CN104445323A - Preparation method of porous activated aluminum oxide adsorbing material - Google Patents
Preparation method of porous activated aluminum oxide adsorbing material Download PDFInfo
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- CN104445323A CN104445323A CN201410657181.5A CN201410657181A CN104445323A CN 104445323 A CN104445323 A CN 104445323A CN 201410657181 A CN201410657181 A CN 201410657181A CN 104445323 A CN104445323 A CN 104445323A
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- adsorbing material
- preparation
- activated alumina
- aluminum oxide
- alumina porous
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 15
- 230000032683 aging Effects 0.000 claims abstract description 14
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 229910001648 diaspore Inorganic materials 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 8
- 230000000694 effects Effects 0.000 claims abstract description 6
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims abstract description 6
- 239000004411 aluminium Substances 0.000 claims description 15
- 229910052782 aluminium Inorganic materials 0.000 claims description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- JKXCZYCVHPKTPK-UHFFFAOYSA-N hydrate;trihydrochloride Chemical compound O.Cl.Cl.Cl JKXCZYCVHPKTPK-UHFFFAOYSA-N 0.000 claims description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 9
- 229910052708 sodium Inorganic materials 0.000 claims description 9
- 239000011734 sodium Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 6
- 241000370738 Chlorion Species 0.000 claims description 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 5
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 5
- 230000007062 hydrolysis Effects 0.000 claims description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims description 5
- 238000001935 peptisation Methods 0.000 claims description 5
- 238000004033 diameter control Methods 0.000 claims description 2
- 230000029087 digestion Effects 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000006227 byproduct Substances 0.000 abstract description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 2
- 239000002253 acid Substances 0.000 abstract 1
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 abstract 1
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- -1 sodium tetrachloroaluminate Chemical compound 0.000 abstract 1
- 229910001538 sodium tetrachloroaluminate Inorganic materials 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 6
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 159000000013 aluminium salts Chemical class 0.000 description 2
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention relates to a preparation method of a porous activated aluminum oxide adsorbing material. The preparation method comprises the following steps: (1) dissolving and hydrolyzing solid sodium tetrachloroaluminate by using an ethanol water solution; (2) adding water into an obtained solution to generate aluminum trichloride hexahydrate; (3) adding ammonia water for reaction to generate hydrated alumina suspension liquid, and ageing to obtain alpha-diaspore; (4) peptizing by using acid to obtain sol, dropwise adding the sol into an oil-ammonia column by adopting a dripping method, allowing the sol to retract to form balls under the effect of a surface tensile force in oil, putting the balls into ammonia water, neutralizing and ageing to form hard gel ball-like substances, washing away oil ammonia by using water and drying; and (5) baking to obtain the porous activated aluminum oxide adsorbing material. The preparation method disclosed by the invention can be used for solving the problems of wastewater treatment, improving cyclic utilization of resources, realizing value maximization and increasing the additional value of byproducts; the porous activated aluminum oxide adsorbing material is good in thermal stability at high temperature, large in specific surface area, good in adsorption performance, simple in production process, convenient to operate, low in cost and basically free of environmental pollution from aspect of production technology.
Description
Technical field
The present invention relates to activated alumina and prepare field, particularly to utilize trade effluent to prepare high temperature resistant for one, the preparation method of the activated alumina porous adsorbing material of high-specific surface area.
Background technology
Aluminium goes out the maximum metal of iron and steel external application amount in the world at present, all be widely used in all trades and professions, shorter to the cycle of losing use value from finished product, particularly in the fertilizer of chemical industry, contain various aluminium salt, if insufficient utilization, being not only the very big pollution to environment, is also the significant wastage of limited resources.
In the evolution of modern industry, often produce the various by product containing aluminium element, its utility value low and in process of production as by product occur and often output is huge, we can be translated into by various means the activated alumina product that added value is high, range of application is wide.
Activated alumina is as the important chemical materials in development of modern industry process, it is the solid material of a kind of porousness, high degree of dispersion, there is very large surface-area, its micropore surface possesses the characteristic required by katalysis, as absorption property, surfactivity, excellent thermostability etc., so be used to widely make sorbent material, siccative and catalyzer and support of the catalyst in the industry such as chemical industry, petrochemical industry, Sweet natural gas and chemical fertilizer.
Therefore making full use of the aluminium salt of industrial waste, carry out the activated alumina of production high added value, is making full use of efficient resource, is also the very big help to reducing discharging, maintaining ecotope.
Summary of the invention
Technical problem to be solved by this invention provides a kind of high high-temp stability good for above-mentioned prior art, the preparation method of the activated alumina porous adsorbing material of high-specific surface area, with for the discharge of industrial aluminium wastewater and insufficient utilization of aluminium element, and the production cost of existing activated alumina and regeneration.
The present invention solves the problems of the technologies described above adopted technical scheme: the preparation method of activated alumina porous adsorbing material, comprises following steps:
1) the excessive aqueous ethanolic solution of solid sodium terachloroaluminate is dissolved hydrolysis, the insoluble sodium-chlor of filtered and recycled;
2) again toward step 1) add appropriate water in the solution of gained, generate the six trichloride hydrate aluminium being insoluble to ethanol;
3) step 2) gained six trichloride hydrate aluminium adds ammoniacal liquor water generation reaction and closes aluminum oxide suspension, then carry out aging, make it to become α-diaspore, and washing is to without chlorion;
4) the sour peptization of α-diaspore is become the good colloidal sol of flowing property, in dripping method instillation oil ammonia column, in oil, shrink balling-up by surface tension effects, then enter in ammoniacal liquor, after neutralizing and be aging, form harder gelatinous ball thing, after washing oily ammonia, carry out drying;
5) gained Aluminium hydroxide roasting is obtained activated alumina porous adsorbing material.
By such scheme, step 1) temperature of reaction control at 20-60 DEG C, stirring velocity 300-500rpm.
By such scheme, step 3) described aging reaction pH controls at 8-9, digestion time 2-24h.
By such scheme, step 4) diameter control of described gelatinous ball thing is at 1-3mm, and drying temperature is 60-100 DEG C.
By such scheme, step 5) maturing temperature control at 500-1000 DEG C.
The present invention utilizes the trade effluent containing sodium terachloroaluminate to dissolve by extracting the excessive water-ethanol that has of solid sodium terachloroaluminate, the water-ethanol that has herein need be excessive, thus get rid of the impact of sodium ion, temperature of reaction controls at 20-60 DEG C, stirring velocity 300-500rpm.
The present invention compared with the prior art, is utilize containing aluminium salt---the trade effluent of sodium terachloroaluminate, to extract sodium terachloroaluminate solid, then generates sodium-chlor and aluminum chloride with there being water-ethanol to dissolve.And then prepare activated alumina with pseudo-boehmite, its process can be shown with following Fig. 1, from the present invention from raw material, solves a difficult problem for wastewater treatment and improves the recycle of limited resources, making value maximization, add the added value of by product; From product, it is good that the activated alumina porous adsorbing material prepared possesses high high-temp stability, and specific surface area is large, and absorption property is good; From production technique, technique is simple, easy to operate, with low cost, basic non-environmental-pollution.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention will be further described in detail, but this explanation can not be construed as limiting the invention.
Embodiment 1
(1) the excessive aqueous ethanolic solution of 19.2g solid sodium terachloroaluminate is dissolved hydrolysis, the insoluble sodium-chlor of filtered and recycled.This process reaction temperature 25 DEG C, needs abundant stirring, stirring velocity 300rpm simultaneously;
(2) in gained ethanolic soln, add appropriate water again, generate the six trichloride hydrate aluminium being insoluble to ethanol;
(3) six trichloride hydrate aluminium and ammoniacal liquor reactivity generate hydrated aluminum oxide suspension: by suspended substance aging 2.5h within the scope of pH=8.0, make it to become α-diaspore, then washing is extremely without chlorion.
(4) the sour peptization of α-diaspore is become the good colloidal sol of flowing property, with in dripping method instillation oil ammonia column, balling-up is shunk by surface tension effects in oil, enter again in ammoniacal liquor, harder gelatinous ball thing is formed after neutralizing and be aging, diameter, at 1.5mm, carries out drying after washing oily ammonia, drying temperature 80 DEG C;
(5) aluminium hydroxide is put into the roasting at 600 DEG C of crucible feeding High Temperature Furnaces Heating Apparatus and obtain activated alumina.
(6) the product XRD analysis obtained after roasting is δ phase, and recording specific surface area through surface analyzer is 156.23 ㎡/g.
Embodiment 2
(1) the excessive aqueous ethanolic solution of 19.2g solid sodium terachloroaluminate is dissolved hydrolysis, the insoluble sodium-chlor of filtered and recycled.This process reaction temperature 35 DEG C, needs abundant stirring, stirring velocity 400rpm simultaneously;
(2) in gained ethanolic soln, add appropriate water again, generate the six trichloride hydrate aluminium being insoluble to ethanol;
(3) six trichloride hydrate aluminium and ammoniacal liquor reactivity generate hydrated aluminum oxide suspension: by suspended substance aging 3h within the scope of pH=8.5, make it to become α-diaspore, then washing is extremely without chlorion.
(4) the sour peptization of α-diaspore is become the good colloidal sol of flowing property, with in dripping method instillation oil ammonia column, balling-up is shunk by surface tension effects in oil, enter again in ammoniacal liquor, harder gelatinous ball thing is formed after neutralizing and be aging, diameter, at 2mm, carries out drying after washing oily ammonia, drying temperature 80 DEG C;
(5) aluminium hydroxide is put into the roasting at 700 DEG C of crucible feeding High Temperature Furnaces Heating Apparatus and obtain activated alumina.
(6) the product XRD analysis obtained after roasting is δ phase, and recording specific surface area through surface analyzer is 167.17 ㎡/g.
Embodiment 3
(1) the excessive aqueous ethanolic solution of 19.2g solid sodium terachloroaluminate is dissolved hydrolysis, the insoluble sodium-chlor of filtered and recycled.This process reaction temperature 45 C, needs abundant stirring, stirring velocity 500rpm simultaneously;
(2) in gained ethanolic soln, add appropriate water again, generate the six trichloride hydrate aluminium being insoluble to ethanol;
(3) six trichloride hydrate aluminium and ammoniacal liquor reactivity generate hydrated aluminum oxide suspension: by suspended substance aging 5h within the scope of pH=9.0, make it to become α-diaspore, then washing is extremely without chlorion.
(4) the sour peptization of α-diaspore is become the good colloidal sol of flowing property, with in dripping method instillation oil ammonia column, balling-up is shunk by surface tension effects in oil, enter again in ammoniacal liquor, harder gelatinous ball thing is formed after neutralizing and be aging, diameter, at 3mm, carries out drying after washing oily ammonia, drying temperature 80 DEG C;
(5) aluminium hydroxide is put into the roasting at 900 DEG C of crucible feeding High Temperature Furnaces Heating Apparatus and obtain activated alumina.
(6) the product XRD analysis obtained after roasting is δ phase, and recording specific surface area through surface analyzer is 159.63 ㎡/g.
Claims (5)
1. the preparation method of activated alumina porous adsorbing material, comprises following steps:
1) the excessive aqueous ethanolic solution of solid sodium terachloroaluminate is dissolved hydrolysis, the insoluble sodium-chlor of filtered and recycled;
2) again toward step 1) add appropriate water in the solution of gained, generate the six trichloride hydrate aluminium being insoluble to ethanol;
3) step 2) gained six trichloride hydrate aluminium adds ammoniacal liquor water generation reaction and closes aluminum oxide suspension, then carry out aging, make it to become α-diaspore, and washing is to without chlorion;
4) the sour peptization of α-diaspore is become the good colloidal sol of flowing property, in dripping method instillation oil ammonia column, in oil, shrink balling-up by surface tension effects, then enter in ammoniacal liquor, after neutralizing and be aging, form harder gelatinous ball thing, after washing oily ammonia, carry out drying;
5) gained Aluminium hydroxide roasting is obtained activated alumina porous adsorbing material.
2. the preparation method of activated alumina porous adsorbing material according to claim 1, is characterized in that: step 1) temperature of reaction control at 20-60 DEG C, stirring velocity 300-500rpm.
3. the preparation method of activated alumina porous adsorbing material according to claim 1, is characterized in that: step 3) described aging reaction pH controls at 8-9, digestion time 2-24h.
4. the preparation method of activated alumina porous adsorbing material according to claim 1, is characterized in that: step 4) diameter control of described gelatinous ball thing is at 1-3mm, and drying temperature is 60-100 DEG C.
5. the preparation method of activated alumina porous adsorbing material according to claim 1, is characterized in that: step 5) maturing temperature control at 500-1000 DEG C.
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| CN201410657181.5A CN104445323B (en) | 2014-11-18 | 2014-11-18 | The preparation method of activated alumina porous adsorbing material |
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| CN201410657181.5A CN104445323B (en) | 2014-11-18 | 2014-11-18 | The preparation method of activated alumina porous adsorbing material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106391035A (en) * | 2016-11-02 | 2017-02-15 | 蚌埠学院 | Heterogeneous Fenton catalyst, preparation method thereof and application of heterogeneous Fenton catalyst to degradation of phenolic wastewater |
| CN109434099A (en) * | 2018-12-18 | 2019-03-08 | 宁波申禾轴承有限公司 | A kind of preparation method of high intensity deep groove ball bearing |
| CN109570509A (en) * | 2018-12-18 | 2019-04-05 | 宁波申禾轴承有限公司 | A kind of preparation method of high intensity bearing |
| CN111921153A (en) * | 2020-04-15 | 2020-11-13 | 浙江安力能源有限公司 | Method for treating sodium tetrachloroaluminate |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101993102B (en) * | 2009-08-20 | 2012-09-26 | 中国科学院过程工程研究所 | Method for inorganically synthesizing organized mesoporous alumina |
-
2014
- 2014-11-18 CN CN201410657181.5A patent/CN104445323B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106391035A (en) * | 2016-11-02 | 2017-02-15 | 蚌埠学院 | Heterogeneous Fenton catalyst, preparation method thereof and application of heterogeneous Fenton catalyst to degradation of phenolic wastewater |
| CN106391035B (en) * | 2016-11-02 | 2018-08-10 | 蚌埠学院 | A kind of heterogeneous type Fenton catalyst and preparation method thereof and the application in phenol wastewater of degrading |
| CN109434099A (en) * | 2018-12-18 | 2019-03-08 | 宁波申禾轴承有限公司 | A kind of preparation method of high intensity deep groove ball bearing |
| CN109570509A (en) * | 2018-12-18 | 2019-04-05 | 宁波申禾轴承有限公司 | A kind of preparation method of high intensity bearing |
| CN111921153A (en) * | 2020-04-15 | 2020-11-13 | 浙江安力能源有限公司 | Method for treating sodium tetrachloroaluminate |
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