CN113336251A - Method for producing high-purity alumina from electrode foil waste sulfuric acid - Google Patents
Method for producing high-purity alumina from electrode foil waste sulfuric acid Download PDFInfo
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- CN113336251A CN113336251A CN202110786713.5A CN202110786713A CN113336251A CN 113336251 A CN113336251 A CN 113336251A CN 202110786713 A CN202110786713 A CN 202110786713A CN 113336251 A CN113336251 A CN 113336251A
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- sulfuric acid
- waste sulfuric
- purity alumina
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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Abstract
The invention relates to the technical field of waste sulfuric acid purification, and discloses a method for producing high-purity alumina by using electrode foil waste sulfuric acid, which comprises the following steps: s1, filtering the waste sulfuric acid by a filter membrane; s2, adding ammonia water into the generated concentrated waste liquid to adjust the pH value; s3, cooling, evaporating and crystallizing to generate aluminum ammonium sulfate; s4, calcining the ammonium aluminum sulfate to generate the high-purity alumina. Solves the problems of solid waste slag generation and high treatment cost in the prior art.
Description
Technical Field
The invention relates to the technical field of waste sulfuric acid purification, in particular to a method for producing high-purity aluminum oxide by using electrode foil waste sulfuric acid.
Background
In the production process of the electrode foil, a lot of waste liquid is generated and discharged, the existing situation is that the discharged waste liquid is mainly a mixture of sulfuric acid and aluminum sulfate, enterprises need to treat the mixture before discharging, and at present, ninety percent of processes in the treatment field adopt lime to neutralize waste residue and discharge, so that a large amount of solid waste residue is generated, the environment is polluted, and a large amount of treatment cost is paid.
Disclosure of Invention
The invention aims to provide a method for producing high-purity alumina from electrode foil waste sulfuric acid, which solves the problems of solid waste slag generation and high treatment cost in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for producing high-purity alumina by using electrode foil waste sulfuric acid comprises the following steps:
s1, filtering the waste sulfuric acid by a filter membrane;
s2, adding ammonia water into the generated concentrated waste liquid to adjust the pH value;
s3, cooling, evaporating and crystallizing to generate aluminum ammonium sulfate;
s4, calcining the ammonium aluminum sulfate to generate the high-purity alumina.
Further, the filtering membrane comprises a first-stage filtering membrane and a second-stage nano filtering membrane, and the waste sulfuric acid is filtered twice.
Further, pure sulfuric acid is generated after the filtration in step S1, and the pure sulfuric acid is recycled.
Further, the PH adjusted in step S2 is 4.5.
Further, the method for preparing the high-purity alumina by the thermal decomposition of the aluminum ammonium sulfate comprises the following steps:
a1, adding aluminum sulfate and ammonia water into a synthesis reactor for neutralization;
a2, cooling and crystallizing the neutralized product;
a3, filtering and washing the crystallized articles;
a4, adding pure water to dissolve crystals, and further cooling and crystallizing;
a5, further filtering to generate ammonium aluminum sulfate and mother liquor, and returning the filtered mother liquor to the step A4 for treatment;
a6, carrying out dehydration roasting decomposition treatment on the aluminum ammonium sulfate, and inputting the generated tail gas into the step A1 through a recovery tower.
The invention has the beneficial effects that:
by applying the method, enterprises reduce the treatment cost and do not generate solid waste residues; the resource recycling is realized, and the zero emission is finally achieved; the enterprise saves about 1000 ten thousand of processing cost; the environmental protection is improved, no solid waste is discharged, and the secondary pollution is reduced; the amount of recovered product is increased, resulting in benefits.
Drawings
FIG. 1 is a flow chart of the process for producing high purity alumina from waste sulfuric acid according to the present invention;
FIG. 2 is a process flow diagram of the method for preparing high-purity alumina by thermal decomposition of aluminum ammonium sulfate according to the present invention.
Detailed Description
Example 1:
as shown in fig. 1-2, this embodiment provides a method for producing high-purity alumina from electrode foil waste sulfuric acid, which includes the following steps:
s1, filtering the waste liquid containing the waste sulfuric acid by a filter membrane;
s2, adding ammonia water into the generated concentrated waste liquid to adjust the pH value; the PH adjusted in step S2 was 4.5.
After ammonia water is added, aluminum sulfate and ammonium sulfate are produced, and the aluminum sulfate and the ammonium sulfate further react to generate aluminum ammonium sulfate. The chemical reaction formula is as follows: al2(SO4)4+ (NH4)2SO4+12H2O → 2NH4Al (SO4) 2.12H 2O
S3, cooling, evaporating and crystallizing to generate aluminum ammonium sulfate;
s4, calcining the ammonium aluminum sulfate to generate the high-purity alumina.
The filtering membrane comprises a first-stage filtering membrane and a second-stage nano filtering membrane, and the waste sulfuric acid is filtered twice.
Pure sulfuric acid is also generated after the filtration in the step S1, and the pure sulfuric acid is recycled.
When the pH is adjusted to be more than 7, aluminum hydroxide is generated.
Also comprises a method for preparing high-purity alumina by thermal decomposition of aluminum ammonium sulfate, which comprises the following steps:
a1, adding aluminum sulfate and ammonia water into a synthesis reactor for neutralization;
a2, cooling and crystallizing the neutralized product; the cooled crystals are aluminum ammonium sulfate and ammonium sulfate.
A3, filtering and washing the crystallized articles; this step filters and washes away impurities in the aluminum ammonium sulfate.
A4, adding pure water to dissolve crystals, further cooling for crystallization, and further purifying;
a5, further filtering to generate ammonium aluminum sulfate and mother liquor, and returning the filtered mother liquor to the step A4 for treatment;
a6, carrying out dehydration roasting decomposition treatment on the aluminum ammonium sulfate, and inputting the generated tail gas into the step A1 through a recovery tower. The tail gas generated is ammonia gas, and the ammonia gas is input into the synthesis reactor again.
Example 2:
in this example, a test is performed on the basis of the method in example 1, and 1000L of waste liquid containing 2N sulfuric acid and 1N aluminum ions is filtered by a membrane to produce 600L of 2N sulfuric acid, which is returned to the factory for further use; adding 25% ammonia water 85L to neutralize the remaining 400L mixed solution, evaporating the neutralized filtrate, cooling to crystallize about 25Kg of aluminum ammonium sulfate, and calcining to obtain 16Kg of alumina.
Finally, it should be noted that: the above are merely preferred embodiments of the present invention, and are not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. The method for producing high-purity alumina by using electrode foil waste sulfuric acid is characterized by comprising the following steps of:
s1, filtering the waste sulfuric acid by a filter membrane;
s2, adding ammonia water into the generated concentrated waste liquid to adjust the pH value;
s3, cooling, evaporating and crystallizing to generate aluminum ammonium sulfate;
s4, calcining the ammonium aluminum sulfate to generate the high-purity alumina.
2. The method for producing high-purity alumina from electrode foil waste sulfuric acid as claimed in claim 1, wherein the filtering membranes comprise a primary filtering membrane and a secondary nano-filtering membrane, and the waste sulfuric acid is filtered twice.
3. The method for producing high-purity aluminum oxide from electrode foil waste sulfuric acid as claimed in claim 2, wherein pure sulfuric acid is generated after filtering in step S1, and the pure sulfuric acid is recycled.
4. The method for producing high-purity alumina from electrode foil waste sulfuric acid as claimed in claim 3, wherein the pH value adjusted in step S2 is 4.5.
5. The method for producing high-purity alumina by using the electrode foil waste sulfuric acid as claimed in claim 4, which is characterized by further comprising a method for preparing high-purity alumina by thermal decomposition of aluminum ammonium sulfate, and the steps are as follows:
a1, adding aluminum sulfate and ammonia water into a synthesis reactor for neutralization;
a2, cooling and crystallizing the neutralized product;
a3, filtering and washing the crystallized articles;
a4, adding pure water to dissolve crystals, and further cooling and crystallizing;
a5, further filtering to generate ammonium aluminum sulfate and mother liquor, and returning the filtered mother liquor to the step A4 for treatment;
a6, carrying out dehydration roasting decomposition treatment on the aluminum ammonium sulfate, and inputting the generated tail gas into the step A1 through a recovery tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110786713.5A CN113336251A (en) | 2021-07-12 | 2021-07-12 | Method for producing high-purity alumina from electrode foil waste sulfuric acid |
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| CN202110786713.5A CN113336251A (en) | 2021-07-12 | 2021-07-12 | Method for producing high-purity alumina from electrode foil waste sulfuric acid |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103241754A (en) * | 2013-05-16 | 2013-08-14 | 贵阳一晶相光电科技有限公司 | Production method of high-purity aluminum oxide |
| CN204824284U (en) * | 2015-08-13 | 2015-12-02 | 唐山紫天化工防腐有限公司 | Sulphuric acid and aluminium ion recovery unit of aluminum alloy oxidation groove waste liquid |
| CN108178174A (en) * | 2016-12-08 | 2018-06-19 | 郑州大学 | A kind of method that sapphire grade high purity aluminium oxide is prepared using anodic oxidation of aluminiun materials waste liquid |
| CN110217931A (en) * | 2019-07-01 | 2019-09-10 | 苏州聚微环保科技有限公司 | A kind of recycling treatment process of spent acid |
| CN212559486U (en) * | 2020-06-12 | 2021-02-19 | 北京水木方科技有限公司 | Aluminum-containing waste sulfuric acid recovery equipment |
-
2021
- 2021-07-12 CN CN202110786713.5A patent/CN113336251A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103241754A (en) * | 2013-05-16 | 2013-08-14 | 贵阳一晶相光电科技有限公司 | Production method of high-purity aluminum oxide |
| CN204824284U (en) * | 2015-08-13 | 2015-12-02 | 唐山紫天化工防腐有限公司 | Sulphuric acid and aluminium ion recovery unit of aluminum alloy oxidation groove waste liquid |
| CN108178174A (en) * | 2016-12-08 | 2018-06-19 | 郑州大学 | A kind of method that sapphire grade high purity aluminium oxide is prepared using anodic oxidation of aluminiun materials waste liquid |
| CN110217931A (en) * | 2019-07-01 | 2019-09-10 | 苏州聚微环保科技有限公司 | A kind of recycling treatment process of spent acid |
| CN212559486U (en) * | 2020-06-12 | 2021-02-19 | 北京水木方科技有限公司 | Aluminum-containing waste sulfuric acid recovery equipment |
Non-Patent Citations (2)
| Title |
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| 殷永泉等: "高纯超细氧化铝的清洁生产工艺", 《化工环保》 * |
| 陈虹等: "溶液酸度对于从含铝废液中回收硫酸铝铵的影响", 《浙江化工》 * |
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Application publication date: 20210903 |