CN104353400A - Preparation method of high-purity high-solid content transparent aluminum sol - Google Patents
Preparation method of high-purity high-solid content transparent aluminum sol Download PDFInfo
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- CN104353400A CN104353400A CN201410631600.8A CN201410631600A CN104353400A CN 104353400 A CN104353400 A CN 104353400A CN 201410631600 A CN201410631600 A CN 201410631600A CN 104353400 A CN104353400 A CN 104353400A
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- purity
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- inorganic acid
- raw material
- aluminum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0004—Preparation of sols
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0004—Preparation of sols
- B01J13/0047—Preparation of sols containing a metal oxide
Abstract
The invention relates to a preparation method of a high-purity high-solid content transparent aluminum sol. The preparation method comprises the following steps: taking high-purity pseudo-boehmite or high-purity aluminum isopropoxide or a mixture of the high-purity pseudo-boehmite and the high-purity aluminum isopropoxide as a raw material, adding Al<3+> and H<+> at the mole ratio of 10:1-20:1 to high-purity water to prepare inorganic acid with certain concentration; regulating a pH value between 1 and 3 and stirring for 20-30 minutes at the temperature between 35 DEG C and 50 DEG C to obtain the high-purity uniform and transparent aluminum sol. The high-purity high-solid content transparent aluminum sol disclosed by the invention has the solid content more than 30% and the purity more than 99.99%, and the transparency and flowability can be stably kept for a long time without precipitates.
Description
Technical field
The present invention relates to a kind of preparation method of Alumina gel, particularly the preparation method of a kind of high-purity, Alumina gel that high solids content is transparent, belongs to technical field of material chemistry.
Background technology
In general, people are referred to as high-purity material the material of purity more than 99.9%; Transparently be divided into optical clear and visually-clear, optical clear aspect is mainly referred to as optical clear to the transmitance of certain specific light more than 15%, and be referred to as optical translucent lower than 15%, visually-clear is then in visible range, formed homogeneous, stable, can through visible ray.Aluminium oxide is widely used in the carrier of petroleum catalyst, as reforming catalyst and hydrogenation catalyst, and γ-Al
2o
3belong to cubic system, it is loosely organized, and specific area is large, is often by the catalyst carrier used.γ-the Al prepared with Alumina gel
2o
3particle has the features such as size uniformity, activity is high, specific area is large, therefore adopts Alumina gel method catalyst carrier γ-Al
2o
3main method; Meanwhile, Alumina gel is uniformly dispersed, good fluidity, can prepare large volume catalyst carrier block, the alumina coating on surface of such as honeycomb ceramic carrier by means such as surface coatings.
Catalyst adopts precious metal or heavy metal often, and price comparison costliness is simultaneously also with toxicity.Therefore should not be subject to the impact of other impurity elements in catalytic process, catalytic efficiency and catalysis precision can be improved.High-purity high-activity catalyst carrier becomes the focus of research now, and has market prospects widely at home and abroad.
Application publication number CN 102432300 A(application number 201110278730.4) Chinese patent literature disclose a kind of preparation method of Alumina gel of size tunable, take inorganic aluminate as raw material, by regulation and control reaction temperature, reactant solubility, reaction generates the Alumina gel of pH when precipitating and obtained different-grain diameter distribution.Application publication number CN 103357358 A(application number 201210105345.4) Chinese patent literature disclose a kind of preparation method of the Alumina gel for chemical binder.Publication number CN 1962062A(application number 200670129591.8) Chinese patent literature disclose a kind of preparation method and application thereof of Alumina gel; Preparation process is as follows: (with boehmite powder for primary raw material, according to aluminium: the molar ratio of water is 1:20-50, joins gradually in deionized water, limit is reinforced stirs, until all disperse l; 2) be take inorganic acid according to the aluminum ions molar ratio of hydrogen ion two, as nitric acid, hydrochloric acid, while stirring acid supplemented solution, at normal temperatures acidolysis, form translucent colloidal sol; (3) stir 2-5 hour continuously at normal temperatures, form stable Alumina gel.Application publication number CN 101928029 A(application number 201010274945.4) Chinese patent literature disclose a kind of preparation method of alumina sol, the method take boehmite as raw material, comprise the following steps of carrying out successively: by boehmite dispersion in deionized water, wherein, boehmite and the coin amount of water are than being 1:2-20; (2) add acid for adjusting pH to 2-5, adopt colloid mill strong stirring to obtain suspension in 0.5-2 hour; (3) oven ageing described suspension being put into 80-90 DEG C obtains aging slurry, time aging-and be 24-72 hour; (4) described aging slurry is taken out, except the precipitation of sub-cloud, obtain described alumina sol.Publication number CN 103288111(application number 201310262472.X) Chinese patent literature disclose the steady alumina sol preparation method of a kind of speed.
Comprise in the prior art processes preparation process of above-mentioned patent document that aging temperature is high, the time is long; Prepared Alumina gel purity and solid content lower.
Summary of the invention
In order to overcome the deficiency of above-mentioned technology, provide a kind of simple to operate, the cycle is short, and purity and the high technical matters of solid content, the invention provides the preparation method of the transparent Alumina gel of a kind of high-purity high solids content.
The technical solution used in the present invention is: the preparation method of the transparent Alumina gel of a kind of high-purity, high solids content, and step is as follows:
(1) aluminum-containing raw material A is taken;
(2) inorganic acid B is taken as peptizing agent;
(3) take high purity water, be made into inorganic acid solution C with inorganic acid B;
(4) dispergation: heated by inorganic acid solution C, stir, slowly add aluminum-containing raw material A while stirring, obtains high-purity, the transparent Alumina gel of high solids content.
Foregoing preparation method, preferred scheme is: when step (2) takes inorganic acid B, according to Al
3+and H
+mol ratio is that 8:1 ~ 22:1 takes inorganic acid B(preferably, according to Al
3+and H
+mol ratio is that 10:1 ~ 20:1 takes inorganic acid B; Be more preferably, according to Al
3+and H
+mol ratio is that 15:1 takes inorganic acid B).
Foregoing preparation method, preferred scheme is: when step (3) takes high purity water, takes high purity water (preferably, take high purity water according to 3 ~ 5 times of aluminum-containing raw material A quality according to 4 ~ 6 times of aluminum-containing raw material A quality; 4(3 according to aluminum-containing raw material A quality) doubly take high purity water).
Foregoing preparation method, preferred scheme is: step (3) gained inorganic acid solution C control ph is 1 ~ 3.
Foregoing preparation method, preferred scheme is: the described inorganic acid B of step (3) is one or several the mixture in 98% concentrated sulfuric acid, 97.5% acetic acid, 65% ~ 68% red fuming nitric acid (RFNA) and 35% hydrochloric acid, is mass concentration.
Foregoing preparation method, preferred scheme is: the described aluminum-containing raw material A of step (1) is that high-purity boehmite or high puring aluminium isopropoxide or both mixtures are (preferred, described high-purity boehmite or high puring aluminium isopropoxide are all adopt alkoxide hydrolysis to obtain, and its purity is more than 99.999%).
Foregoing preparation method, preferred scheme is: step (3) described high purity water is distilled water or ion exchange water, and its resistivity reaches more than 12M Ω.
Foregoing preparation method, preferred scheme is: the described dispergation process of step (4), and inorganic acid solution C is with heating water bath (preferred, be heated to 35 ~ 50 DEG C).
Foregoing preparation method, preferred scheme is: the described dispergation process of step (4), mixing time 20 ~ 30min.
Foregoing preparation method, preferred scheme is: the solids content of the transparent Alumina gel of gained high-purity, high solids content reaches more than 20% (preferred, solids content reaches more than 30%), and purity reaches more than 99.99%.
The main implementation method of the present invention is: with high-purity boehmite or high puring aluminium isopropoxide or both mixtures for raw material, by Al
3+and H
+be 10:1 ~ 20:1 in molar ratio, add high purity water and configure certain density inorganic acid, regulate pH value between 1 ~ 3, temperature controls to carry out stirring 20 ~ 30min between 35 ~ 50 DEG C, can obtain the Alumina gel of high-purity homogeneous transparent, the solids content of this Alumina gel can reach more than 30%, and purity can reach more than 99.99%, and steady in a long-termly can keep transparent and mobility, without precipitate.
Comprise the following steps:
(1) the aluminum-containing raw material A such as boehmite or aluminium isopropoxide of certain mass is taken;
In described step (1), the hydrolysis equation of aluminium isopropoxide is:
Al(OPr
iso)+4H
2O→AlOOH+6Pr
isoOH
(2) according to Al
3+and H
+be 10:1 ~ 20:1 in molar ratio, take the inorganic acid B of certain mass as peptizing agent.
(3) according to aluminum-containing raw material A quality 3 ~ 5 times, take high purity water, be made into inorganic acid solution C with inorganic acid B, and regulate pH value 1 ~ 3.
Described inorganic acid B be 98% concentrated sulfuric acid, 97.5% acetic acid, 65% ~ Lane 68% nitric acid and 35% hydrochloric acid in one or several mixture.
(4) by inorganic acid solution C Heating Water to 35 ~ 50 DEG C, stir, simultaneously slowly add aluminum-containing raw material A while stirring, stir 20 ~ 30min.
The solids content of gained Alumina gel of the present invention can reach more than 30%, and purity can reach more than 99.99%, and steady in a long-termly can keep transparent and mobility, without precipitate.High-purity boehmite or high puring aluminium isopropoxide or both mixtures are all adopt alkoxide hydrolysis to obtain, and its purity is more than 99.999%.Described high solids content generally to refer in vitreosol boehmite or is converted into the content of boehmite more than 30% by aluminium isopropoxide.
The present invention and invention difference are in the past:
(1) the Alumina gel purity prepared of the present invention is high, and the general purity of aluminum-containing raw material that adopts is 99.999%, and colloidal sol purity >=99.99% of preparation.
(2) the Alumina gel solid content prepared by the present invention is high, and general solid content >=20%, reaches as high as more than 30%.
(3) Alumina gel prepared by the present invention can reach visually-clear, and increases along with the growth transparency of resting period.
(4) Alumina gel prepared of the present invention can long storage time, and has higher mobility, and long storage time simultaneously, without precipitate.
(5) preparation method of high-purity provided by the present invention, the transparent Alumina gel of high solids content, simple to operate, with low cost, easily realize suitability for industrialized production, aging temperature is low, manufacturing cycle is short, can stablize and effectively prepare high-purity, the transparent Alumina gel of high solids content.
Detailed description of the invention
Describe in detail to the present invention in conjunction with specific embodiments now, protection domain is not by this restriction.
Embodiment 1: the preparation method of the transparent Alumina gel of a kind of high-purity, high solids content
(1) boehmite powder 120g is taken;
(2) take content be 65% ~ 68% red fuming nitric acid (RFNA) 6.3g be placed in beaker, add 400g high purity water simultaneously and red fuming nitric acid (RFNA) diluted, and stir, regulate pH value 1, configuration dilute nitric acid solution A;
(3) salpeter solution A is placed in heating water bath, regulates temperature to be 40 DEG C, slowly add boehmite powder while stirring, after stirring 30min, can obtain purity is 99.99%, and solid content is the transparent Alumina gel of 30%.
Embodiment 2: the preparation method of the transparent Alumina gel of a kind of high-purity, high solids content
(1) high puring aluminium isopropoxide 204g is taken;
(2) take content be 65% ~ 68% red fuming nitric acid (RFNA) 6.3g be placed in beaker, add 300g high purity water simultaneously and red fuming nitric acid (RFNA) diluted, and stir, regulate pH value to be 3, configuration dilute nitric acid solution A;
(3) high puring aluminium isopropoxide is placed in heating water bath, regulates temperature to be 50 DEG C, slowly add dilute nitric acid solution A while stirring, after stirring 20min, can obtain purity is 99.99%, and solid content is the transparent Alumina gel of 26%.
Embodiment 3: the preparation method of the transparent Alumina gel of a kind of high-purity, high solids content
(1) boehmite powder 120g is taken;
(2) take content be 35% red fuming nitric acid (RFNA) 7.3g be placed in beaker, add 360g high purity water simultaneously and red fuming nitric acid (RFNA) diluted, and stir, regulate pH value 3, configuration dilute hydrochloric acid solution B;
(3) molten for nitric acid B is placed in heating water bath, regulates temperature to be 30 DEG C, slowly add boehmite powder while stirring, after stirring 30min, can obtain purity is 99.99%, and solid content is the transparent Alumina gel of 33%.
Embodiment 4: the preparation method of the transparent Alumina gel of a kind of high-purity, high solids content
(1) high puring aluminium isopropoxide of certain mass is taken; Described high puring aluminium isopropoxide adopts alkoxide hydrolysis to obtain, and its purity is more than 99.999%.Hydrolysis equation is: Al (OPr
iso)+4H
2o → AlOOH+6Pr
isooH
(2) according to Al
3+and H
+be 15:1 in molar ratio, take the hydrochloric acid of the mass concentration 35% of certain mass as peptizing agent.
(3) according to aluminium isopropoxide quality 4 times, take ion exchange water (its resistivity reaches more than 12M Ω), be made into inorganic acid solution C with hydrochloric acid, and adjust ph be 1 ~ 3.
(4) by inorganic acid solution C heating water bath to 35 ~ 50 DEG C, stir, simultaneously slowly add aluminum-containing raw material A while stirring, stir 20 ~ 30min.
The solids content of the transparent Alumina gel of gained high-purity, high solids content reaches 35%, and purity reaches 99.99%.
It should be pointed out that detailed description of the invention is the more representational example of the present invention, obvious technical scheme of the present invention is not limited to above-described embodiment.A lot of distortion can also be had.Those of ordinary skill in the art, mentions or associates disclosed in from then in file, all should think the claimed scope of this patent.
Claims (10)
1. a preparation method for high-purity, the transparent Alumina gel of high solids content, is characterized in that:
(1) aluminum-containing raw material A is taken;
(2) inorganic acid B is taken as peptizing agent;
(3) take high purity water, be made into inorganic acid solution C with inorganic acid B;
(4) dispergation: heated by inorganic acid solution C, stir, slowly add aluminum-containing raw material A while stirring, obtains high-purity, the transparent Alumina gel of high solids content.
2. preparation method according to claim 1, is characterized in that: when step (2) takes inorganic acid B, according to Al
3+and H
+mol ratio is that 8:1 ~ 22:1 takes inorganic acid B(preferably, according to Al
3+and H
+mol ratio is that 10:1 ~ 20:1 takes inorganic acid B; Be more preferably, according to Al
3+and H
+mol ratio is that 15:1 takes inorganic acid B).
3. preparation method according to claim 1, is characterized in that: when step (3) takes high purity water, takes high purity water (preferably, take high purity water according to 3 ~ 5 times of aluminum-containing raw material A quality according to 4 ~ 6 times of aluminum-containing raw material A quality; High purity water is taken) according to 4 times of aluminum-containing raw material A quality.
4. preparation method according to claim 1, is characterized in that: step (3) gained inorganic acid solution C control ph is 1 ~ 3.
5. preparation method according to claim 1, is characterized in that: the described inorganic acid B of step (3) is one or several the mixture in 98% concentrated sulfuric acid, 97.5% acetic acid, 65% ~ 68% red fuming nitric acid (RFNA) and 35% hydrochloric acid, is mass concentration.
6. preparation method according to claim 1, it is characterized in that: the described aluminum-containing raw material A of step (1) is that high-purity boehmite or high puring aluminium isopropoxide or both mixtures are (preferred, described high-purity boehmite or high puring aluminium isopropoxide are all adopt alkoxide hydrolysis to obtain, and its purity is more than 99.999%).
7. preparation method according to claim 1, is characterized in that: step (3) described high purity water is distilled water or ion exchange water, and its resistivity reaches more than 12M Ω.
8. preparation method according to claim 1, is characterized in that: the described dispergation process of step (4), and inorganic acid solution C is with heating water bath (preferred, be heated to 35 ~ 50 DEG C).
9. preparation method according to claim 1, is characterized in that: the described dispergation process of step (4), mixing time 20 ~ 30min.
10. preparation method according to claim 1, is characterized in that: the solids content of the transparent Alumina gel of gained high-purity, high solids content reaches more than 20% (preferred, solids content reaches more than 30%), and purity reaches more than 99.99%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107597029A (en) * | 2017-10-30 | 2018-01-19 | 苏州瑞晶纳米材料制备与应用研究有限公司 | A kind of preparation method of high-purity Alumina gel |
| CN107720791A (en) * | 2017-10-20 | 2018-02-23 | 大连理工大学 | A kind of method for preparing high purity pseudoboehmite adhesive |
| CN110950365A (en) * | 2019-12-20 | 2020-04-03 | 大连理工大学 | Low-acid-content high-purity alumina sol and preparation method thereof |
| CN113546613A (en) * | 2021-06-24 | 2021-10-26 | 北京佳安氢源科技股份有限公司 | Preparation method and application of aluminum sol |
| CN115172059A (en) * | 2022-08-09 | 2022-10-11 | 西安稀有金属材料研究院有限公司 | Method for preparing aluminum electrolytic capacitor anode foil by combining aerosol spraying method |
| CN115611523A (en) * | 2022-10-24 | 2023-01-17 | 深圳市日升质电子科技有限公司 | Manufacturing process of electric insulation heat conduction glass |
| CN116081668A (en) * | 2023-03-06 | 2023-05-09 | 成都超纯应用材料有限责任公司 | Boehmite sol dispersing agent, preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962062A (en) * | 2006-11-24 | 2007-05-16 | 天津市环科机动车尾气催化净化技术有限公司 | Preparation method of aluminium sol and application thereof |
| CN103204526A (en) * | 2012-01-15 | 2013-07-17 | 湖南晟通科技集团有限公司 | A method for preparing an alumina sol |
-
2014
- 2014-11-12 CN CN201410631600.8A patent/CN104353400A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962062A (en) * | 2006-11-24 | 2007-05-16 | 天津市环科机动车尾气催化净化技术有限公司 | Preparation method of aluminium sol and application thereof |
| CN103204526A (en) * | 2012-01-15 | 2013-07-17 | 湖南晟通科技集团有限公司 | A method for preparing an alumina sol |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107720791A (en) * | 2017-10-20 | 2018-02-23 | 大连理工大学 | A kind of method for preparing high purity pseudoboehmite adhesive |
| CN107597029A (en) * | 2017-10-30 | 2018-01-19 | 苏州瑞晶纳米材料制备与应用研究有限公司 | A kind of preparation method of high-purity Alumina gel |
| CN110950365A (en) * | 2019-12-20 | 2020-04-03 | 大连理工大学 | Low-acid-content high-purity alumina sol and preparation method thereof |
| CN113546613A (en) * | 2021-06-24 | 2021-10-26 | 北京佳安氢源科技股份有限公司 | Preparation method and application of aluminum sol |
| CN115172059A (en) * | 2022-08-09 | 2022-10-11 | 西安稀有金属材料研究院有限公司 | Method for preparing aluminum electrolytic capacitor anode foil by combining aerosol spraying method |
| CN115611523A (en) * | 2022-10-24 | 2023-01-17 | 深圳市日升质电子科技有限公司 | Manufacturing process of electric insulation heat conduction glass |
| CN116081668A (en) * | 2023-03-06 | 2023-05-09 | 成都超纯应用材料有限责任公司 | Boehmite sol dispersing agent, preparation method and application thereof |
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Application publication date: 20150218 |