CN105174293A - Preparation method of pseudo-boehmite with centralized pore size distribution - Google Patents
Preparation method of pseudo-boehmite with centralized pore size distribution Download PDFInfo
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- CN105174293A CN105174293A CN201510574331.0A CN201510574331A CN105174293A CN 105174293 A CN105174293 A CN 105174293A CN 201510574331 A CN201510574331 A CN 201510574331A CN 105174293 A CN105174293 A CN 105174293A
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Abstract
The invention provides a preparation method of pseudo-boehmite with centralized pore size distribution. The preparation method comprises the following steps: neutralizing and gelatinizing an aluminum source compound under normal pressure, adding obtained slurry into a reaction kettle, and performing hydro-thermal treatment at the temperature of 100 to 200 DEG C for 0.5 to 24h; after the reaction is finished, performing solid-liquid separation and washing to obtained slurry to obtain an impurity-removed product namely a filter cake; drying and crushing the filter cake to obtain the pseudo-boehmite with the centralized pore size distribution. A preparation process is simple, and the method is low in cost and suitable for industrial production; by controlling hydro-thermal reaction conditions, a series of high-performance pseudo-boehmite products with the centralized pore size distribution can be prepared, and are suitable for serving as multiple types of catalyst carriers and have a wide application prospect.
Description
Technical field
The invention belongs to field of inorganic material preparing technology, relate to a kind of preparation method of pseudo-boehmite, particularly a kind of method by preparing the pseudo-boehmite that pore size distribution is concentrated in aluminum source compound with the laggard row hydro-thermal reaction of plastic.
Background of invention
Alumina supporter is widely used in various chemical field, especially for the hydrogenation catalyst in petroleum refining process, hydrotreatment application spans plurality of raw materials type and operational condition, but there is one or more common target, namely heteroatom contaminants (sulphur, nitrogen, oxygen, metal) is removed, improve the H/C ratio in product, thus reduce aromatics, density and/or carbon residue, cracking carbon bond is to reduce boiling range and molecular-weight average.Along with petroleum resources in poor quality and heaviness day by day, a large amount of organometallic compound and bituminous matter is there is in stock oil, require that various petroleum refinement support of the catalyst has enough large hole to spread, prevent or slow down the poisoning of catalyzer or inactivation, support of the catalyst also will keep large specific surface simultaneously, active ingredient is better disperseed thus guarantees that catalyzer has high catalytic activity.With day by day becoming more meticulous of refining of petroleum, the alumina supporter with large specific surface and pore volume is not the requirement that can meet the processing of different fractions oil, therefore proposes the concept in effective hole.For specific distillate, the hole with specific pore size distribution is considered to effective hole, for the too little reactant in aperture cannot by or the too large reactant in aperture be not enough to rest on the hole reacted in hole and be called as invalid hole, this just requires that alumina supporter has large surface and pore volume also will have narrow pore distribution simultaneously.
The main raw material producing alumina supporter is pseudo-boehmite (A1OOHnH
2o, n=0.08 ~ 0.62), also claiming false boehmite, is that a class composition is uncertain, crystallization is imperfect, have a kind of aluminium hydroxide of thin fold lamella, has the features such as specific surface is high, pore volume is large.The performance of alumina supporter determines primarily of the performance of pseudo-boehmite, particularly the pore structure of pseudo-boehmite determines the pore structure of alumina supporter substantially, therefore, high performance alumina supporter be prepared, first will obtain high performance pseudo-boehmite split.The preparation method of industrial pseudo-boehmite mainly contains: neutralisation, kind point-score, aluminium alcoholates method.Wherein neutralisation is current domestic widely used production method, specifically can be subdivided into aluminum nitrate method, Tai-Ace S 150 method, carborization, two aluminium method, pH value swing method etc.The existing major defect preparing the method for pseudo-boehmite is the product adopting single method to produce, and aperture control scope is little, pore distribution disperse, causes aluminum oxide producer a set of explained hereafter kind very limited, cannot adapt to the requirement of different catalysts.
CN101704538B discloses a kind of hydrothermal method preparing series of special-shaped graded pseudo-boehmite, aluminium salt, urea, vitriol are carried out hydrothermal treatment consists jointly, prepare the product of the various shapes such as fusiform, ellipsoid shape, three-dimensional flower-shaped, tiny balloon, but the product specific surface that this method obtains is all less, is distributed in 50 ~ 105m more
2between/g, such carrier, for the preparation of catalyzer, is unfavorable for the high dispersing of active ingredient.
CN1045461C disclose a kind of with aluminum salt solution or acid solution and alkaline solution or composite alkali aluminum salts solution for basic raw material, two kinds of solution alternately add reactor, make the method for pH value alternatively swinging between acid and alkali obtain aluminium glue, obtain specific surface 250 ~ 350m
2the concentrated hole of/g, pore volume 0.55 ~ 0.75ml/g, aperture 4 ~ 10nm accounts for the γ-Al of cumulative volume 75 ~ 90%
2o
3method.The carrier aperture that this method obtains is all between 5 ~ 7nm, and aperture can not regulate and control.
CN101357771B disclose a kind of can in higher aluminium salt concentration range with the scale preparation method realizing high-ratio surface pseudo boehmite microsphere under relative gentle hydrothermal reaction condition.The product specific surface area that this method obtains reaches as high as 371.8m2/g, but pore volume is lower, maximum 0.44ml/g, and aperture is all within the scope of 3.4 ~ 8.9nm simultaneously, cannot obtain wide aperture pseudo-boehmite equally.
CN103787388A discloses a kind of pseudo-boehmite dry glue powder and aqueous solution of urea hydrothermal treatment consists, shaping, dry, roasting obtains the method for concentrated pore distribution and alumina supporter with high specific surface area further, and this method obtains the alumina supporter that the pore volume with 10 ~ 20nm hole accounts for total pore volume about 80%.
Summary of the invention
For the deficiencies in the prior art, the preparation method of the pseudo-boehmite that the object of the present invention is to provide a kind of pore size distribution to concentrate.The present invention obtains the concentrated pseudo-boehmite powder of a series of pore size distribution by the simple hydrothermal conditions that controls.Present method preparation technology is simple, with low cost, easily carries out suitability for industrialized production.
The present invention is a kind of method being prepared pseudo-boehmite by aluminum source compound neutralization-hydrothermal treatment consists, it is characterized in that:
Comprise the steps:
(1) in aluminum source compound being carried out in atmospheric conditions and plastic; Wherein neutral temperature is 30 ~ 90 DEG C, and in addition and pH value be 7 ~ 8 or anti-addition in and endpoint pH be 7 ~ 8;
(2) step (1) gained slurry is added reactor and carry out hydrothermal treatment consists 0.5 ~ 24h in 100 ~ 200 DEG C;
(3) after reaction terminates, step (2) gained slurries are carried out solid-liquid separation, washing, obtains the product cake of imurity-removal;
(4) dry, pulverizing, obtains pseudo-boehmite powder;
According to method of the present invention, in the aluminum source compound wherein described in step (1) and plastic comprise in acidic aluminum source and alkaline matter and plastic, or in alkaline aluminium source and acidic substance and plastic, or in acidic aluminum source and alkaline aluminium source and plastic.
According to method of the present invention, wherein, the acidic aluminum source described in step (1) comprises Tai-Ace S 150, aluminum nitrate, exsiccated ammonium alum or aluminum chloride; Alkalescence aluminium source comprises sodium metaaluminate or potassium metaaluminate; Alkaline matter comprises sodium hydroxide, sodium carbonate, potassium hydroxide or ammoniacal liquor; Acidic substance comprise sulfuric acid, hydrochloric acid or nitric acid.
According to method of the present invention, wherein, step (4) gained pseudo-boehmite powder is that most probable pore size is at 6 ~ 20nm; Wherein, most probable pore size is the pseudo-boehmite powder of 6 ~ 12nm, and 80% hole integrated distribution is within the scope of most probable pore size ± 2nm; Most probable pore size is the pseudo-boehmite powder of 12 ~ 20nm, and 80% hole integrated distribution is within the scope of most probable pore size ± 3nm.Described pseudo-boehmite powder specific surface is 260 ~ 320m
2/ g, pore volume is 0.7 ~ 1.2ml/g, and most probable pore size ± 3nm endoporus accounts for total pore volume 80 ~ 90%.
Present invention also offers a kind of pseudo-boehmite powder, the most probable pore size of described pseudo-boehmite powder is at 6 ~ 20nm; Wherein, most probable pore size is the pseudo-boehmite powder of 6 ~ 12nm, and 80% hole integrated distribution is within the scope of most probable pore size ± 2nm; Most probable pore size is the pseudo-boehmite powder of 12 ~ 20nm, and 80% hole integrated distribution is within the scope of most probable pore size ± 3nm.
The present invention adopts neutralization-hydrothermal method, and emphasis, by regulating and the condition of plastic and hydrothermal condition, controls the changes such as the growth of product particle, crystal formation be perfect, and then controls size, crystalline phase, the pattern of crystal grain, thus forms the pseudo-boehmite that pore size distribution concentrates.Pseudo-boehmite prepared by the present invention has narrow pore size distribution, to make with it, for catalyzer prepared by carrier has high effective hole, effectively to improve selectivity of catalyst.
Embodiment:
Embodiment 1
End water 5L is added at 20L stirring tank, after being heated to 70 ~ 75 DEG C, under the condition of rapid stirring, also stream adds alum liquor (concentration counts 95g/L with aluminum oxide) and sodium aluminate solution (concentration counts 300g/L with aluminum oxide), hierarchy of control pH value is 7.0 ~ 7.5, charging is stopped after adding 8.0kg alum liquor and 5.2kg sodium aluminate solution altogether, gained slurry is transferred to after adding 20L autoclave, in 200 DEG C of hydrothermal treatment consists 1h, by gained slurries solid-liquid separation after process terminates, deionized water wash, obtain the product cake of imurity-removal, in 120 DEG C of dryings, pulverizing obtains pseudo-boehmite powder, its physico-chemical property is in table 1.
Embodiment 2
End water 5L is added at 20L stirring tank, after being heated to 80 ~ 85 DEG C, under the condition of rapid stirring, also stream adds alum liquor (concentration counts 95g/L with aluminum oxide) and sodium aluminate solution (concentration counts 300g/L with aluminum oxide), hierarchy of control pH value is 7.0 ~ 7.5, charging is stopped after adding 8.0kg alum liquor and 5.0kg sodium aluminate solution altogether, gained slurry is transferred to after adding 20L autoclave, in 200 DEG C of hydrothermal treatment consists 4h, by gained slurries solid-liquid separation after process terminates, deionized water wash, obtain the product cake of imurity-removal, in 120 DEG C of dryings, pulverizing obtains pseudo-boehmite powder, its physico-chemical property is in table 1.
Embodiment 3
End water 5L is added at 20L stirring tank, after being heated to 70 ~ 75 DEG C, under the condition of rapid stirring, also stream adds alum liquor (concentration counts 95g/L with aluminum oxide) and sodium aluminate solution (concentration counts 300g/L with aluminum oxide), hierarchy of control pH value is 7.5 ~ 8.0, charging is stopped after adding 8.0kg alum liquor and 5.3kg sodium aluminate solution altogether, gained slurry is transferred to after adding 20L autoclave, in 200 DEG C of hydrothermal treatment consists 12h, by gained slurries solid-liquid separation after process terminates, deionized water wash, obtain the product cake of imurity-removal, in 120 DEG C of dryings, pulverizing obtains pseudo-boehmite powder, its physico-chemical property is in table 1.
Embodiment 4
Add end water 8L at 20L stirring tank, after being heated to 40 ~ 45 DEG C, adding 8kg sodium aluminate solution (concentration counts 300g/L with aluminum oxide), pass into CO subsequently
2gas, controlling endpoint pH is 7.5, gained slurry is transferred to after adding 20L autoclave, in 100 DEG C of hydrothermal treatment consists 24h, by gained slurries solid-liquid separation after process terminates, deionized water wash, obtain the product cake of imurity-removal, dry, pulverize in 120 DEG C and obtain pseudo-boehmite powder, its physico-chemical property is in table 1.
Embodiment 5
Add end water 5L at 20L stirring tank, after being heated to 80 ~ 85 DEG C, add 8.0kg alum liquor (concentration counts 95g/L with aluminum oxide), slowly add ammoniacal liquor subsequently, controlling endpoint pH is 7.5, is transferred to by gained slurry after adding 20L autoclave, in 180 DEG C of hydrothermal treatment consists 8h, by gained slurries solid-liquid separation after process terminates, deionized water wash, obtains the product cake of imurity-removal, in 120 DEG C of dryings, pulverizing obtains pseudo-boehmite powder, and its physico-chemical property is in table 1.
Embodiment 6
Add end water 5L at 20L stirring tank, after being heated to 80 ~ 85 DEG C, add 8.0kg alum liquor (concentration counts 95g/L with aluminum oxide), slowly add ammoniacal liquor subsequently, controlling endpoint pH is 7.5, is transferred to by gained slurry after adding 20L autoclave, in 150 DEG C of hydrothermal treatment consists 1h, by gained slurries solid-liquid separation after process terminates, deionized water wash, obtains the product cake of imurity-removal, in 120 DEG C of dryings, pulverizing obtains pseudo-boehmite powder, and its physico-chemical property is in table 1.
Comparative example 1
End water 5L is added at 20L stirring tank, after being heated to 70 ~ 75 DEG C, under the condition of rapid stirring, also stream adds alum liquor (concentration counts 95g/L with aluminum oxide) and sodium aluminate solution (concentration counts 300g/L with aluminum oxide), hierarchy of control pH value is 7.0 ~ 7.5, charging is stopped after adding 8.0kg alum liquor and 5.2kg sodium aluminate solution altogether, be warming up to 85 ~ 90 DEG C of burin-in process 2h subsequently, by gained slurries solid-liquid separation after aging end, deionized water wash, obtain the product cake of imurity-removal, in 120 DEG C of dryings, pulverizing obtains pseudo-boehmite powder, its physico-chemical property is in table 1.
Comparative example 2
Add end water 8L at 20L stirring tank, after being heated to 40 ~ 45 DEG C, adding 8kg sodium aluminate solution (concentration counts 300g/L with aluminum oxide), pass into CO subsequently
2gas, controlling endpoint pH is 7.5, is warming up to 85 ~ 90 DEG C of burin-in process 2h subsequently, by gained slurries solid-liquid separation after aging end, deionized water wash, obtains the product cake of imurity-removal, dry, pulverize in 120 DEG C and obtain pseudo-boehmite powder, its physico-chemical property is in table 1.
Comparative example 3
End water 5L is added at 20L stirring tank, after being heated to 80 ~ 85 DEG C, adding 8.0kg alum liquor (concentration counts 95g/L with aluminum oxide), slowly add ammoniacal liquor subsequently, controlling endpoint pH is 7.5, be warming up to 85 ~ 90 DEG C of burin-in process 2h subsequently, by gained slurries solid-liquid separation after terminating, deionized water wash, obtain the product cake of imurity-removal, dry, pulverize in 120 DEG C and obtain pseudo-boehmite powder, its physico-chemical property is in table 1.
The physico-chemical property of each embodiment of table 1 and comparative example product
Claims (6)
1. neutralization-hydrothermal method prepares a method for pseudo-boehmite, it is characterized in that:
Comprise the steps:
1) in being carried out in atmospheric conditions by aluminum source compound and plastic, controlling neutral temperature is 30 ~ 90 DEG C, and in addition and pH value be 7 ~ 8 or anti-addition in and endpoint pH be 7 ~ 8;
2) by step 1) gained slurry adds reactor and carries out hydrothermal treatment consists 0.5 ~ 24h in 100 ~ 200 DEG C;
3) after reaction terminates, by step 2) gained slurries carry out solid-liquid separation, and washing, obtains the product cake of imurity-removal;
4) dry, pulverizing, obtains pseudo-boehmite powder.
2. method according to claim 1, it is characterized in that, step 1) described in aluminum source compound in and plastic comprise in acidic aluminum source and alkaline matter and plastic, or in alkaline aluminium source and acidic substance and plastic, or in acidic aluminum source and alkaline aluminium source and plastic.
3. method according to claim 2, is characterized in that, acidic aluminum source comprises Tai-Ace S 150, aluminum nitrate, exsiccated ammonium alum or aluminum chloride; Alkalescence aluminium source comprises sodium metaaluminate or potassium metaaluminate; Alkaline matter comprises sodium hydroxide, sodium carbonate, potassium hydroxide or ammoniacal liquor; Acidic substance comprise sulfuric acid, hydrochloric acid or nitric acid.
4. method according to claim 1, is characterized in that, step 4) gained pseudo-boehmite powder is that most probable pore size is at 6 ~ 20nm; Wherein, most probable pore size is the pseudo-boehmite powder of 6 ~ 12nm, and 80% hole integrated distribution is within the scope of most probable pore size ± 2nm; Most probable pore size is the pseudo-boehmite powder of 12 ~ 20nm, and 80% hole integrated distribution is within the scope of most probable pore size ± 3nm.
5. method according to claim 1, is characterized in that, described pseudo-boehmite powder specific surface is 260 ~ 320m
2/ g, pore volume is 0.7 ~ 1.2ml/g, and most probable pore size ± 3nm endoporus accounts for total pore volume 80 ~ 90%.
6., by the pseudo-boehmite powder that method described in claim 1 is obtained, it is characterized in that, the most probable pore size of described pseudo-boehmite powder is at 6 ~ 20nm; Wherein, most probable pore size is the pseudo-boehmite powder of 6 ~ 12nm, and 80% hole integrated distribution is within the scope of most probable pore size ± 2nm; Most probable pore size is the pseudo-boehmite powder of 12 ~ 20nm, and 80% hole integrated distribution is within the scope of most probable pore size ± 3nm.
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Cited By (7)
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| CN105645446A (en) * | 2016-03-24 | 2016-06-08 | 中国铝业股份有限公司 | Aging method of pseudo-boehmite prepared by carbonation method |
| CN110015673A (en) * | 2018-01-10 | 2019-07-16 | 北京化工大学 | Boehmite and preparation method thereof |
| CN110240187A (en) * | 2018-08-24 | 2019-09-17 | 广州凌玮科技股份有限公司 | A kind of easily distributed nm boehmite preparation method of inkjet printing adsorbing medium |
| CN112452316A (en) * | 2020-11-02 | 2021-03-09 | 青岛惠城环保科技股份有限公司 | Preparation method of easily peptized pseudo-boehmite |
| CN112479240A (en) * | 2020-11-30 | 2021-03-12 | 上海簇睿低碳能源技术有限公司 | Preparation method of high-viscosity pseudo-boehmite |
| 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 |
| WO2024046421A1 (en) * | 2022-08-31 | 2024-03-07 | 中国石油化工股份有限公司 | Mesoporous pseudo-boehmite having hydroxyl-rich surface, catalytic cracking catalyst containing pseudo-boehmite, and preparation and use thereof |
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| WO2024046421A1 (en) * | 2022-08-31 | 2024-03-07 | 中国石油化工股份有限公司 | Mesoporous pseudo-boehmite having hydroxyl-rich surface, catalytic cracking catalyst containing pseudo-boehmite, and preparation and use thereof |
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Effective date of registration: 20161031 Address after: No. three road 300131 Tianjin city Hongqiao District dingzigu No. 85 Applicant after: CNOOC TIANJIN CHEMICAL RESEARCH & DESIGN INSTITUTE Co.,Ltd. Applicant after: CNOOC ENERGY TECHNOLOGY & SERVICES Ltd. Address before: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Applicant before: CHINA NATIONAL OFFSHORE OIL Corp. Applicant before: CNOOC TIANJIN CHEMICAL RESEARCH & DESIGN INSTITUTE Co.,Ltd. Applicant before: CNOOC ENERGY TECHNOLOGY & SERVICES Ltd. |
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