN111003869A (en) * | 2019-12-26 | 2020-04-14 | 安徽工业大学 | Hydrofluoric acid wastewater resource utilization method |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1032150A (en) * | 1987-09-24 | 1989-04-05 | 莽济民 | Process for producing flocculant of polymeric aluminium chloride |
| CN1051541A (en) * | 1989-11-06 | 1991-05-22 | 五邑大学 | Polymerized aluminium chloride synthesized from waste slag generated in processing aluminium shaped material |
| CN1090555A (en) * | 1993-02-04 | 1994-08-10 | 阜新市福利环保净水剂厂 | A kind of technology of producing flocculant of polymeric aluminium chloride |
| CN1180661A (en) * | 1996-10-21 | 1998-05-06 | 贾久顺 | Method for producing polymerized aluminium-chloride |
| CN1205306A (en) * | 1997-07-15 | 1999-01-20 | 吉林化学工业公司龙江净水剂厂 | Method of preparing polymerization aluminium chloride |
| CN1334241A (en) * | 2000-07-14 | 2002-02-06 | 任忠胜 | Process for preparing polyaluminium chloride |
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2003
- 2003-06-30 CN CNB03132469XA patent/CN100337923C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100460328C (en) * | 2007-04-28 | 2009-02-11 | 王军 | Technical process for producing chloride aluminum |
| CN104761030A (en) * | 2015-03-20 | 2015-07-08 | 杭州萧山三江净水剂有限公司 | Special efficient polyaluminum chloride for printing and dyeing wastewater, and preparation method thereof |
| CN111003869A (en) * | 2019-12-26 | 2020-04-14 | 安徽工业大学 | Hydrofluoric acid wastewater resource utilization method |
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| CN100337923C (en) | 2007-09-19 |
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Granted publication date: 20070919 Termination date: 20100630 |