CN103950961A - Method for preparing aluminum hydroxide from industrial waste residue generated in aluminum alloy surface treatment - Google Patents
Method for preparing aluminum hydroxide from industrial waste residue generated in aluminum alloy surface treatment Download PDFInfo
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- CN103950961A CN103950961A CN201410135831.XA CN201410135831A CN103950961A CN 103950961 A CN103950961 A CN 103950961A CN 201410135831 A CN201410135831 A CN 201410135831A CN 103950961 A CN103950961 A CN 103950961A
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- aluminium hydroxide
- hydroxide
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Abstract
A method for preparing aluminum hydroxide from an industrial waste residue generated in aluminum alloy surface treatment is provided. The method comprises the following steps: (1) leaching an aluminum element in the industrial waste residue with an alkaline aqueous solution; (2) carrying out solid-liquid separation to obtain an aluminum-containing filtrate; (3) adjusting the pH value of the filtrate with an acid, and precipitating to obtain aluminum hydroxide; and (4) carrying out solid-liquid separation, to obtain an aluminum hydroxide solid precipitate. The method can efficiently separate and recycle the aluminum element in the aluminum alloy surface treatment industrial waste residue, and realizes resource utilization of the aluminum alloy surface treatment industrial waste residue.
Description
Technical field
The present invention relates to the production method of aluminium hydroxide, belong to waste residue resource in aluminum alloy surface processing industry and utilize field, particularly a kind of industrial residue producing with aluminum alloy surface treating processes is prepared the method for aluminium hydroxide.
Background technology
Aluminium alloy is at present output maximum, most widely used non-ferrous metal in the world.For improving aluminum alloy surface corrosion resisting property, improve that it is ornamental and functional, aluminium alloy must carry out surface treatment before dispatching from the factory.The annual aluminum alloy surface producing of China is processed the about millions of tons of industrial residue, and most processing modes that adopt discarded landfill, not only cause the waste of bauxite resource, also bring serious secondary pollution.Therefore the recycling of aluminum alloy surface processing industrial residue receives increasing concern.
As CN102351224A discloses a kind of processing method of preparing active alumina from aluminum section industrial wastewater alkaline residues, obtain activated alumina by steps such as washing, grinding, oven dry, granulation, dry, calcinings.CN102503208A discloses a kind of method of utilizing aluminum section industrial wastewater alkaline residues to prepare high strength cement fine powder additive, by add additive to calcine and ball-milling processing to alkaline residue, obtains the fine powder that can be used as high strength cement additive.
The main component of aluminum alloy surface processing is the incomplete hydrated alumina of crystallization and part amorphous body, also has some metal-salts (nickel, copper, tin, iron etc.), inorganic impurity and organic impurity etc., and wherein the tool recycling of aluminium element is worth.Aluminium hydroxide is a kind of important environmental protection inorganic fire retardant, it have fire-retardant, eliminate smoke, fill three large functions, and under nontoxic, good stability, high temperature, do not produce toxic gas, the endothermic temperature lower (235～350 DEG C) that dewaters, can with the feature such as many kinds of substance synergy.Current global aluminium hydroxide fire retardant consumption exceedes 600,000 tons/year, accounts for the more than 80% of inorganic combustion inhibitor consumption.
At present, the production method of aluminium hydroxide is raw material mainly with bauxite greatly, the report that also useful aluminium ash, aluminium powder are raw material, but taking aluminum alloy surface treating processes produce industrial residue as the technology of raw material production aluminium hydroxide also rarely found.
Processing separation and purification aluminium hydroxide industrial residue from aluminum alloy surface is the feasible way of realizing containing aluminium industrial residue recycling, carry out high efficiency separation recovery by the aluminium element that aluminum alloy surface is processed in industrial residue, can realize the reasonable recycling of bauxite resource in industrial residue, create good Social benefit and economic benefit.
Summary of the invention
The present invention is directed to existing aluminum alloy surface processing industrial residue and be difficult to the problem reclaiming, resource utilization is not high, provide a kind of and turn waste into wealth, technique simply processes from aluminum alloy surface the method for extracting aluminium hydroxide the industrial residue producing, reaches the object that realizes changing rejected material to useful resource regeneration, improves resource utilization.
For achieving the above object, the present invention adopts following technical scheme:
Process with aluminum alloy surface the method that the industrial residue producing is prepared aluminium hydroxide, comprise the following steps:
(1) with the aluminium element in alkaline aqueous solution lixiviate industrial residue;
(2) carry out solid-liquid separation, obtain containing aluminium filtrate;
(3) regulate filtrate pH value, precipitated aluminium hydroxide with acid;
(4) carry out solid-liquid separation, obtain aluminium hydroxide solid precipitation.
Aluminum alloy surface is processed industrial residue in leaching process, and the aluminium hydroxide in industrial residue and alkali reaction generate meta-aluminate; While regulating filtrate pH value with acid, meta-aluminate and acid-respons, generate aluminium hydroxide.Through the operation of this two step, the impurity in industrial residue is removed as silicon-dioxide, ironic hydroxide, magnesium hydroxide etc., thereby can obtain the aluminium hydroxide product with higher degree.
As optimal technical scheme, method of the present invention, described industrial residue is the waste residue producing in aluminum alloy surface treating processes.
Al in industrial residue of the present invention (OH)
3the weight percentage of giving money as a gift is not particularly limited, but Al (OH) in preferred described industrial residue
3weight percentage>=30% of giving money as a gift, for example, be 35%, 42%, 48%, 55%, 65% etc., more preferably>=50%.In addition, if water content is too high to such an extent as to affect subsequent operations in industrial residue, can first use equipment for separating liquid from solid processing, reduce water content.
As optimal technical scheme, method of the present invention, described in step (1), alkaline aqueous solution is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution.
Preferably, the usage quantity of described alkaline aqueous solution for make in industrial residue aluminium hydroxide with to add the mol ratio of hydroxide ion be 1:1～1:4, be for example 1:1.5,1:2,1:2.5,1:3,1:3.5,1:3.8 etc., be preferably 1:2～1:3.In industrial residue aluminium hydroxide with add hydroxide ion mol ratio during lower than 1:1, aluminium hydroxide cannot dissolve completely, aluminium hydroxide extraction yield is low; During higher than 1:4, sodium hydroxide is seriously superfluous, not only causes waste, and can increase sour usage quantity in the time that next step uses acid to regulate filtrate pH value, causes waste, and produces a large amount of waste water.
As optimal technical scheme, method of the present invention, described in step (1), the temperature of lixiviate is room temperature～90 DEG C, for example, be 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 85 DEG C etc., is preferably 50～70 DEG C.When temperature is too low, abstraction reaction is carried out slowly, and production efficiency is low; When excess Temperature, solution evaporation loss amount is large, and energy expenditure is large, and production cost is high.
Preferably, the time of described lixiviate is 10min～120min, for example, be 20min, 40min, 50min, 60min, 65min, 80min, 95min, 110min etc., is preferably 35min～70min.Time is too short, and reaction is carried out not exclusively, and aluminium hydroxide extraction yield is low; Overlong time, production cost is high.
As optimal technical scheme, method of the present invention, described in step (3), acid is the one kind or two or more mixing in sulfuric acid, hydrochloric acid or nitric acid, or passes into CO
2regulate pH value.
Preferably, temperature when described adjusting filtrate pH value is 10～60 DEG C, for example, be 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 55 DEG C etc., is preferably 20～40 DEG C.When temperature is too low, abstraction reaction is carried out slowly, and production efficiency is low; When excess Temperature, solution evaporation loss amount is large, and energy expenditure is large, and production cost is high.
Preferably, described pH value is adjusted to 4.5～7.0, for example, be 4.7,5.0,5.3,5.6,5.9,6.2,6.5,6.8 etc., is preferably 5.0～6.0.PH value is too low, the aluminium hydroxide of generation can with excessive acid-respons, generate aluminium salt, not only yield poorly, and cause sour waste; PH is too high, and meta-aluminate does not change into aluminium hydroxide completely, yields poorly.
Separation method in the present invention is not specifically limited, can use the separate mode of any applicable the inventive method, as optimal technical scheme, method of the present invention, described separation adopts the one kind or two or more combination in centrifugation, vacuum filtration device suction filtration, filter press.
As optimal technical scheme, method of the present invention, also comprises the steps:
(5) wash precipitation with water;
(6) dry.
Preferably, the described water of step (5) is process water and/or deionized water; The number of times of described washing, more than 1 time, is preferably 3 times.
Preferably, the time of described water washing precipitation is 20min～60min at every turn, for example, be 25min, 30min, 35min, 40min, 45min, 50min, 55min etc., is preferably 30～40min.The time of water washing precipitation is too short, and impurity is removed not exclusively; Overlong time, production cost is high.
As optimal technical scheme, method of the present invention, comprises the steps:
(1) at room temperature～90 DEG C, soak industrial residue 10min～120min with alkaline aqueous solution; The usage quantity of described alkaline aqueous solution for make in industrial residue aluminium hydroxide with to add the mol ratio of hydroxide ion be 1:1～1:4;
(2) solution that soaks industrial residue gained with alkaline aqueous solution is carried out to solid-liquid separation, obtain containing aluminium filtrate;
(3) gained filtrate is regulated at 10～60 DEG C to pH value to 4.5～7.0, precipitated aluminium hydroxide;
(4) solution of aluminium hydroxide precipitation is carried out to solid-liquid separation, obtain aluminium hydroxide solid precipitation;
(5) aluminium hydroxide solid precipitation is washed 3 times with water to each 20min～60min;
(6) the aluminium hydroxide solid precipitation through washing is dried, obtain aluminium hydroxide product.
The present invention compared with prior art, the present invention can effectively utilize the industrial residue, the minimizing aluminum alloy surface that in aluminum alloy surface treating processes, produce to process the pollution of industrial residue to environment, have advantages of that technical process is short, the aluminium element rate of recovery is high in industrial residue, the aluminium element rate of recovery can reach more than 90%, and the purity of gained aluminium hydroxide product more than 85%, can meet the application in the fields such as fire retardant, material of construction, synthetic rubber, coating completely.
Brief description of the drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment helps to understand the present invention, should not be considered as concrete restriction of the present invention.
Process flow sheet of the present invention is shown in Fig. 1.
Embodiment 1
(1) at 60 DEG C, soak industrial residue 60min with aqueous sodium hydroxide solution, the add-on of aqueous sodium hydroxide solution for make in industrial residue aluminium hydroxide with to add the mol ratio of hydroxide ion be 1:2.5;
(2) solution of the aqueous solution soaking industrial residue gained with alkali is used to vacuum filtration device suction filtration, obtain containing aluminium filtrate;
(3) at 30 DEG C, add sulphuric acid soln pH value to be adjusted to 5.0, precipitated aluminium hydroxide suction filtration gained filtrate;
(4) solution of aluminium hydroxide precipitation is used to vacuum filtration device suction filtration, obtain aluminium hydroxide solid precipitation;
(5) aluminium hydroxide solid precipitation is washed 3 times with water to each 50min;
(6) the aluminium hydroxide solid precipitation through washing is dried, obtain aluminium hydroxide product.
Embodiment 2
(1) at 70 DEG C, soak industrial residue 45min with aqueous sodium hydroxide solution, the add-on of aqueous sodium hydroxide solution for make in industrial residue aluminium hydroxide with to add the mol ratio of hydroxide ion be 1:2;
(2) solution of the aqueous solution soaking industrial residue gained with alkali is carried out to vacuum filtration device suction filtration, obtain containing aluminium filtrate;
(3) suction filtration gained filtrate is passed into CO at 20 DEG C
2pH value is adjusted to 6.0, precipitated aluminium hydroxide;
(4) solution of aluminium hydroxide precipitation is carried out to vacuum filtration device suction filtration, obtain aluminium hydroxide solid precipitation;
(5) aluminium hydroxide solid precipitation is washed 3 times with water to each 60min;
(6) the aluminium hydroxide solid precipitation through washing is dried, obtain aluminium hydroxide product.
Embodiment 3
(1) at 25 DEG C, soak industrial residue 120min with potassium hydroxide aqueous solution, the add-on of potassium hydroxide aqueous solution for make in industrial residue aluminium hydroxide with to add the mol ratio of hydroxide ion be 1:4;
(2) solution of the aqueous solution soaking industrial residue gained with alkali is carried out to centrifugation, obtain containing aluminium filtrate;
(3) at 10 DEG C, add hydrochloric acid soln pH value to be adjusted to 4.5, precipitated aluminium hydroxide suction filtration gained filtrate;
(4) solution of aluminium hydroxide precipitation is used to filter press, obtain aluminium hydroxide solid precipitation;
(5) aluminium hydroxide solid precipitation is washed 5 times with water to each 20min;
(6) the aluminium hydroxide solid precipitation through washing is dried, obtain aluminium hydroxide product.
Embodiment 4
(1) at 90 DEG C, soak industrial residue 10min with aqueous sodium hydroxide solution, the add-on of aqueous sodium hydroxide solution for make in industrial residue aluminium hydroxide with to add the mol ratio of hydroxide ion be 1:1;
(2) solution of the aqueous solution soaking industrial residue gained with alkali is used to filter press, obtain containing aluminium filtrate;
(3) at 60 DEG C, add sulphuric acid soln pH value to be adjusted to 7.0, precipitated aluminium hydroxide suction filtration gained filtrate;
(4) solution of aluminium hydroxide precipitation is carried out to centrifugation, obtain aluminium hydroxide solid precipitation;
(5) aluminium hydroxide solid precipitation is washed 4 times with water to each 30min;
(6) the aluminium hydroxide solid precipitation through washing is dried, obtain aluminium hydroxide product.
Applicant's statement, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, and the selections of the equivalence replacement to the each raw material of product of the present invention and the interpolation of ancillary component, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (9)
1. process with aluminum alloy surface the method that the industrial residue producing is prepared aluminium hydroxide, comprise the following steps:
(1) with the aluminium element in alkaline aqueous solution lixiviate industrial residue;
(2) carry out solid-liquid separation, obtain containing aluminium filtrate;
(3) regulate filtrate pH value, precipitated aluminium hydroxide with acid;
(4) carry out solid-liquid separation, obtain aluminium hydroxide solid precipitation.
2. method according to claim 1, is characterized in that, described industrial residue is the waste residue producing in aluminum alloy surface treating processes.
3. method according to claim 1 and 2, is characterized in that, described in step (1), alkaline aqueous solution is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution;
Preferably, the usage quantity of described alkaline aqueous solution for make in industrial residue aluminium hydroxide with to add the mol ratio of hydroxide ion be 1:1～1:4, be preferably 1:2～1:3.
4. according to the method described in claim 1-3 any one, it is characterized in that, described in step (1), the temperature of lixiviate is room temperature～90 DEG C, is preferably 50～70 DEG C;
Preferably, the time of described lixiviate is 10min～120min, is preferably 35min～70min.
5. according to the method described in claim 1-4 any one, it is characterized in that, described in step (3), acid is the one kind or two or more mixing in sulfuric acid, hydrochloric acid or nitric acid, or passes into CO
2regulate pH value;
Preferably, temperature when described adjusting filtrate pH value is 10～60 DEG C, is preferably 20～40 DEG C;
Preferably, described pH value is adjusted to 4.5～7.0, is preferably 5.0～6.0.
6. according to the method described in claim 1-5 any one, it is characterized in that, described separation adopts the one kind or two or more combination in centrifugation, vacuum filtration device suction filtration, filter press.
7. according to the method described in claim 1-6 any one, it is characterized in that, also comprise the steps:
(5) wash precipitation with water;
(6) dry.
8. method according to claim 7, is characterized in that, the described water of step (5) is process water and/or deionized water; The number of times of described washing, more than 1 time, is preferably 3 times;
Preferably, the time of described water washing precipitation is 20min～60min at every turn, is preferably 30～40min.
9. method according to claim 1, is characterized in that, comprises the steps:
(1) at room temperature～90 DEG C, soak industrial residue 10min～120min with alkaline aqueous solution; The usage quantity of described alkaline aqueous solution for make in industrial residue aluminium hydroxide with to add the mol ratio of hydroxide ion be 1:1～1:4;
(2) solution that soaks industrial residue gained with alkaline aqueous solution is carried out to solid-liquid separation, obtain containing aluminium filtrate;
(3) gained filtrate is regulated at 10～60 DEG C to pH value to 4.5～7.0, precipitated aluminium hydroxide;
(4) solution of aluminium hydroxide precipitation is carried out to solid-liquid separation, obtain aluminium hydroxide solid precipitation;
(5) aluminium hydroxide solid precipitation is washed 3 times with water to each 20min～60min;
(6) the aluminium hydroxide solid precipitation through washing is dried, obtain aluminium hydroxide product.
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| CN201410135831.XA CN103950961A (en) | 2014-04-04 | 2014-04-04 | Method for preparing aluminum hydroxide from industrial waste residue generated in aluminum alloy surface treatment |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106590689A (en) * | 2016-12-26 | 2017-04-26 | 荆门市格林美新材料有限公司 | Method for preparing composite flame retardant through recovering aluminum and magnesium from different types of sludge |
| CN107381526A (en) * | 2017-07-11 | 2017-11-24 | 高嵘 | Spent acid processing method after aluminium section bar and aluminium alloy cleaning |
| CN109292745A (en) * | 2018-08-28 | 2019-02-01 | 杭州轩辉环境设备有限公司 | Aluminum ions process in a kind of removal phosphoric acid solution |
| CN109650419A (en) * | 2017-10-10 | 2019-04-19 | 广东科达洁能股份有限公司 | The method and system that a kind of pair of Aluminum sludge is comprehensively utilized |
| CN110760706A (en) * | 2018-07-26 | 2020-02-07 | 中国科学院过程工程研究所 | Method for preparing copper-containing aluminum alloy by recycling aviation industry aluminum alloy waste |
| CN111020221A (en) * | 2019-12-11 | 2020-04-17 | 深圳雅居乐环保科技有限公司 | Method for preparing aluminum smelting composite fluxing agent by using aluminum alkaline residues |
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| CN1287186A (en) * | 1999-09-06 | 2001-03-14 | 谭红卫 | Treatment of waste alkali solution and settled sludge after chemical milling |
| CN1350065A (en) * | 2000-10-19 | 2002-05-22 | 中国科学院福建物质结构研究所 | Comprehensive utilization of waste from aluminium smeltery |
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2014
- 2014-04-04 CN CN201410135831.XA patent/CN103950961A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1287186A (en) * | 1999-09-06 | 2001-03-14 | 谭红卫 | Treatment of waste alkali solution and settled sludge after chemical milling |
| CN1350065A (en) * | 2000-10-19 | 2002-05-22 | 中国科学院福建物质结构研究所 | Comprehensive utilization of waste from aluminium smeltery |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106590689A (en) * | 2016-12-26 | 2017-04-26 | 荆门市格林美新材料有限公司 | Method for preparing composite flame retardant through recovering aluminum and magnesium from different types of sludge |
| CN106590689B (en) * | 2016-12-26 | 2018-06-19 | 荆门市格林美新材料有限公司 | The method that magnalium prepares composite flame-retardant agent is recycled from different sludge |
| CN107381526A (en) * | 2017-07-11 | 2017-11-24 | 高嵘 | Spent acid processing method after aluminium section bar and aluminium alloy cleaning |
| CN109650419A (en) * | 2017-10-10 | 2019-04-19 | 广东科达洁能股份有限公司 | The method and system that a kind of pair of Aluminum sludge is comprehensively utilized |
| CN110760706A (en) * | 2018-07-26 | 2020-02-07 | 中国科学院过程工程研究所 | Method for preparing copper-containing aluminum alloy by recycling aviation industry aluminum alloy waste |
| US11939644B2 (en) | 2018-07-26 | 2024-03-26 | The Boeing Company | Method for regenerating copper-containing aluminum alloy from aluminum alloy scrap |
| CN109292745A (en) * | 2018-08-28 | 2019-02-01 | 杭州轩辉环境设备有限公司 | Aluminum ions process in a kind of removal phosphoric acid solution |
| CN109292745B (en) * | 2018-08-28 | 2021-09-24 | 杭州轩辉环境设备有限公司 | Process method for removing aluminum ions in phosphoric acid solution |
| CN111020221A (en) * | 2019-12-11 | 2020-04-17 | 深圳雅居乐环保科技有限公司 | Method for preparing aluminum smelting composite fluxing agent by using aluminum alkaline residues |
| CN111020221B (en) * | 2019-12-11 | 2022-04-05 | 广州雅居乐固体废物处理有限公司 | Method for preparing aluminum smelting composite fluxing agent by using aluminum alkaline residues |
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Application publication date: 20140730 |