CN103833118B - Preparation method of polyaluminium chloride coagulant - Google Patents
Preparation method of polyaluminium chloride coagulant Download PDFInfo
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- CN103833118B CN103833118B CN201410101932.5A CN201410101932A CN103833118B CN 103833118 B CN103833118 B CN 103833118B CN 201410101932 A CN201410101932 A CN 201410101932A CN 103833118 B CN103833118 B CN 103833118B
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Abstract
The invention discloses a preparation method of polyaluminium chloride coagulant. The preparation method comprises the following steps: completely reacting industrial grade aluminium hydroxide serving as a main raw material with a sodium hydroxide solution under conditions of heating and stirring so as to form a transparent solution; cooling the reaction solution to room temperature, and then adding citric acid to the reaction solution; after the citric acid reacts with the reaction solution and is uniformly mixed, dropwise adding hydrochloric acid to the mixed solution, and rapidly stirring; and at the end of the reaction, obtaining colorless, transparent and viscous liquid which is the polyaluminium chloride coagulant solution. The preparation method has the advantages of simple process, short reaction period, low corrosion to equipment and low production cost; and the polyaluminium chloride coagulant has excellent flocculating performance and can be widely applied to feed water treatment and wastewater treatment.
Description
Technical field
The invention belongs to flocculation agent preparing technical field, be specifically related to a kind of preparation method of polymerize aluminum chloride coagulating agent.
Background technology
Coagulating agent is the core of coagulation Pollution control technology, and it is widely used in Water purification and sewage treatment area.At present, the inorganic polymer coagulant generally used mainly is divided into polymeric aluminum class coagulating agent and polymeric iron class coagulating agent.
Polymerize aluminum chloride is a kind of application inorganic polymer coagulant very widely.It the effect such as to catch mainly through absorption charge neutrality, compression double electric layer, adsorption bridging, net, de-steady, the collision of the colloidal solid making to be difficult to sedimentation in water body, assemble, precipitation, to reach the object of purifying water body.Although polymerize aluminum chloride has, consumption is few, the advantage such as of fine quality, easy to use of purifying waste water, and its hydrolysis is more weak, flco small volume, and settling velocity is slower.The synthetic method of polymerize aluminum chloride, by the difference of production technique, can be divided into acid pasting, alkali solution technique, neutralisation, pyrolysis method, compressive reaction method, electroosmose process, electrolytic process etc.And when adopting aluminium hydroxide to be raw material, it mainly adopts acid pasting to prepare polymerize aluminum chloride.Because aluminium hydroxide solubility in acid is poor, so generally need to carry out at high temperature under high pressure, therefore higher to the requirement of reactor, and the product obtained often basicity is lower.
When adopting alkali solution technique to prepare polymerize aluminum chloride, not only can improve the basicity of product, its energy consumption is corresponding reduction also, and is also less than acid pasting to the corrodibility of equipment.But in alkali solution technique preparation process, if proportioning raw materials is unbalance or misoperation, very easily form the alumine hydroxide colloid of indissoluble, affect the quality of polymerize aluminum chloride coagulating agent.
Summary of the invention
The object of the invention is to overcome prior art above shortcomings, a kind of preparation method of brand-new polymerize aluminum chloride coagulating agent is provided.
Realize above-mentioned purpose, the present invention adopts following technical scheme:
A preparation method for polymerize aluminum chloride coagulating agent, with technical grade aluminium hydroxide for main raw material, under heating, agitation condition, aluminium hydroxide and sodium hydroxide solution complete reaction form clear solution; After solution is cooled to room temperature, add citric acid solution; To be mixed even time, to mixed solution and dripping hydrochloric acid soln, obtain colourless, transparent, thick liquid, be polymerize aluminum chloride coagulating agent;
Wherein, the mass ratio of aluminium hydroxide and sodium hydroxide solution is 1.25 ~ 1.75:1; The concentration of sodium hydroxide solution is 40% ~ 50%; Aluminium hydroxide and citric acid mass ratio are 5.8 ~ 8.8:1; Citric acid concentration is 28% ~ 40%; The concentration of hydrochloric acid soln is 18% ~ 19%.
Further, concrete steps are as follows:
(1) by concentration be 40% ~ 50% sodium hydroxide solution be heated to micro-boiling; Again under fast stirring, industrial aluminium hydroxide is added in proportion in reaction vessel; After reacting about 45min, form clear solution;
(2) after step (1) made liquid cooling to room temperature, rapid stirring limit, limit drips citric acid solution 20 ~ 30ml that concentration is 28% ~ 40% in proportion; After dropwising, continue rapid stirring 5min, treat its complete reaction, mixing;
(3) by concentration be 18% ~ 19% hydrochloric acid soln slowly drop in step (2) gained homogeneous solution, and accelerate stir; After reacting completely, obtain colourless, transparent, thickness polymerize aluminum chloride coagulating agent.
Compared to existing technology, tool of the present invention has the following advantages:
1, technical process is simple, and reaction time is short, and energy consumption is little, easy to operate, basicity easy to control.
2, in preparation process, do not need pressurization, reduce the requirement to reactor, to the corrodibility yet corresponding reduction of reactor.
3, the present invention introduces certain density citric acid solution in preparation process, and it greatly reduces the generation of insoluble alumine hydroxide colloid in this method synthesized polymer aluminum chloride process, significantly improves polymeric aluminum chlorides solution quality.
4, the polymerize aluminum chloride that prepared by the present invention is liquid product.Stable chemical nature at normal temperatures, not perishable, and easy to use.
5, the polymerize aluminum chloride that prepared by the present invention has turbidity, feature that COD clearance is high.Polymerize aluminum chloride prepared by the present invention can be widely used in Water purification and sewage disposal.
embodiment:
Below in conjunction with specific embodiment, the present invention is described in further detail.
embodiment 1:a preparation method for polymerize aluminum chloride coagulating agent, comprises the steps:
(1) 40g sodium hydroxide is placed in reactor, adds the distilled water of 100ml; Sodium hydroxide solution is preheated to micro-boiling; Under fast stirring, 50g aluminium hydroxide is added in reactor; After reacting about 1h, aluminium hydroxide dissolves completely, forms clear solution.
(2) after above-mentioned clear solution is cooled to room temperature, it is that the citric acid solution 30ml of 28% is in reactor that rapid stirring limit, limit adds massfraction; After adding, continue rapid stirring 5min, treat its complete reaction, mixing.
(3) by concentration be 18% ~ 19% hydrochloric acid soln slowly drop in step (2) gained homogeneous solution, and accelerate stir; In dropping process, when pH value is 6 ~ 8, first can generate a large amount of aluminum hydroxide gel, continue to drip hydrochloric acid soln, gel starts to dissolve, and after gel dissolves completely, colourless, transparent, the thick liquid that obtain are polymerize aluminum chloride coagulant solution.
Product quality indicator is as follows:
In drinking water treatment, turbidity removal rate: 96.50%.
To sanitary sewage (COD
cr: 127 ~ 145 mg/L; Turbidity 56 ~ 66 NTU; PH:8.40 ~ 8.75) turbidity removal rate: 95.67%; To sanitary sewage COD clearance: 82.33%.
embodiment 2:a preparation method for polymerize aluminum chloride coagulating agent, comprises the steps:
(1) 40g sodium hydroxide is placed in reactor, adds the distilled water of 100ml; Sodium hydroxide solution is preheated to micro-boiling; Under fast stirring, 60g aluminium hydroxide is added in reactor; After reacting about 1h, aluminium hydroxide dissolves completely, forms clear solution.
(2) after above-mentioned clear solution is cooled to room temperature, it is that the citric acid solution 25ml of 35% is in reactor that rapid stirring limit, limit adds massfraction; After adding, continue rapid stirring 5min, treat its complete reaction, mixing.
(3) by concentration be 18% ~ 19% hydrochloric acid soln slowly drop in step (2) gained homogeneous solution, and accelerate stir; In dropping process, when pH value is 6 ~ 8, first can generate a large amount of aluminum hydroxide gel, continue to drip hydrochloric acid soln, gel starts to dissolve, and after gel dissolves completely, colourless, transparent, the thick liquid that obtain are polymerize aluminum chloride coagulant solution.
Product quality indicator is as follows:
In drinking water treatment, turbidity removal rate: 97.93%.
To sanitary sewage (COD
cr: 127 ~ 145 mg/L; Turbidity 56 ~ 66 NTU; PH:8.40 ~ 8.75) turbidity removal rate: 97.45%; To sanitary sewage COD clearance: 87.19%.
embodiment 3:a preparation method for polymerize aluminum chloride coagulating agent, comprises the steps:
(1) 40g sodium hydroxide is placed in reactor, adds the distilled water of 80ml; Sodium hydroxide solution is preheated to micro-boiling; Under fast stirring, 60g aluminium hydroxide is added in reactor; After reacting about 1h, aluminium hydroxide dissolves completely, forms clear solution.
(2) after above-mentioned clear solution is cooled to room temperature, it is that the citric acid solution 20ml of 40% is in reactor that rapid stirring limit, limit adds massfraction; After adding, continue rapid stirring 5min, treat its complete reaction, mixing.
(3) by concentration be 18% ~ 19% hydrochloric acid soln slowly drop in step (2) gained homogeneous solution, and accelerate stir; In dropping process, when pH value is 6 ~ 8, first can generate a large amount of aluminum hydroxide gel, continue to drip hydrochloric acid soln, gel starts to dissolve, and after gel dissolves completely, colourless, transparent, the thick liquid that obtain are polymerize aluminum chloride coagulant solution.
Product quality indicator is as follows:
In drinking water treatment, turbidity removal rate: 98.22%.
To sanitary sewage (COD
cr: 127 ~ 145 mg/L; Turbidity 56 ~ 66 NTU; PH:8.40 ~ 8.75) turbidity removal rate: 97.60%; To sanitary sewage COD clearance: 86.42%.
embodiment 4:a preparation method for polymerize aluminum chloride coagulating agent, comprises the steps:
(1) 40g sodium hydroxide is placed in reactor, adds the distilled water of 80ml; Sodium hydroxide solution is preheated to micro-boiling; Under fast stirring, 70g aluminium hydroxide is added in reactor; After reacting about 1h, aluminium hydroxide dissolves completely, forms clear solution.
(2) after above-mentioned clear solution is cooled to room temperature, it is that the citric acid solution 20ml of 40% is in reactor that rapid stirring limit, limit adds massfraction; After adding, continue rapid stirring 5min, treat its complete reaction, mixing.
(3) by concentration be 18% ~ 19% hydrochloric acid soln slowly drop in step (2) gained homogeneous solution, and accelerate stir; In dropping process, when pH value is 6 ~ 8, first can generate a large amount of aluminum hydroxide gel, continue to drip hydrochloric acid soln, gel starts to dissolve, but in dissolution process, the insoluble alumine hydroxide colloid of forming section, is polymerize aluminum chloride coagulant solution by filtering colourless, transparent, the thick liquid that obtain.
Product quality indicator is as follows:
In drinking water treatment, turbidity removal rate: 92.12%.
To sanitary sewage (COD
cr: 127 ~ 145 mg/L; Turbidity 56 ~ 66 NTU; PH:8.40 ~ 8.75) turbidity removal rate: 94.76%; To sanitary sewage COD clearance: 82.10%.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (2)
1. a preparation method for polymerize aluminum chloride coagulating agent, is characterized in that, comprises the steps:
With technical grade aluminium hydroxide for main raw material, under heating, agitation condition, aluminium hydroxide and sodium hydroxide solution complete reaction form clear solution; After solution is cooled to room temperature, add citric acid solution; To be mixed even time, to mixed solution and dripping hydrochloric acid soln, obtain colourless, transparent, thick liquid, be polymerize aluminum chloride coagulating agent;
Wherein, the mass ratio of aluminium hydroxide and sodium hydroxide is 1.25 ~ 1.75:1; The concentration of sodium hydroxide solution is 40% ~ 50%; Aluminium hydroxide and citric acid mass ratio are 5.8 ~ 8.8:1; Citric acid concentration is 28% ~ 40%; The concentration of hydrochloric acid soln is 18% ~ 19%.
2. the preparation method of polymerize aluminum chloride coagulating agent according to claim 1, it is characterized in that, concrete steps are as follows:
(1) by concentration be 40% ~ 50% sodium hydroxide solution be heated to micro-boiling; Again under fast stirring, industrial aluminium hydroxide is added in proportion in reaction vessel; After reacting about 45min, form clear solution;
(2) after step (1) made liquid cooling to room temperature, rapid stirring limit, limit drips citric acid solution 20 ~ 30ml that concentration is 28% ~ 40% in proportion; After dropwising, continue rapid stirring 5min, treat its complete reaction, mixing;
(3) by concentration be 18% ~ 19% hydrochloric acid soln slowly drop in step (2) gained homogeneous solution, and accelerate stir; After reacting completely, obtain colourless, transparent, thickness polymerize aluminum chloride coagulating agent.
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| CN104724803B (en) * | 2015-03-10 | 2016-08-24 | 重庆大学 | A kind of preparation method and applications of coagulant |
| CN108862516B (en) * | 2018-07-03 | 2021-11-30 | 贵州大学 | Method for co-production of sewage treatment coagulant by producing acid from phosphogypsum and fly ash |
| CN112794423A (en) * | 2020-12-31 | 2021-05-14 | 西安吉利电子化工有限公司 | Defluorination agent and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100813111B1 (en) * | 2006-10-23 | 2008-03-17 | (주) 에코솔루텍 | The preparation method of poly aluminium chloride from waste acid |
| CN101830546A (en) * | 2010-04-13 | 2010-09-15 | 沈阳化工学院 | Poly-aluminum chloride-magnesium printing and dyeing wastewater coagulant and preparation method thereof |
| CN102115234A (en) * | 2009-12-30 | 2011-07-06 | 中国科学院生态环境研究中心 | Preparation method of flocculant capable of removing phosphate from red mud |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100813111B1 (en) * | 2006-10-23 | 2008-03-17 | (주) 에코솔루텍 | The preparation method of poly aluminium chloride from waste acid |
| CN102115234A (en) * | 2009-12-30 | 2011-07-06 | 中国科学院生态环境研究中心 | Preparation method of flocculant capable of removing phosphate from red mud |
| CN101830546A (en) * | 2010-04-13 | 2010-09-15 | 沈阳化工学院 | Poly-aluminum chloride-magnesium printing and dyeing wastewater coagulant and preparation method thereof |
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Application publication date: 20140604 Assignee: Dongguan Huaqing Water Purification Technology Co., Ltd. Assignor: Chongqing University Contract record no.: 2015440000806 Denomination of invention: Preparation method of polyaluminium chloride coagulant Granted publication date: 20150325 License type: Exclusive License Record date: 20151201 |
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Effective date of registration: 20160715 Address after: 510000 Guangdong Province, Dongguan city Wangniudun Du Wu Cun Industrial Zone Patentee after: Dongguan Huaqing Water Purification Technology Co., Ltd. Address before: 400044 Shapingba District Sha Street, No. 174, Chongqing Patentee before: Chongqing University |