CN110127736A - A kind of preparation method of high glutinous macropore boehmite - Google Patents
A kind of preparation method of high glutinous macropore boehmite Download PDFInfo
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- CN110127736A CN110127736A CN201910454521.7A CN201910454521A CN110127736A CN 110127736 A CN110127736 A CN 110127736A CN 201910454521 A CN201910454521 A CN 201910454521A CN 110127736 A CN110127736 A CN 110127736A
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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
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
- C01F7/141—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
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Abstract
The present invention relates to a kind of preparation methods of high glutinous macropore boehmite, described method includes following steps: aluminum salt solution and meta-aluminate solution being mixed, under the conditions of 15-45 DEG C of temperature, carry out neutralization reaction, it obtains and neutralizes material, the pH value for neutralizing material is 6.5-8.5；By the neutralization material under the conditions of 50-80 DEG C of temperature, crystallization is carried out, obtains crystallization material, filters the crystallization material, obtains crystallized cake and crystallization filtrate, washs the crystallized cake, obtains wet cake；Into the wet cake plus water mashing obtains slurry, it is added into the slurry auxiliary agent, under the conditions of 80-95 DEG C of temperature, carry out aging reaction 30-180min, aging material is obtained, the aging material is filtered, obtains aging filter cake and aging filtrate, the aging filter cake is dried, high glutinous macropore boehmite is obtained.
Description
Technical field
The invention belongs to the synthesis technical fields of compound, and in particular to a kind of preparation side of high glutinous macropore boehmite
Method.
Background technique
Boehmite also known as monohydrate alumina, false boehmite, crystal phase purity is high, peptization performance are good, caking property
By force, have the characteristics that specific surface height, Kong Rong great, can be used as preparing petroleum refinement catalyst, reforming catalyst and production tail gas vapor
The adsorbent of tail gas cleaning catalyst, binder or carrier, but existing boehmite viscosity is insufficient, and hole holds not enough
Greatly, therefore, this field needs to develop the boehmite of a kind of high viscosity, macropore.
Summary of the invention
In view of the above problems, it proposes on the present invention overcomes the above problem or at least be partially solved in order to provide one kind
The height for stating problem sticks the preparation method of macropore boehmite.
The embodiment of the present invention provides a kind of preparation method of high glutinous macropore boehmite, and the method includes walking as follows
It is rapid:
Aluminum salt solution and meta-aluminate solution are mixed, under the conditions of 15-45 DEG C of temperature, carry out neutralization reaction, in acquisition
And material, the pH value for neutralizing material are 6.5-8.5；
By the neutralization material under the conditions of 50-80 DEG C of temperature, crystallization is carried out, crystallization material is obtained, described in filtering
Crystallization material obtains crystallized cake and crystallization filtrate, washs the crystallized cake, obtains wet cake；
Into the wet cake plus water mashing obtains slurry, auxiliary agent is added into the slurry, in 80-95 DEG C of temperature condition
Under, aging reaction 30-180min is carried out, aging material is obtained, filters the aging material, obtains aging filter cake and aging filter
Liquid dries the aging filter cake, obtains high glutinous macropore boehmite.
Further, the aluminum salt solution is aluminum sulfate solution, by mass percentage, in the aluminum sulfate solution, oxygen
Change aluminium content is 6-10%, sulfate radical content 20-28%.
Further, by mass percentage, in the aluminum sulfate solution, alumina content 8%, sulfate radical content is
24%.
Further, the meta-aluminate solution is sodium aluminate solution, in the sodium aluminate solution, alumina concentration
For 20-100g/L, by mass percentage.
Further, in the sodium aluminate solution, alumina concentration 50g/L.
Further, the neutralization reaction temperature is 30 DEG C, and the pH value for neutralizing material is 7.0.
Further, the crystallization temperature is 70 DEG C.
Further, temperature is used to carry out the washing for 80-95 DEG C of distilled water.
Further, the auxiliary agent is the inorganic and/or organic bases auxiliary agent without sodium ion and chloride ion, including
(NH4)2CO3、NH4HCO3, at least one of urea and isopropanol.
Further, the aging reaction temperature is 90 DEG C, and the aging reaction time is 60min, the drying temperature
It is 80-100 DEG C.
One or more technical solutions in the embodiment of the present invention, have at least the following technical effects or advantages:
The preparation method of high glutinous macropore boehmite provided by the invention, first by aluminum salt solution and meta-aluminate solution
Mixing carries out neutralization reaction, and by controlling reaction temperature, reaction speed and reaction slurry pH value, it is heavy to generate macropore boehmite
It forms sediment, this process is typical double decomposition neutralization reaction, produces white precipitate and water, white precipitate are macropore boehmites；
Then washing is filtered to precipitating until this process is mainly washed off to next stage hydrothermal aging after impurity qualified
The unfavorable sodium ion of process carries out slurrying processing to filter cake, auxiliary agent is added in the process, carries out polycondensation reaction, reaction master
Macropore boehmite is acted on by the auxiliary agent being added, two hydrones that dissociate generate double-core Double-bridge type complex, connect
This complex can lose two H+ and form the Double-bridge type complex of stable oxygen-oxygen bond, in two oxygroup Double-bridge type complexs
Hydrone be detached from become 0H group, H20 molecule formed Double-bridge type complex, and then formed four oxygroup bridge-type polynuclear complexs,
It is as follows:
0-0 base is alternately present, and forms netted or lock shape polynuclear complex, as follows:
Can be slowly stable by this polynuclear complex of high temperature ageing, there is extremely strong caking property, be finally filtered, washed,
Drying crushes and prepares high glutinous macropore boehmite.
Detailed description of the invention
By reading the following detailed description of the preferred embodiment, various other advantages and benefits are common for this field
Technical staff will become clear.The drawings are only for the purpose of illustrating a preferred embodiment, and is not considered as to the present invention
Limitation.And throughout the drawings, identical component is indicated with identical reference pattern.In the accompanying drawings:
Fig. 1 shows the flow chart of the high glutinous macropore boehmite of preparation of the embodiment of the present invention；
Specific embodiment
Below in conjunction with specific embodiment and embodiment, it is specifically described the present invention, advantages of the present invention and various effects
It thus will clearly present.It will be understood by those skilled in the art that these specific embodiments and embodiment are for illustrating
The present invention is not intended to limit the present invention.
Throughout the specification, unless otherwise specified, terms used herein are interpreted as usual in this field
Used meaning.Therefore, unless otherwise defined, all technical and scientific terms used herein has leads with belonging to the present invention
The identical meaning of the general understanding of field technique personnel.Contradiction if it exists, this specification are preferential.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention, can pass through
Market is commercially available or can be prepared by existing method.
The application provides a kind of preparation method of high glutinous macropore boehmite, and described method includes following steps:
Aluminum salt solution and meta-aluminate solution are mixed, under the conditions of 15-45 DEG C of temperature, carry out neutralization reaction, in acquisition
And material, the pH value for neutralizing material are 6.5-8.5；
By the neutralization material under the conditions of 50-80 DEG C of temperature, crystallization is carried out, crystallization material is obtained, described in filtering
Crystallization material obtains crystallized cake and crystallization filtrate, washs the crystallized cake, obtains wet cake；
Into the wet cake plus water mashing obtains slurry, auxiliary agent is added into the slurry, in 80-95 DEG C of temperature condition
Under, aging reaction 30-180min is carried out, aging material is obtained, filters the aging material, obtains aging filter cake and aging filter
Liquid dries the aging filter cake, obtains high glutinous macropore boehmite.
In the application, the aluminum salt solution is aluminum sulfate solution, by mass percentage, in the aluminum sulfate solution, oxygen
Change aluminium content is 6-10%, sulfate radical content 20-28%.
Preferably, by mass percentage, in the aluminum sulfate solution, alumina content 8%, sulfate radical content is
24%.
In the application, the meta-aluminate solution is sodium aluminate solution, in the sodium aluminate solution, alumina concentration
For 20-100g/L, by mass percentage.
Preferably, in the sodium aluminate solution, alumina concentration 50g/L.
In the application, the neutralization reaction temperature is 30 DEG C, and the pH value for neutralizing material is 7.0.
Preferably, the crystallization temperature is 70 DEG C.
In the application, temperature is used to carry out the washing for 80-95 DEG C of distilled water.
In the application, the auxiliary agent is the inorganic and/or organic bases auxiliary agent without sodium ion and chloride ion, including
(NH4)2CO3、NH4HCO3, at least one of urea and isopropanol.
Preferably, the aging reaction temperature is 90 DEG C, and the aging reaction time is 60min, and the drying temperature is
80-100℃。
It is carried out below in conjunction with the preparation method that height of 3 specific embodiments to the application sticks macropore boehmite detailed
Explanation.
Embodiment 1
A kind of preparation method of high glutinous macropore boehmite, described method includes following steps:
Aluminum sulfate solution and sodium aluminate solution are mixed, under the conditions of 15 DEG C of temperature, neutralization reaction is carried out, is neutralized
Material, the pH value for neutralizing material are 6.5；By mass percentage, in the aluminum sulfate solution, alumina content 6%,
Sulfate radical content is 20%；In the sodium aluminate solution, alumina concentration 20g/L；
By the neutralization material under the conditions of 50 DEG C of temperature, crystallization is carried out, crystallization material is obtained, filters the crystallization
Material obtains crystallized cake and crystallization filtrate, uses temperature for crystallized cake described in 80 DEG C of distillation water washing, obtain wet filter
Cake；
Into the wet cake plus water mashing obtains slurry, is added into the slurry auxiliary agent, under the conditions of 80 DEG C of temperature,
Aging reaction 30min is carried out, aging material is obtained, filters the aging material, obtains aging filter cake and aging filtrate, 80 DEG C of temperature
The degree lower drying aging filter cake, obtains high glutinous macropore boehmite.
Embodiment 2
A kind of preparation method of high glutinous macropore boehmite, described method includes following steps:
Aluminum sulfate solution and sodium aluminate solution are mixed, under the conditions of 45 DEG C of temperature, neutralization reaction is carried out, is neutralized
Material, the pH value for neutralizing material are 8.5；By mass percentage, in the aluminum sulfate solution, alumina content is
10%, sulfate radical content 28%；In the sodium aluminate solution, alumina concentration 100g/L；
By the neutralization material under the conditions of 80 DEG C of temperature, crystallization is carried out, crystallization material is obtained, filters the crystallization
Material obtains crystallized cake and crystallization filtrate, uses temperature for crystallized cake described in 95 DEG C of distillation water washing, obtain wet filter
Cake；
Into the wet cake plus water mashing obtains slurry, auxiliary agent is added into the slurry, in 95 DEG C of temperature conditions
Under, aging reaction 180min is carried out, aging material is obtained, filters the aging material, obtains aging filter cake and aging filtrate, 90
The aging filter cake is dried at a temperature of DEG C, obtains high glutinous macropore boehmite.
Embodiment 3
A kind of preparation method of high glutinous macropore boehmite, described method includes following steps:
Aluminum sulfate solution and sodium aluminate solution are mixed, under the conditions of 30 DEG C of temperature, neutralization reaction is carried out, is neutralized
Material, the pH value for neutralizing material are 7；By mass percentage, in the aluminum sulfate solution, alumina content 8%, sulphur
Acid group content is 24%；In the sodium aluminate solution, alumina concentration 50g/L；
By the neutralization material under the conditions of 70 DEG C of temperature, crystallization is carried out, crystallization material is obtained, filters the crystallization
Material obtains crystallized cake and crystallization filtrate using crystallized cake described in distillation water washing at a temperature of 90 °C and obtains wet filter
Cake；
Into the wet cake plus water mashing obtains slurry, is added into the slurry auxiliary agent, under the conditions of 90 DEG C of temperature,
Aging reaction 60min is carried out, aging material is obtained, filters the aging material, obtains aging filter cake and aging filtrate, 100 DEG C
At a temperature of dry the aging filter cake, obtain high glutinous macropore boehmite.
Macropore boehmite is sticked to height made from embodiment 1-3 and carries out performance detection, testing result is as shown in table 1.
Table 1
| Peptization index/% | Kong Rong/mL.g-1 | Specific surface/m2.g-1 | |
| Embodiment 1 | 97.8 | 0.7335 | 362.5 |
| Embodiment 2 | 98.2 | 0.8101 | 342.1 |
| Embodiment 3 | 98.7 | 0.8335 | 331.1 |
Compared with prior art, the preparation method that the height of the application sticks macropore boehmite has the following characteristics that
The present invention is using the high glutinous macropore boehmite of precipitation method production, and by controlling different process conditions, production is high
Glutinous macropore boehmite, peptization index, Kong Rong, aperture, intensity and the specific surface area and SiO of the invention product2、Fe2O3With
Na2The properties such as the content of O, compensating for common macropore boehmite does not have the shortcomings that caking property, enhances with common big
Hole boehmite is the intensity of the catalyst of raw material, expands the use scope of macropore boehmite, is able to satisfy more extensively
Application field.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that include a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
Although preferred embodiments of the present invention have been described, it is created once a person skilled in the art knows basic
Property concept, then additional changes and modifications may be made to these embodiments.So it includes excellent that the following claims are intended to be interpreted as
It selects embodiment and falls into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (10)
1. a kind of preparation method of high glutinous macropore boehmite, which is characterized in that described method includes following steps:
Aluminum salt solution and meta-aluminate solution are mixed, under the conditions of 15-45 DEG C of temperature, neutralization reaction is carried out, obtains corrective
Material, the pH value for neutralizing material are 6.5-8.5；
By the neutralization material under the conditions of 50-80 DEG C of temperature, crystallization is carried out, crystallization material is obtained, filters the crystallization
Material obtains crystallized cake and crystallization filtrate, washs the crystallized cake, obtains warm filter cake；
Into the wet cake plus water mashing obtains slurry, is added into the slurry auxiliary agent, under the conditions of 80-95 DEG C of temperature,
Aging reaction 30-180min is carried out, aging material is obtained, filters the aging material, obtains aging filter cake and aging filtrate, is dried
The aging filter cake is done, high glutinous macropore boehmite is obtained.
2. a kind of preparation method of high glutinous macropore boehmite according to claim 1, which is characterized in that the aluminium salt
Solution is aluminum sulfate solution, and by mass percentage, in the aluminum sulfate solution, alumina content 6-10%, sulfate radical contains
Amount is 20-28%.
3. a kind of preparation method of high glutinous macropore boehmite according to claim 2, which is characterized in that press quality hundred
Divide than counting, in the aluminum sulfate solution, alumina content 8%, sulfate radical content 24%.
4. a kind of preparation method of high glutinous macropore boehmite according to claim 1, which is characterized in that the inclined aluminium
Acid salt solution is sodium aluminate solution, in the sodium aluminate solution, alumina concentration 20-100g/L, by mass percentage
Meter.
5. a kind of preparation method of high glutinous macropore boehmite according to claim 4, which is characterized in that the inclined aluminium
In acid sodium solution, alumina concentration 50g/L.
6. a kind of preparation method of high glutinous macropore boehmite according to claim 1, which is characterized in that the neutralization
Reaction temperature is 30 DEG C, and the pH value for neutralizing material is 7.0.
7. a kind of preparation method of high glutinous macropore boehmite according to claim 1, which is characterized in that the crystallization
Reaction temperature is 70 DEG C.
8. a kind of preparation method of high glutinous macropore boehmite according to claim 1, which is characterized in that use temperature
The washing is carried out for 80-95 DEG C of distilled water.
9. a kind of preparation method of high glutinous macropore boehmite according to claim 1, which is characterized in that the auxiliary agent
Including (NH4)2CO3、NH4HCO3, at least one of urea and isopropanol.
10. a kind of preparation method of high glutinous macropore boehmite according to claim 1, which is characterized in that described old
Changing reaction temperature is 90 DEG C, and the aging reaction time is 60min, and the drying temperature is 80-100 DEG C.
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Cited By (7)
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| CN110639484A (en) * | 2019-09-25 | 2020-01-03 | 山东金滢新材料有限公司 | Preparation method of pseudo-boehmite |
| CN113277536A (en) * | 2021-05-24 | 2021-08-20 | 中铝山东有限公司 | Washing process for reducing water consumption for pseudo-boehmite washing |
| CN113562753A (en) * | 2021-05-12 | 2021-10-29 | 中铝山东新材料有限公司 | Macroporous pseudo-boehmite and preparation method thereof |
| CN114853039A (en) * | 2022-05-24 | 2022-08-05 | 北京化工大学 | Pseudo-boehmite with high specific surface area and high pore volume and preparation method thereof |
| CN115124056A (en) * | 2022-06-29 | 2022-09-30 | 中国铝业股份有限公司 | Pseudo-boehmite, preparation method and application thereof |
| CN115818688A (en) * | 2022-10-24 | 2023-03-21 | 中铝郑州有色金属研究院有限公司 | Nano boehmite and preparation method thereof |
| CN115974115A (en) * | 2022-12-14 | 2023-04-18 | 南昌宝弘新材料技术有限公司 | Pseudo-boehmite and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110639484A (en) * | 2019-09-25 | 2020-01-03 | 山东金滢新材料有限公司 | Preparation method of pseudo-boehmite |
| CN113562753A (en) * | 2021-05-12 | 2021-10-29 | 中铝山东新材料有限公司 | Macroporous pseudo-boehmite and preparation method thereof |
| CN113277536A (en) * | 2021-05-24 | 2021-08-20 | 中铝山东有限公司 | Washing process for reducing water consumption for pseudo-boehmite washing |
| CN114853039A (en) * | 2022-05-24 | 2022-08-05 | 北京化工大学 | Pseudo-boehmite with high specific surface area and high pore volume and preparation method thereof |
| CN115124056A (en) * | 2022-06-29 | 2022-09-30 | 中国铝业股份有限公司 | Pseudo-boehmite, preparation method and application thereof |
| CN115124056B (en) * | 2022-06-29 | 2024-01-23 | 中国铝业股份有限公司 | Pseudo-boehmite and preparation method and application thereof |
| CN115818688A (en) * | 2022-10-24 | 2023-03-21 | 中铝郑州有色金属研究院有限公司 | Nano boehmite and preparation method thereof |
| CN115818688B (en) * | 2022-10-24 | 2024-04-16 | 中铝郑州有色金属研究院有限公司 | Nanometer boehmite and preparation method thereof |
| CN115974115A (en) * | 2022-12-14 | 2023-04-18 | 南昌宝弘新材料技术有限公司 | Pseudo-boehmite and preparation method thereof |
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