CN106587085A - Preparation method of high-aperture aluminosilica gel - Google Patents
Preparation method of high-aperture aluminosilica gel Download PDFInfo
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- CN106587085A CN106587085A CN201510664896.8A CN201510664896A CN106587085A CN 106587085 A CN106587085 A CN 106587085A CN 201510664896 A CN201510664896 A CN 201510664896A CN 106587085 A CN106587085 A CN 106587085A
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Abstract
The invention relates to a preparation method of high-aperture aluminosilica gel. The problems of small aperture, scattered aperture distribution, narrow silica-alumina ratio adjusting range and non-uniform silicon and aluminum distribution of aluminosilica gel synthesized in the prior art are mainly solved in the invention. The high-aperture aluminosilica gel prepared from pseudo-boehmite and silica sol through a pH swing technology well solves the problems. The method has the advantages of simplicity in operation and good repeatability, and the prepared aluminosilica gel has the characteristics of high aperture, wide silica-alumina ratio adjusting range, good stability and low production cost, and can be used in the fields of adsorption separation and catalysis.
Description
Technical field
The present invention relates to a kind of preparation method of large aperture Alusil.
Background technology
Alusil, chemical molecular formula mSiO2·nAl2O3·xH2O, is a kind of salic silica gel, stable chemical nature,
Do not burn, insoluble in any solvent.Integrate silica gel and aluminium glue advantage, absorbability and pore silicon in low relative temperature
Quite, in high relative humidity, absorbability is higher than Kiselgel A by 6～10%, and heat stability is than Kiselgel A (200 DEG C) for glue
It is high more than 150 DEG C, Alusil in physical property have higher specific surface area, pore volume and aperture, can by adjust silica alumina ratio come
The acidity on adjustment surface, is mainly used in gas dehydration, and temp.-changing adsorption separates lighter hydrocarbons, it is also possible to urging in petroleum chemical industry
Agent and catalyst carrier.It is more in the applied research of catalytic field to Alusil, split primarily as hydrofinishing, hydrogenation
Change or the research of catalytic cracking catalyst carrier.
At present, the method for preparing Alusil for industrially using, mainly there is three kinds：1) mix during preparing silica gel few
Amount aluminium salt, by hydrolysis Alusil is obtained, and this method is restricted to the incorporation of aluminum, and incorporation is too high to affect Alusil
Pore structure, the incorporation of general aluminum is limited to less than 20%；2) macropore Alusil is prepared using template agent method, such as Germany
The SIRAL series of products of Sasol companies, it is relatively costly；3) carbonizatin method is using aluminium salt and silicon-containing compound and CO2Gas plastic,
Plastic process adopts pH swing methods, swing process to introduce silicon source, and the Alusil aperture that the method is obtained is less, need to add opening up hole agent
Carry out hole diameter enlargement.
CN1765742A discloses a kind of method of preparing amorphous silicon alumnium using carbonization, including sodium aluminate solution and siliceous chemical combination
The mixture and CO of thing solution2Gas plastic, is filtered, washed and dried, and wherein plastic process is to adopt pH swing methods, and
And every time in swing process, silicon-containing compound solution is that distribution is added.The preparation method low cost, it is pollution-free.Gained
Amorphous silica-alumina has larger specific surface area and pore volume, suitable acidity, and the silicon oxide containing q.s, can conduct
Catalytic cracking, be hydrocracked and hydrotreating catalyst carrier component, be alternatively arranged as the carrier component of olefin oligomerization catalyst.
GB2166971 discloses a kind of amorphous silica-alumina preparation method, and it is first under high pH (12-12.5) by composite alkali aluminum
After hydrochlorate and silicate mixing, then it is obtained with reacting aluminum sulfate, knowable to the embodiment of the patent, the SiO of its product sial2
Content less than in the case of 35w%, specific surface 277m2/ g, pore volume 0.31ml/g.Although having lytic activity, it
Shortcoming remain pore volume and specific surface is not high, be not enough to separately as carrier component during the metal component for carrying higher amount.Should
Patented method is a kind of using the quick hybrid mode plastic of pump, and high to equipment requirements, production difficulty is big, with certain production
Limitation.
US4758338 pH swing methods are formed after pH value 2-10 swings obtain alumina sol silicon compound is added
Amorphous silica-alumina, but the process operation is complicated, it is difficult to control, and the SiO of its product2It is not high, highest only 8.7w%,
Be mainly used as do not need acidic cleavage function Hydrobon catalyst carrier, product specific surface 308m2/ g, pore volume can
Up to 1.78ml/g, but the pore volume of 3-10nm only 0.31ml/g, mainly on the macropore of 10-100nm.EP0788270 is one
Plant and process aluminium oxide, then hydrothermal treatment with waterglass or Ludox to improve amorphous silica-alumina product property, it is final without fixed
Shape sial contains SiO2In 6-12w%, the 12w% hydrothermal treatment consists that product specific surface highest Ludox process is obtained are without fixed
Shape sial, specific surface also only has 214m2/g, and the preparation method condition of the product is harsh, and hydrothermal treatment consists energy consumption is big.
CN1210755A discloses a kind of highly acidity, the preparation method of the macropore amorphous silica-alumina of high-ratio surface, its silicon oxide
Content is 10-50w%, specific surface area 350-600m2/ g, the silica content that the method is introduced is also severely limited.
CN101239328B is the invention discloses a kind of amorphous silica-alumina and preparation method thereof.The amorphous silica-alumina is using simultaneously
Stream coprecipitation method, not only process is simple, easy to control, while using CO2With wind stirring, the full and uniform mixing of reactant is made,
Ensure that silicon and aluminium atom effectively interact, so as to form the sial of bigger serface and pore volume, pore size distribution is concentrated very much,
The pore volume of 4～10nm of aperture accounts for the 85%～95% of total pore volume,>The pore volume of 15nm accounts for less than the 5% of total pore volume.The life
Product process without containing ammonia, nitrogen waste water discharge, without environmentally friendly pollution problem.
The content of the invention
One of the technical problem to be solved be in order to solve prior art preparation Alusil aperture is little, pore-size distribution
Do not concentrate, the problem that silica alumina ratio range of accommodation is narrow and Distribution of silicon and aluminium is uneven, there is provided a kind of new large aperture Alusil.The material
The characteristics of with pore-size distribution concentration, wide silica alumina ratio range of accommodation and uniform Distribution of silicon and aluminium.
The two of the technical problem to be solved are to provide a kind of preparation method of large aperture Alusil.
To solve one of above-mentioned technical problem, the technical solution used in the present invention is as follows：A kind of large aperture Alusil, including with
Lower weight relationships composition：SiO2:Al2O3=1:99～80:20.
In above-mentioned technical proposal, the specific surface area of Alusil is 300～500m2/ g, 0.5～1.4cm of pore volume3/ g, aperture 8～
12nm distributions account for 75～90%.
To solve the two of above-mentioned technical problem, the technical solution used in the present invention is as follows：A kind of preparation side of large aperture Alusil
Method, comprises the following steps：
1. boehmite is added to the water into stirring to pulp；
2. to 1. middle addition Ludox, stir, then acid adding control slurry pH value temperature is risen to into 30 to after 3～5～
90 DEG C, 0.5～3h of constant temperature；
3. in quick whipping process to being slowly added dropwise alkali liquor, control slurry pH value to 9～10 in 2..
4. filtering and washing, drying finished product.
In above-mentioned technical proposal, the 280～300m of specific surface area of described boehmite2/ g, 0.7～1.1cm of pore volume3/g、
9～13nm of average pore size.
In above-mentioned technical proposal, solid-liquid weight ratio is 5 in described pulper slurry:1～10:1.
In above-mentioned technical proposal, described Ludox specification is SiO in colloidal sol2Percentage by weight is 20～40%.
In above-mentioned technical proposal, described acid be in acetic acid, citric acid, oxalic acid, nitric acid, hydrochloric acid, phosphoric acid or sulphuric acid extremely
Few one kind.
In above-mentioned technical proposal, whipping temp rises to 50～90 DEG C after acid adding.
In above-mentioned technical proposal, described alkali is ammonia or at least one in organic amine.
In above-mentioned technical proposal, drying temperature is 70～150 DEG C, drying time is 6～48h.
The large aperture Alusil that the present invention is provided can be used for the fields such as adsorbing separation, catalysis.
Present invention employs pH value swing method, number of oscillations be 1 time less than traditional processing method, it is big in boehmite
Ludox is introduced on the basis of pore structure, can increasing specific surface area, eliminate aperture, allow pore-size distribution more to concentrate, while also changing
The acidity of Alusil has been apt to it, sial ratio modulation scope is wide, better than traditional method.In addition, by stirring temperature in preparation process
Degree, pH value and drying temperature control can the parameter such as the pore volume of modulation Alusil product, aperture within the specific limits, take
Obtained preferable technique effect.
Below by embodiment, the present invention is further elaborated.
Specific embodiment
【Embodiment 1】
100g macropore boehmites (the neat continuous heavy rain chemical industry of Shandong Zibo) are added in 1L water and is beaten, 30 minutes backward serosity
Middle addition 175g Ludox (SiO2Content 40w%), continue to be stirred until homogeneous, nitric acid is added in serosity and slurry is controlled
Liquid pH value is 5.0, is warming up to 60 DEG C, and constant temperature is stirred 1 hour, be slowly added dropwise in serosity ammonia and quickly stirring up to
Slurry pH value is 10, continues to stir 1 hour, is cooled to 30 DEG C, filtering and washing, dries 12 hours in 100 DEG C, i.e.,
Obtain Alusil product (SiO2Weight accounts for 50w%).
N is carried out to obtained Alusil under the conditions of this2The parameter indexs such as absorption test, specific surface area, pore volume, aperture are shown in
Table 1.
【Embodiment 2】
100g macropore boehmites (the neat continuous heavy rain chemical industry of Shandong Zibo) are added in 1L water and is beaten, 30 minutes backward serosity
Middle addition 75g Ludox (SiO2Content 40w%), continue to be stirred until homogeneous, nitric acid is added in serosity and slurry is controlled
Liquid pH value is 5.0, is warming up to 60 DEG C, and constant temperature is stirred 1 hour, be slowly added dropwise in serosity ammonia and quickly stirring up to
Slurry pH value is 10, continues to stir 1 hour, is cooled to 30 DEG C, filtering and washing, dries 12 hours in 100 DEG C, i.e.,
Obtain Alusil product (SiO2Weight accounts for 30w%).
N is carried out to obtained Alusil under the conditions of this2The parameter indexs such as absorption test, specific surface area, pore volume, aperture are shown in
Table 1.
【Embodiment 3】
100g macropore boehmites (the neat continuous heavy rain chemical industry of Shandong Zibo) are added in 1L water and is beaten, 30 minutes backward serosity
Middle addition 19.4g Ludox (SiO2Content 40w%), continue to be stirred until homogeneous, nitric acid is added in serosity and slurry is controlled
Liquid pH value is 5.0, is warming up to 60 DEG C, and constant temperature is stirred 1 hour, be slowly added dropwise in serosity ammonia and quickly stirring up to
Slurry pH value is 10, continues to stir 1 hour, is cooled to 30 DEG C, filtering and washing, dries 12 hours in 100 DEG C, i.e.,
Obtain Alusil product (SiO2Weight accounts for 10w%).
N is carried out to obtained Alusil under the conditions of this2The parameter indexs such as absorption test, specific surface area, pore volume, aperture are shown in
Table 1.
【Embodiment 4】
100g macropore boehmites (the neat continuous heavy rain chemical industry of Shandong Zibo) are added in 1L water and is beaten, 30 minutes backward serosity
Middle addition 408g Ludox (SiO2Content 40w%), continue to be stirred until homogeneous, nitric acid is added in serosity and slurry is controlled
Liquid pH value is 5.0, is warming up to 60 DEG C, and constant temperature is stirred 1 hour, be slowly added dropwise in serosity ammonia and quickly stirring up to
Slurry pH value is 10, continues to stir 1 hour, is cooled to 30 DEG C, filtering and washing, dries 12 hours in 100 DEG C, i.e.,
Obtain Alusil product (SiO2Weight accounts for 70w%).
N is carried out to obtained Alusil under the conditions of this2The parameter indexs such as absorption test, specific surface area, pore volume, aperture are shown in
Table 1.
【Embodiment 5】
100g macropore boehmites (the neat continuous heavy rain chemical industry of Shandong Zibo) are added in 0.8L water and is beaten, 30 minutes backward slurries
175g Ludox (SiO are added in liquid2Content 40w%), continue to be stirred until homogeneous, nitric acid is added in serosity and is controlled
Slurry pH value is 5.0, is warming up to 60 DEG C, and constant temperature is stirred 1 hour, ammonia is slowly added dropwise in serosity and is quickly stirred straight
It is 10 to slurry pH value, continues to stir 1 hour, be cooled to 30 DEG C, filtering and washing is dried 12 hours in 100 DEG C,
Obtain final product Alusil product (SiO2Weight accounts for 50w%).
N is carried out to obtained Alusil under the conditions of this2The parameter indexs such as absorption test, specific surface area, pore volume, aperture are shown in
Table 1.
【Embodiment 6】
100g macropore boehmites (the neat continuous heavy rain chemical industry of Shandong Zibo) are added in 1L water and is beaten, 30 minutes backward serosity
Middle addition 233.3g Ludox (SiO2Content 30w%), continue to be stirred until homogeneous, nitric acid is added in serosity and is controlled
Slurry pH value is 5.0, is warming up to 60 DEG C, and constant temperature is stirred 1 hour, ammonia is slowly added dropwise in serosity and is quickly stirred straight
It is 10 to slurry pH value, continues to stir 1 hour, be cooled to 30 DEG C, filtering and washing is dried 12 hours in 100 DEG C,
Obtain final product Alusil product (SiO2Weight accounts for 50w%).
N is carried out to obtained Alusil under the conditions of this2The parameter indexs such as absorption test, specific surface area, pore volume, aperture are shown in
Table 1.
【Embodiment 7】
100g macropore boehmites (the neat continuous heavy rain chemical industry of Shandong Zibo) are added in 1L water and is beaten, 30 minutes backward serosity
Middle addition 175g Ludox (SiO2Content 40w%), continue to be stirred until homogeneous, hydrochloric acid is added in serosity and slurry is controlled
Liquid pH value is 5.0, is warming up to 60 DEG C, and constant temperature is stirred 1 hour, be slowly added dropwise in serosity ammonia and quickly stirring up to
Slurry pH value is 10, continues to stir 1 hour, is cooled to 30 DEG C, filtering and washing, dries 12 hours in 100 DEG C, i.e.,
Obtain Alusil product (SiO2Weight accounts for 50w%).
N is carried out to obtained Alusil under the conditions of this2The parameter indexs such as absorption test, specific surface area, pore volume, aperture are shown in
Table 1.
【Embodiment 8】
100g macropore boehmites (the neat continuous heavy rain chemical industry of Shandong Zibo) are added in 1L water and is beaten, 30 minutes backward serosity
Middle addition 175g Ludox (SiO2Content 40w%), continue to be stirred until homogeneous, acetic acid is added in serosity and slurry is controlled
Liquid pH value is 5.0, is warming up to 60 DEG C, and constant temperature is stirred 1 hour, be slowly added dropwise in serosity ammonia and quickly stirring up to
Slurry pH value is 10, continues to stir 1 hour, is cooled to 30 DEG C, filtering and washing, dries 12 hours in 100 DEG C, i.e.,
Obtain Alusil product (SiO2Weight accounts for 50w%).
N is carried out to obtained Alusil under the conditions of this2The parameter indexs such as absorption test, specific surface area, pore volume, aperture are shown in
Table 1.
【Embodiment 9】
100g macropore boehmites (the neat continuous heavy rain chemical industry of Shandong Zibo) are added in 1L water and is beaten, 30 minutes backward serosity
Middle addition 175g Ludox (SiO2Content 40w%), continue to be stirred until homogeneous, nitric acid is added in serosity and slurry is controlled
Liquid pH value is 4.0, is warming up to 60 DEG C, and constant temperature is stirred 1 hour, be slowly added dropwise in serosity ammonia and quickly stirring up to
Slurry pH value is 10, continues to stir 1 hour, is cooled to 30 DEG C, filtering and washing, dries 12 hours in 100 DEG C, i.e.,
Obtain Alusil product (SiO2Weight accounts for 50w%).
N is carried out to obtained Alusil under the conditions of this2The parameter indexs such as absorption test, specific surface area, pore volume, aperture are shown in
Table 1.
【Embodiment 10】
100g macropore boehmites (the neat continuous heavy rain chemical industry of Shandong Zibo) are added in 1L water and is beaten, 30 minutes backward serosity
Middle addition 175g Ludox (SiO2Content 40w%), continue to be stirred until homogeneous, nitric acid is added in serosity and slurry is controlled
Liquid pH value is 3.0, is warming up to 60 DEG C, and constant temperature is stirred 1 hour, be slowly added dropwise in serosity ammonia and quickly stirring up to
Slurry pH value is 10, continues to stir 1 hour, is cooled to 30 DEG C, filtering and washing, dries 12 hours in 100 DEG C, i.e.,
Obtain Alusil product (SiO2Weight accounts for 50w%).
N is carried out to obtained Alusil under the conditions of this2The parameter indexs such as absorption test, specific surface area, pore volume, aperture are shown in
Table 1.
【Embodiment 11】
100g macropore boehmites (the neat continuous heavy rain chemical industry of Shandong Zibo) are added in 1L water and is beaten, 30 minutes backward serosity
Middle addition 175g Ludox (SiO2Content 40w%), continue to be stirred until homogeneous, nitric acid is added in serosity and slurry is controlled
Liquid pH value is 5.0, is warming up to 80 DEG C, and constant temperature is stirred 1 hour, be slowly added dropwise in serosity ammonia and quickly stirring up to
Slurry pH value is 10, continues to stir 1 hour, is cooled to 30 DEG C, filtering and washing, dries 12 hours in 100 DEG C, i.e.,
Obtain Alusil product (SiO2Weight accounts for 50w%).
N is carried out to obtained Alusil under the conditions of this2The parameter indexs such as absorption test, specific surface area, pore volume, aperture are shown in
Table 1.
【Embodiment 12】
100g macropore boehmites (the neat continuous heavy rain chemical industry of Shandong Zibo) are added in 1L water and is beaten, 30 minutes backward serosity
Middle addition 175g Ludox (SiO2Content 40w%), continue to be stirred until homogeneous, nitric acid is added in serosity and slurry is controlled
Liquid pH value is 5.0, is warming up to 60 DEG C, and constant temperature is stirred 1 hour, be slowly added dropwise in serosity ammonia and quickly stirring up to
Slurry pH value is 9, continues to stir 1 hour, is cooled to 30 DEG C, and filtering and washing is dried 12 hours in 100 DEG C, is obtained final product
Alusil product (SiO2Weight accounts for 50w%).
N is carried out to obtained Alusil under the conditions of this2The parameter indexs such as absorption test, specific surface area, pore volume, aperture are shown in
Table 1.
【Embodiment 13】
100g macropore boehmites (the neat continuous heavy rain chemical industry of Shandong Zibo) are added in 1L water and is beaten, 30 minutes backward serosity
Middle addition 175g Ludox (SiO2Content 40w%), continue to be stirred until homogeneous, nitric acid is added in serosity and slurry is controlled
Liquid pH value is 5.0, is warming up to 90 DEG C, and constant temperature is stirred 1 hour, urea liquid is slowly added dropwise in serosity and is quickly stirred
Until slurry pH value is 10, continue to stir 1 hour, be cooled to 30 DEG C, filtering and washing is dried 12 hours in 100 DEG C,
Obtain final product Alusil product (SiO2Weight accounts for 50w%).
Carry out the parameter indexs such as N2 absorption tests, specific surface area, pore volume, aperture to obtained Alusil under the conditions of this to be shown in
Table 1.
【Embodiment 14】
100g macropore boehmites (the neat continuous heavy rain chemical industry of Shandong Zibo) are added in 1L water and is beaten, 30 minutes backward serosity
Middle addition 175g Ludox (SiO2Content 40w%), continue to be stirred until homogeneous, nitric acid is added in serosity and slurry is controlled
Liquid pH value is 5.0, is warming up to 60 DEG C, and constant temperature is stirred 1 hour, be slowly added dropwise in serosity ammonia and quickly stirring up to
Slurry pH value is 10, continues to stir 1 hour, is cooled to 30 DEG C, filtering and washing, dries 12 hours in 130 DEG C, i.e.,
Obtain Alusil product (SiO2Weight accounts for 50w%).
N is carried out to obtained Alusil under the conditions of this2The parameter indexs such as absorption test, specific surface area, pore volume, aperture are shown in
Table 1.
【Embodiment 15】
100g macropore boehmites (the neat continuous heavy rain chemical industry of Shandong Zibo) are added in 1L water and is beaten, 30 minutes backward serosity
Middle addition 175g Ludox (SiO2Content 40w%), continue to be stirred until homogeneous, nitric acid is added in serosity and slurry is controlled
Liquid pH value is 5.0, is warming up to 60 DEG C, and constant temperature is stirred 1 hour, be slowly added dropwise in serosity ammonia and quickly stirring up to
Slurry pH value is 10, continues to stir 1 hour, is cooled to 30 DEG C, filtering and washing, dries 24 hours in 130 DEG C, i.e.,
Obtain Alusil product (SiO2Weight accounts for 50w%).
N is carried out to obtained Alusil under the conditions of this2The parameter indexs such as absorption test, specific surface area, pore volume, aperture are shown in
Table 1.
【Comparative example 1】
Commercially available SiO2Content is 30% Alusil A, carries out N2The ginsengs such as absorption test, specific surface area, pore volume, aperture
Number index is shown in table 1.
【Comparative example 2】
Commercially available SiO2Content is 10% Alusil B, carries out N2The ginsengs such as absorption test, specific surface area, pore volume, aperture
Number index is shown in table 1.
Table 1
Claims (10)
1. a kind of large aperture Alusil, including following weight relationships is constituted：SiO2:Al2O3=1:99～80:20.
2. large aperture Alusil according to claim 1, it is characterised in that 300～500m of specific surface area2/ g, 0.5～1.4cm of pore volume3/ g, 8～12nm of aperture account for total pore volume 75～90%.
3. the preparation method of the large aperture Alusil described in claim 1 or 2, comprises the following steps：
1. boehmite is added to the water into stirring to pulp；
2. to 1. middle addition Ludox, stir, then temperature is risen to 30～90 DEG C by acid adding control slurry pH value to after 3～5,0.5～3h of constant temperature；
3. in quick whipping process to being slowly added dropwise alkali liquor, control slurry pH value to 9～10 in 2..
4. filtering and washing, drying finished product.
4. the preparation method of large aperture Alusil according to claim 3, it is characterised in that the 280～300m of specific surface area of described boehmite2/ g, 0.7～1.1cm of pore volume3/ g, 9～13nm of average pore size.
5. the preparation method of large aperture Alusil according to claim 3, it is characterised in that solid-liquid weight ratio is 5 in described pulper slurry:1～10:1.
6. the preparation method of large aperture Alusil according to claim 3, it is characterised in that described Ludox specification is SiO in colloidal sol2Percentage by weight is 20～40%.
7. the preparation method of large aperture Alusil according to claim 3, it is characterised in that described acid is at least one in acetic acid, citric acid, oxalic acid, nitric acid, hydrochloric acid, phosphoric acid or sulphuric acid.
8. the preparation method of large aperture Alusil according to claim 3, it is characterised in that whipping temp rises to 50～90 DEG C after acid adding.
9. the preparation method of large aperture Alusil according to claim 3, it is characterised in that described alkali is ammonia or at least one in organic amine.
10. the preparation method of large aperture Alusil according to claim 3, it is characterised in that drying temperature is 70～150 DEG C, drying time is 6～48h.
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| CN112340742A (en) * | 2021-01-11 | 2021-02-09 | 东营一鸣新材料有限公司 | Macroporous high-purity silica-alumina gel and preparation method thereof |
| CN113184860A (en) * | 2021-05-18 | 2021-07-30 | 济南大学 | Preparation method of pore structure controllable silica-alumina gel |
| CN114700030A (en) * | 2022-05-19 | 2022-07-05 | 青岛惠城环保科技股份有限公司 | Preparation method of fire-resistant oil adsorption regenerant |
| CN115957798A (en) * | 2021-10-09 | 2023-04-14 | 中国石油化工股份有限公司 | Catalytic cracking catalyst with rich mesoporous structure and preparation method thereof |
| CN115990505A (en) * | 2021-10-18 | 2023-04-21 | 中国石油化工股份有限公司 | Catalytic cracking auxiliary agent containing large-particle-size sol and preparation method thereof |
| CN115990496A (en) * | 2021-10-18 | 2023-04-21 | 中国石油化工股份有限公司 | Catalytic cracking auxiliary agent containing large-particle-size sol and preparation method thereof |
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