CN104150517B - The useless comprehensive utilization production method of a kind of process two - Google Patents
The useless comprehensive utilization production method of a kind of process two Download PDFInfo
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- CN104150517B CN104150517B CN201410378343.1A CN201410378343A CN104150517B CN 104150517 B CN104150517 B CN 104150517B CN 201410378343 A CN201410378343 A CN 201410378343A CN 104150517 B CN104150517 B CN 104150517B
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Abstract
The invention discloses the useless comprehensive utilization production method of a kind of process two, to comprise the process trade mark be the aluminium mud of HW17 and the trade mark is the Waste Sulfuric Acid of HW34 or the comprehensive utilization production method of waste hydrochloric acid, be that HW17 aluminium mud is by hot-air dry desorption by the trade mark, become solid aluminum mud after desorption completes, the acidity value controlling the solid aluminum mud after desorption is 7.8 ~ 8.2; Three (pungent-last of the ten Heavenly stems) alkyl tertiary amine extraction agent is added respectively in Waste Sulfuric Acid or waste hydrochloric acid; The Waste Sulfuric Acid processed or waste hydrochloric acid are put in the reactor with insulation jacket, more slowly add the solid aluminum mud processed, hybrid reaction obtains polymerize aluminum chloride, then successively through spraying dry and water film dedusting, obtains pure clear polymerize aluminum chloride.The aluminum-containing raw material of the waste of pre-treatment and discarded hydrochloric acid, sulfuric acid as raw materials for production, while achieving the dual function of reserved resource and protection of the environment, are solved the problem of the effective energy-conserving and environment-protective of realization truly by the present invention.
Description
Technical field
The present invention relates to the useless comprehensive utilization production method of a kind of process two, belong to offal treatment recycling production field.
Background technology
China is aluminium alloy big producing country, oxidized aluminum alloy pond (HW17) aluminium mud is one of the most unmanageable problem inside industry, normal processing method is piled up, landfill, same chemical plant, Condenser Factory, the tankage concentration of technical process inside the factories such as Electroplate Factory is that 15% ~ 20% abraum salt (sulphur) acid (HW34) current also not good treatment process carries out process recovery.
Polymerize aluminum chloride, also referred to as aluminium chlorohydroxide, it is the middle macromolecular compound between six water aluminum chlorides and aluminium hydroxide, because pure clear polymerize aluminum chloride to be built bridge the macromolecular compound be polymerized by hydroxyl, thus very easily water-soluble and hydrolysis can occur and produce the series of physical chemical actions such as cohesion, absorption, precipitation.Therefore, aluminum chloride is often used as water conditioner, with except the foreign material in anhydrating, but because the concentration of aluminum chloride of the routine of preparation is low, drying condition is more difficult, so usually all with liquid product supply, usage quantity is very large, and production cost is higher, thus limits to some extent its application.
Polymerize aluminum chloride is as a kind of conventional High-efficient Water treatment additive, and the chloride raw material such as calcium aluminate powder or bauxite is its important raw materials for production.Production process not only needs to consume a large amount of Mineral resources, also need hydrochloric acid as starting material, very adverse influence is had to environment and resources, but along with expanding economy, the generation of waste water but gets more and more, therefore the processing requirements for waste water is also thereupon more and more higher, and the demand as the pure clear polymerize aluminum chloride of High-efficient Water treatment additive is also increasing.
In prior art; using the aluminum-containing raw material of waste and discarded hydrochloric acid, sulfuric acid etc. inorganic acid as raw materials for production; achieve the dual function of reserved resource and protection of the environment; but production technique is comparatively complicated; and other supplementary additives of production are many, can not effective energy-conserving and environment-protective of realization truly.
Summary of the invention
The object of the invention is to for deficiency of the prior art, provide a kind of process two useless comprehensive utilization production method, obviously improve waste reprocessing utilizing status, achieve the dual function of reserved resource and protection of the environment.
For solving the problems of the technologies described above, the technical solution used in the present invention is: the useless comprehensive utilization production method of a kind of process two, to comprise the process trade mark be the aluminium mud of HW17 and the trade mark is the Waste Sulfuric Acid of HW34 or the comprehensive utilization production method of waste hydrochloric acid, its innovative point is: the described trade mark to be the treatment process of the aluminium mud of HW17 be by water content be 72 ~ 73% the trade mark be that HW17 aluminium mud is by hot-air dry desorption, becoming water content after desorption completes is 8.6 ~ 9.6%, the solid-state aluminium-containing sludge of aluminium content 98 ~ 99%, the acidity value controlling the solid-state aluminium-containing sludge after desorption is 7.8 ~ 8.2,
The described trade mark be the treatment process of the Waste Sulfuric Acid of HW34 or waste hydrochloric acid for add 3 times three (pungent-last of the ten Heavenly stems) alkyl tertiary amine extraction agents in Waste Sulfuric Acid or waste hydrochloric acid respectively, each add-on ratio is 0.6:1 ~ 1.2, and each extraction time is 3 ~ 5min;
Described method of comprehensive utilization is be that the Waste Sulfuric Acid of 0.5 ~ 0.6 ton of HW34 or waste hydrochloric acid are put in the reactor with insulation jacket by the trade mark processed, slowly add 0.5 ~ 0.6 ton of solid aluminum mud processed again, hybrid reaction obtains the polymerize aluminum chloride that purity is 30 ~ 32.7%, then successively through spraying dry and water film dedusting, pure clear polymerize aluminum chloride is obtained.
Further, the control method of described acidity value be divided into acid adjustment, alkali tune and in and tertiary treatment; Described acid adjustment step is, by acidity regulator A, the solid aluminum mud PH after desorption is adjusted to 4 ~ 5, leaves standstill 10 ~ 20min; Acid solid aluminum mud PH is adjusted to 9 ~ 10 for adding acidity regulator B by described alkali tune step, leaves standstill 20 ~ 30min; Described neutralization procedure, for pH value is adjusted to 7.8 ~ 8.2 by acidity regulator A by alkaline solid-state aluminium mud, leaves standstill 5 ~ 10min.
Further, in described method of comprehensive utilization, hybrid reaction is specially by mixture first through the reaction 2 ~ 3h that is once rapidly heated, and arranging warming temperature is 50 ~ 60 degree, and the heating-up time controls at 8 ~ 10min; The reaction that is rapidly heated terminates rear isothermal reaction 24 ~ 30h, and carry out secondary temperature elevation reaction 1 ~ 2h after insulation reaction, arranging warming temperature is 65 ~ 75 degree, and the heating-up time controls at 5 ~ 8min.
Further, the described warming temperature being once rapidly heated reaction is 57 degree; Heating-up time controls at 8.5min.
Further, described secondary be rapidly heated reaction warming temperature be 72 degree, the heating-up time controls at 6min.
Further, the described time being once rapidly heated reaction is 2.5h.
Further, described secondary be rapidly heated reaction time be 1.5h.
Further, in described hot-air dry, the temperature of warm air is 45 ~ 60 DEG C, and the hot-air dry time is 12 ~ 15h.
Beneficial effect of the present invention is as follows:
(1) the present invention has carried out unique reaction pre-treatment to the aluminum feedstock of waste and discarded hydrochloric acid, sulfuric acid, and aluminum feedstock regulates acidity process through three grades, and the detrimental impurity in raw material is precipitated through the change of PH; The extraction agent access control of spent acid, the spent acid of extraction has good purity, eliminates oils and solid impurity.
(2) the present invention using the aluminum-containing raw material of the waste of pre-treatment and discarded hydrochloric acid, sulfuric acid etc. inorganic acid as raw materials for production; while achieving the dual function of reserved resource and protection of the environment; solve complex manufacturing in prior art; and other supplementary additives of production are many, can not the problem of effective energy-conserving and environment-protective of realization truly.
(3) the present invention is for after the two process recyclings of giving up, raw material availability improves, production efficiency is high and stable, shortened short in the follow-up reaction times, adopt the reaction that is rapidly heated first, save the reaction times while ensure that production efficiency, improve reaction effect, reduce production cost.
(4) the inventive method raw material availability reaches 99.3 ~ 99.6%, in the pure clear polymerize aluminum chloride of finished product of the present invention, aluminum chloride content can reach 30 ~ 32.7%, product purity reaches 98 ~ 99%, good product mobility, do not condense phenomenon, the clearance of chemical oxygen demand COD is stabilized between 89 ~ 91%; Chroma removal rate is stabilized between 93 ~ 95%.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is elaborated.
Embodiment 1
The useless comprehensive utilization production methods of a kind of process two, comprise aluminium mud that the process trade mark is HW17 and the trade mark is the Waste Sulfuric Acid of HW34 or the comprehensive utilization production method of waste hydrochloric acid;
The present embodiment by water content be 72% the trade mark be HW17 aluminium mud by hot-air dry desorption, hot-air dry temperature is 45-60 DEG C, and time of drying is 12-15h; Becoming water content after desorption completes is 8.6%, the solid-state aluminium-containing sludge of aluminium content 98 ~ 99%, and the acidity value controlling the solid-state aluminium-containing sludge after desorption is 7.8;
Be add 3 times three (pungent-last of the ten Heavenly stems) alkyl tertiary amine extraction agents respectively in the Waste Sulfuric Acid of HW34 or waste hydrochloric acid by the trade mark, each add-on ratio is 0.6:1, and each extraction time is 3min;
Be that the Waste Sulfuric Acid of 0.5 ton or the waste hydrochloric acid of HW34 is put in the reactor with insulation jacket by the trade mark processed, slowly add 0.5 ton of solid aluminum mud processed again, hybrid reaction obtains the polymerize aluminum chloride that purity is 30%, then successively through spraying dry and water film dedusting, pure clear polymerize aluminum chloride is obtained.
Wherein, the control method of acidity value be divided into acid adjustment, alkali tune and in and tertiary treatment; Acid adjustment step is, by acidity regulator A sulfuric acid, the solid aluminum mud PH after desorption is adjusted to 4, leaves standstill 10min; Acid solid aluminum mud PH is adjusted to 9 for adding acidity regulator B carbide slag by alkali tune step, leaves standstill 20min; Neutralization procedure, for pH value is adjusted to 7.8 by acidity regulator A sulfuric acid by alkaline solid-state aluminium-containing sludge, leaves standstill 5min;
Especially, in method of comprehensive utilization, hybrid reaction adopts by mixture first through the reaction 2 ~ 3h that is once rapidly heated, and arranging warming temperature is 50 degree, and the heating-up time controls at 8min; The reaction that is rapidly heated terminates rear isothermal reaction 24h, and carry out secondary temperature elevation reaction 1h after insulation reaction, arranging warming temperature is 65 degree, and the heating-up time controls at 5min.
The method raw material availability of the present embodiment reaches 99.3%, and in the pure clear polymerize aluminum chloride of finished product, aluminum chloride content can reach 32%, and product purity reaches 98%, production process does not produce new waste, good product mobility, phenomenon of not condensing, the clearance of chemical oxygen demand COD is stabilized in 89%; Chroma removal rate is stabilized in 93%.
Embodiment 2
The useless comprehensive utilization production methods of a kind of process two, comprise aluminium mud that the process trade mark is HW17 and the trade mark is the Waste Sulfuric Acid of HW34 or the comprehensive utilization production method of waste hydrochloric acid;
The present embodiment by water content be 73% the trade mark be HW17 aluminium mud by hot-air dry desorption, hot-air dry temperature is 60 DEG C, and time of drying is 12-15h; Becoming water content after desorption completes is 9.6%, the solid aluminum mud of aluminium content 99%, and the acidity value controlling the solid-state aluminium-containing sludge after desorption is 4-5;
Be add 3 times three (pungent-last of the ten Heavenly stems) alkyl tertiary amine extraction agents respectively in the Waste Sulfuric Acid of HW34 or waste hydrochloric acid by the trade mark, each add-on ratio is 0.6:1.2, and each extraction time is 5min;
Be that the Waste Sulfuric Acid of 0.6 ton or the waste hydrochloric acid of HW34 is put in the reactor with insulation jacket by the trade mark processed, slowly add 0.5 ton of solid aluminum mud processed again, hybrid reaction obtains the polymerize aluminum chloride that purity is 32%, then successively through spraying dry and water film dedusting, pure clear polymerize aluminum chloride is obtained.
Wherein, the control method of acidity value be divided into acid adjustment, alkali tune and in and tertiary treatment; Acid adjustment step is, by acidity regulator A hydrochloric acid, the solid aluminum mud PH after desorption is adjusted to 5, leaves standstill 20min; Acid solid aluminum mud PH is adjusted to 10 for adding acidity regulator B carbide slag by alkali tune step, leaves standstill 30min; Neutralization procedure, for pH value is adjusted to 8.2 by acidity regulator A hydrochloric acid by alkaline solid-state aluminium mud, leaves standstill 10min;
Especially, in method of comprehensive utilization, hybrid reaction adopts by mixture first through the reaction 3h that is once rapidly heated, and arranging warming temperature is 60 degree, and the heating-up time controls at 10min; The reaction that is rapidly heated terminates rear isothermal reaction 30h, and carry out secondary temperature elevation reaction 2h after insulation reaction, arranging warming temperature is 75 degree, and the heating-up time controls at 8min.
The method raw material availability of the present embodiment reaches 99.6%, and in the pure clear polymerize aluminum chloride of finished product, aluminum chloride content can reach 35%, and product purity reaches 99%, production process does not produce new waste, good product mobility, phenomenon of not condensing, the clearance of chemical oxygen demand COD is stabilized in 91%; Chroma removal rate is stabilized in 95%.
Claims (6)
1. the useless comprehensive utilization production method of process two, to comprise the process trade mark be the aluminium mud of HW17 and the trade mark is the comprehensive utilization production method of the waste hydrochloric acid of HW34, it is characterized in that: the described trade mark to be the treatment process of the aluminium mud of HW17 be by water content be 72 ~ 73% the trade mark be that HW17 aluminium mud is by hot-air dry desorption, becoming water content after desorption completes is 8.6 ~ 9.6%, the solid aluminum mud of aluminium content 98 ~ 99%, the acidity value controlling the solid aluminum mud after desorption is 7.8 ~ 8.2;
The control method of described acidity value be divided into acid adjustment, alkali tune and in and tertiary treatment; Described acid adjustment step is, by acid, the solid aluminum sludge pH after desorption is adjusted to 4 ~ 5, leaves standstill 10 ~ 20min; Acid solid aluminum sludge pH is adjusted to 9 ~ 10 for adding alkali by described alkali tune step, leaves standstill 20 ~ 30min; Described neutralization procedure, for pH value is adjusted to 7.8 ~ 8.2 by acid by alkaline solid-state aluminium mud, leaves standstill 5 ~ 10min;
The described trade mark be the treatment process of the waste hydrochloric acid of HW34 for add 3 times three (pungent-last of the ten Heavenly stems) alkyl tertiary amine extraction agents in waste hydrochloric acid respectively, each add-on ratio is 0.6:1 ~ 1.2, and each extraction time is 3 ~ 5min;
Described method of comprehensive utilization is be that the waste hydrochloric acid of 0.5 ~ 0.6 ton of HW34 is put in the reactor with insulation jacket by the trade mark processed, slowly add 0.5 ~ 0.6 ton of solid aluminum mud processed again, hybrid reaction obtains the polymerize aluminum chloride that purity is 30 ~ 32.7%, then successively through spraying dry and water film dedusting, pure clear polymerize aluminum chloride is obtained;
In described method of comprehensive utilization, hybrid reaction is specially by mixture first through the reaction 2 ~ 3h that is once rapidly heated, and arranging warming temperature is 50 ~ 60 degree, and the heating-up time controls at 8 ~ 10min; The reaction that is rapidly heated terminates rear isothermal reaction 24 ~ 30h, and carry out secondary temperature elevation reaction 1 ~ 2h after insulation reaction, arranging warming temperature is 65 ~ 75 degree, and the heating-up time controls at 5 ~ 8min.
2. the useless comprehensive utilization production method of process two according to claim 1, is characterized in that: the described warming temperature being once rapidly heated reaction is 57 degree; Heating-up time controls at 8.5min.
3. the useless comprehensive utilization production method of process according to claim 2 two, is characterized in that: the be rapidly heated warming temperature of reaction of described secondary is 72 degree, and the heating-up time controls at 6min.
4. the useless comprehensive utilization production method of process two according to claim 2, is characterized in that: the described time being once rapidly heated reaction is 2.5h.
5. the useless comprehensive utilization production method of process according to claim 3 two, is characterized in that: be rapidly heated time of reaction of described secondary is 1.5h.
6. the useless comprehensive utilization production method of process two according to claim 1, it is characterized in that: in described hot-air dry, the temperature of warm air is 45 ~ 60 DEG C, the hot-air dry time is 12 ~ 15h.
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| CN104529104A (en) * | 2014-12-30 | 2015-04-22 | 新奥科技发展有限公司 | Sludge pretreatment method |
| CN104961147A (en) * | 2015-06-06 | 2015-10-07 | 李松群 | Production method of pure-clear polymeric aluminum chloride |
| CN110015678B (en) * | 2019-05-20 | 2021-07-06 | 河南爱尔福克化学股份有限公司 | Production process of concentrated polyaluminum chloride |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1367759A (en) * | 1999-08-03 | 2002-09-04 | 加拿大国家科学研究院 | Hybrid chemical and biological process for decontaminating sludge from municipal sewage |
| CN103739179A (en) * | 2013-06-24 | 2014-04-23 | 四川海普流体技术有限公司 | Sludge pre-treatment method |
| CN103819064A (en) * | 2014-03-10 | 2014-05-28 | 中钢集团武汉安全环保研究院有限公司 | Method for removing heavy metals from sludge by pickling of composite acids |
| CN103833060A (en) * | 2014-03-24 | 2014-06-04 | 南通科纯化工有限公司 | Method for producing pure poly aluminum chloride |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS63175700A (en) * | 1987-01-13 | 1988-07-20 | Mitsubishi Paper Mills Ltd | Treatment of sludge |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1367759A (en) * | 1999-08-03 | 2002-09-04 | 加拿大国家科学研究院 | Hybrid chemical and biological process for decontaminating sludge from municipal sewage |
| CN103739179A (en) * | 2013-06-24 | 2014-04-23 | 四川海普流体技术有限公司 | Sludge pre-treatment method |
| CN103819064A (en) * | 2014-03-10 | 2014-05-28 | 中钢集团武汉安全环保研究院有限公司 | Method for removing heavy metals from sludge by pickling of composite acids |
| CN103833060A (en) * | 2014-03-24 | 2014-06-04 | 南通科纯化工有限公司 | Method for producing pure poly aluminum chloride |
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