CN108046280A - A kind of Alusil and preparation method thereof - Google Patents
A kind of Alusil and preparation method thereof Download PDFInfo
- Publication number
- CN108046280A CN108046280A CN201711421111.XA CN201711421111A CN108046280A CN 108046280 A CN108046280 A CN 108046280A CN 201711421111 A CN201711421111 A CN 201711421111A CN 108046280 A CN108046280 A CN 108046280A
- Authority
- CN
- China
- Prior art keywords
- alusil
- acid
- temperature
- treatment
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
- C01B33/28—Base exchange silicates, e.g. zeolites
- C01B33/2807—Zeolitic silicoaluminates with a tridimensional crystalline structure possessing molecular sieve properties; Isomorphous compounds wherein a part of the aluminium ore of the silicon present may be replaced by other elements such as gallium, germanium, phosphorus; Preparation of zeolitic molecular sieves from molecular sieves of another type or from preformed reacting mixtures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
-
- 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
-
- 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
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Silicon Compounds (AREA)
- Catalysts (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of Alusil and preparation method thereof, belong to the technical field of Alusil.In the Alusil of the present invention, Al2O3Mass content for 3 8%, SiO2Mass content be not less than 82%；The specific surface area of Alusil is 300 550m2/ g, pore volume are 0.6 1.0mL/g, and compression strength is not less than 50N；The present invention gives the preparation method of above-mentioned Alusil, by sodium silicate, aluminium salt and raw material acid by collosol and gel, aging, exchange acid treatment, washing, ammonia treatment and drying and obtain.Silica alumina ratio adjustable range is wide in the Alusil of the present invention, pore volume and large specific surface area, and compression strength is high, and skeleton structure and even intensity, product quality are stablized；Preparation process is simple, easy to operate, can be widely applied to catalyst and catalyst carrier, adsorbing separation and the fields such as system with molecular sieve for preparing is standby.
Description
Technical field
The invention belongs to the technical fields of Alusil, particularly relate to a kind of Alusil and preparation method thereof.
Background technology
Alusil is a kind of silica gel containing aluminium oxide, chemical molecular formula mSiO2·nAl2O3·xH2O, chemically
Matter is stable, do not burn, insoluble in any solvent, is mainly used for the catalyst and catalyst carrier of petroleum chemical industry, industrially
It is additionally operable to drying machine, liquid absorbent and gas separation etc..
The preparation method of Alusil in the prior art, there are mainly three types of：1) sol-gal process adds aluminium salt, and this method obtains
Alusil in silica aluminum chemistry key coordinate bond is stable, skeleton structure is stable, product strength is high, stable skeleton structure is conducive to
The adjustment of pore structure and the load of catalyst, the solution control during colloidal sol and gel of this method are uneven, it is impossible to shape
Into homogeneous solution, majority is suspension or emulsion, so as to influence the uniformity of product；2) sial is prepared using template agent method
Glue is, it is necessary to increase template removing step, and the complex procedures, existing during template agent removing is removed influences frame strength, hole
The problem of structure and impurity content, also, template agent method also there are environmental protection treatment it is difficult and of high cost the problem of；3) carbonizatin method utilizes
Aluminium salt and silicon-containing compound and carbon dioxide reaction gel, gel process introduce silicon source by pH swing methods in swing process, should
The Alusil pore volume aperture that method obtains is smaller, it is necessary to which reaming, frame strength and specific surface area after reaming can all decline, cause
It is subject to certain restrictions in application field.
United States Patent (USP) US4758338 discloses a kind of preparation method of Alusil, using pH swing method control ph in 2-
10 and obtain alumina sol, then add in silicon source and obtain amorphous silicon aluminium glue, the reaction process of this method is complicated, it is difficult to control
System, also, product strength is not high, and dioxide-containing silica is low, no more than 10%.Chinese CN106587085A discloses a kind of macropore
The preparation method of Alusil, adds in Ludox after boehmite is beaten, control ph adds in alkali after 3-5 and heat preservation and adjusts slurry
Liquid pH value obtains silica-alumina gel in 9-10, and macropore Alusil is obtained after drying；This method reaction process is by mixing evenness, raw material
Boehmite mashing, the limitation of the pH value uniformity, reaction process cannot obtain uniform silica-alumina gel, silica aluminum chemistry coordinate bond
Content is low, also, obtained macropore Alusil intensity is low, is restricted on field is used.Chinese CN1765742A is public
A kind of method that carbonizatin method prepares amorphous silicon aluminium glue, sodium aluminate solution and the mixing of silicon-containing compound solution have been opened, has been passed through dioxy
Change carbon gas by control ph plastic, product is obtained after filtration washing drying；The manufacturing cost of this method is low, and obtained nothing is determined
Type Alusil has big specific surface area and pore volume, can as catalytic cracking carrier of hydrocracking catalyst, although this method is anti-
Answer the silicon-aluminum sol that process initial stage obtains more uniform, with the progress of the process of later stage gel, the product uniformity declines, obtains
Product strength is low.
The content of the invention
The present invention provides a kind of Alusil and preparation method thereof, solves the dioxide-containing silica of Alusil in the prior art
The problem of low and specific surface area, pore volume and intensity cannot be taken into account.
A kind of Alusil of the present invention, is mainly realized by the following technical programs：In the Alusil,
Al2O3Mass content be 3-8%, SiO2Mass content be not less than 82%；The specific surface area of the Alusil is 300-
550m2/ g, pore volume 0.6-1.0mL/g, compression strength are not less than 50N.
In the Alusil of the present invention, SiO2Content is high, Al2O3Content is adjustable, and silica alumina ratio adjustable range is wide, skeleton structure and
Even intensity, large pore volume, large specific surface area, compression strength is high, and skeleton structure and pore structure are stablized, good product quality, big pore volume
It is taken into account with specific surface area and high compressive strength, can be widely applied to catalyst and catalyst carrier, adsorbing separation and molecular sieve
The fields such as preparation.
As a kind of preferred embodiment, the pore volume of the Alusil is 0.7-0.9mL/g, pore size 6-
10nm.The Alusil large pore volume of the present invention, uniform pore diameter, skeleton structure are stablized, and can be resistant to ammonia treatment, and properties of product are stablized,
Have a wide range of application.
A kind of preparation method of Alusil of the present invention, is mainly realized by the following technical programs：Including
Following steps：1) aluminium salt and raw material acid are taken, is mixed, is added water, the acid solution of aluminium salt is made, the mass concentration for making aluminium salt is 1-
20%, the mass concentration of raw material acid is 5-45%；Sodium silicate is taken, adds in water, the flower bulb alkali soluble that mass concentration is 5-25% is made
Liquid；2) sodium silicate solution obtained by step 1) is added in the acid solution obtained by step 1), sodium silicate solution and acid solution
Volume ratio is 15-18:5-7 carries out solgel reaction, reaction pressure 0.05-1.5MPa, after reaction at 15-45 DEG C
PH value is 2.5-8.5, obtains gel；3) by the gel obtained by step 1), aging exchanges acid treatment, washing, and ammonia treatment is dried, obtained
Alusil.
The present invention is using sodium silicate as silicon source, and using aluminium salt as silicon source, aluminium salt can be aluminium chloride, aluminum nitrate and aluminum sulfate etc.
Deng aluminium salt is first dissolved into raw material acid,, can since aluminium salt has been formulated into raw material acid in colloidal sol and gel reaction process
With raw material acid complete miscibility and forming homogeneous liquid, homogeneous gel can be formed with sodium silicate reaction, solution to be transparent or
Translucent liquid ensure that the skeleton of Alusil and the uniformity of intensity in reaction process, in aging and exchange the work of acid soak
Under, the skeleton structure and pore structure of Alusil are further stabilized, by washing and ammonia treatment is by low adsorption and low activity
Micropore and aperture are disposed to obtain the pore volume of bigger, large pore volume, compression strength height；The preparation process is simple, operation
It is convenient, it is easy to accomplish industrialization can be widely applied to the fields such as catalyst and catalyst carrier, adsorbing separation and system with molecular sieve for preparing be standby
Method.
As a kind of preferred embodiment, the balling-up distance of the gel obtained by the step 1) is 1-3m, and is being received
Into row buffering in device, the pH value of water is 6.0-9.0 in receiver, and the temperature of water is 20-40 DEG C in receiver.Raw material acid can be
Organic acid, or inorganic acid can be monoacid or polyacid, be preferably sulfuric acid；The solgel reaction is in reactor
It is interior to carry out and use receiver into row buffering.
As a kind of preferred embodiment, in the step 2), during ammonia treatment, ammonia used is ammonium hydroxide, ammonium chloride, sulphur
Any one or a few in sour ammonium, ammonium carbonate or ammonium hydrogen carbonate, concentration for the treatment of 0.05-1.5%, treatment temperature 20-90
DEG C, processing time 1-12h；Preferably：Ammonia used is ammonium hydroxide, and concentration for the treatment of 0.1-1%, treatment temperature is 40-80 DEG C,
Processing time is 4-8h.The purpose of ammonia treatment is also that micropore by low adsorption and low activity and aperture are disposed to obtain bigger
Pore volume, at this point, the micropore and aperture that wash the low adsorption do not disposed and low activity are handled again, so as to obtain
The pore volume of bigger.
As a kind of preferred embodiment, the mass concentration of the sodium silicate is 10-20%, and the mass concentration of aluminium salt is
5-15%, the mass concentration of raw material acid is 10-30%, and the pH value of reaction is 3.5-7.5.Due to sodium silicate, aluminium salt and raw material acid
Concentration can influence the acid-base reaction i.e. uniformity of solgel reaction, the present invention strictly controls the concentration of three kinds of raw materials, obtains
Uniform gel has been arrived, the skeleton uniformity of Alusil in reaction process and the uniformity of intensity has been fully ensured that, has improved silicon
The comprehensive performance of aluminium glue.
As a kind of preferred embodiment, in the step 2), during aging, temperature is 25-85 DEG C, time 0.5-
50h；Preferably：Temperature is 30-60 DEG C, time 2-35h.By the control of aging temperature and ageing time, further stablize
The skeleton structure and pore structure of Alusil, to improve the quality stability of Alusil.
As a kind of preferred embodiment, in the step 2), when exchanging acid treatment, exchanged acid is hydrochloric acid, sulfuric acid, nitre
Any one or a few in sour aluminium, nitric acid, aluminum sulfate, oxalic acid or citric acid, the mass concentration of exchanged acid is 0.05-10%,
Treatment temperature is 30-100 DEG C, processing time 1-12h；Preferably：The mixing that exchanged acid is sulfuric acid, oxalic acid and aluminum sulfate form
Acid, the mass concentration of exchanged acid is 0.1-5%, and treatment temperature is 30-60 DEG C, processing time 2-6h.Exchanged acid is not stringent
Acid in meaning is the acid substance of its solution display, including hydrochloric acid, sulfuric acid, also including aluminum nitrate and aluminum sulfate；After aging
Gel, which is placed directly in exchanged acid, to be impregnated, so as to further stabilize the skeleton structure and pore structure of Alusil, to carry
The quality stability of high Alusil.
As a kind of preferred embodiment, in the step 2), during washing, temperature is 20-90 DEG C, washes the pH of terminal
It is worth for 4.5-7.0, the gel specific resistance after washing is not less than 1000 Ω cm；Preferably：Temperature is 30-60 DEG C, washes terminal
PH value 5.0-6.5.The purpose of washing is that micropore by low adsorption and low activity and aperture are disposed to obtain the pore volume of bigger
Product judges washing terminal by pH value, and it is easy to judge, easy to control.
As a kind of preferred embodiment, in the step 2), during drying, temperature is 80-400 DEG C, time 12-
48h；Preferably：Using stoving process twice, the temperature of drying is 80-200 DEG C, time 10-36h for the first time, second of baking
Dry temperature is 200-400 DEG C, time 2-12h.Drying is exactly in order to remove the moisture in Alusil, so as to obtain drying
Particle；After drying, final product is obtained by screening and packing.
Compared with prior art, the beneficial effects of the invention are as follows：In the Alusil of the present invention, SiO2Content is high, Al2O3Contain
Measure adjustable, silica alumina ratio adjustable range is wide, skeleton structure and even intensity, large pore volume, large specific surface area, and compression strength is high, skeleton
Structure and pore structure are stablized, and good product quality, big pore volume and specific surface area and high compressive strength are taken into account, can be widely applied to urge
The fields such as agent and catalyst carrier, adsorbing separation and system with molecular sieve for preparing be standby；The preparation process is simple, easy to operate, it is easy to accomplish
Industrialization.
Specific embodiment
Technical scheme is clearly and completely described below in conjunction with specific embodiments of the present invention, is shown
So, described embodiment is only the part of the embodiment of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, those of ordinary skill in the art's all other embodiments obtained without creative efforts, all
Belong to the scope of protection of the invention.
A kind of Alusil of the present invention, in the Alusil, Al2O3Mass content be 3-8%, SiO2Mass content
Not less than 82%；The specific surface area of the Alusil is 300-550m2/ g, pore volume 0.6-1.0mL/g, compression strength are not less than
50N。
Preferably, the pore volume of the Alusil is 0.7-0.9mL/g, pore size 6-10nm.
A kind of preparation method of Alusil of the present invention, comprises the following steps：1) aluminium salt and raw material acid are taken, mixes, adds water,
The acid solution of aluminium salt is made, makes the mass concentration of aluminium salt for 1-20%, the mass concentration of raw material acid is 5-45%；Take sodium silicate,
Water is added in, the sodium silicate solution that mass concentration is 5-25% is made；2) sodium silicate solution obtained by step 1) is added to step
1) in the acid solution obtained by, the volume ratio of sodium silicate solution and acid solution is 15-18:5-7, progress colloidal sol coagulates at 15-45 DEG C
Glue reacts, reaction pressure 0.05-1.5MPa, and the pH value after reaction is 2.5-8.5, obtains gel；It 3) will be solidifying obtained by step 1)
Glue, aging exchange acid treatment, washing, and ammonia treatment dries, obtains Alusil.
Specifically he, the balling-up of the gel obtained by the step 1) distance is 1-3m, and is received in the receiver into row buffering
The pH value of water is 6.0-9.0 in device, and the temperature of water is 20-40 DEG C in receiver.
Further, in the step 2), during ammonia treatment, ammonia used is ammonium hydroxide, ammonium chloride, ammonium sulfate, ammonium carbonate or
Any one or a few in ammonium hydrogen carbonate, concentration for the treatment of 0.05-1.5%, treatment temperature are 20-90 DEG C, and processing time is
1-12h；More preferably：Ammonia used is ammonium hydroxide, and concentration for the treatment of 0.1-1%, treatment temperature is 40-80 DEG C, and processing time is
4-8h。
Preferably, the mass concentration of the sodium silicate is 10-20%, and the mass concentration of aluminium salt is 5-15%, raw material acid
Mass concentration is 10-30%, and the pH value of reaction is 3.5-7.5.
Yet further, in the step 2), during aging, temperature is 25-85 DEG C, time 0.5-50h；More preferably：
Temperature is 30-60 DEG C, time 2-35h.
Again less preferably, in the step 2), when exchanging acid treatment, exchanged acid is hydrochloric acid, sulfuric acid, aluminum nitrate, nitric acid, sulphur
Any one or a few in sour aluminium, oxalic acid or citric acid, the mass concentration of exchanged acid is 0.05-10%, treatment temperature 30-
100 DEG C, processing time 1-12h；More preferably：The mixed acid that exchanged acid is sulfuric acid, oxalic acid and aluminum sulfate form, exchanged acid
Mass concentration is 0.1-5%, and treatment temperature is 30-60 DEG C, processing time 2-6h.
More specifically, in the step 2), during washing, temperature is 20-90 DEG C, washes the pH value of terminal as 4.5-7.0, water
Gel specific resistance after washing is not less than 1000 Ω cm；More preferably：Temperature is 30-60 DEG C, washes the pH value 5.0- of terminal
6.5。
Further, in the step 2), during drying, temperature is 80-400 DEG C, time 12-48h；More preferably：
Using stoving process twice, the temperature of drying is 80-200 DEG C, time 10-36h for the first time, and the temperature of second of drying is
200-400 DEG C, time 2-12h.
Embodiment one
A kind of preparation method of Alusil of the present invention, comprises the following steps：
1) aluminium salt and raw material acid are taken, is mixed, is added water, the acid solution of aluminium salt is made, the mass concentration for making aluminium salt is 8%, former
The mass concentration of material acid is 15%；Sodium silicate is taken, adds in water, the sodium silicate solution that mass concentration is 10% is made；
2) sodium silicate solution obtained by step 1) is added in the acid solution obtained by step 1), sodium silicate solution and acid solution
Volume ratio be 15:5, it is placed in reactor, carries out solgel reaction, temperature is 35 DEG C, reaction pressure 0.34Mpa, instead
PH value after answering is 6.5, obtains gel, the balling-up distance of gel is 3m；
3) above-mentioned gained gel is subjected to burin-in process, temperature is 35 DEG C, ageing time 2h；
4) gel after above-mentioned aging is swapped into acid treatment, the mass concentration of exchanged acid is 0.6%, and treatment temperature is
30 DEG C, processing time 3h, wherein, the mixed acid that exchanged acid is sulfuric acid, oxalic acid and aluminum sulfate form；
5) by above-mentioned exchanged acid, treated that gel is washed, and temperature is 40 DEG C, and washing terminal is that pH value is 5.5, water
Wash rear 1200 Ω cm of gel specific resistance；
6) by after above-mentioned washing gel carry out ammonia treatment, all ammonia be ammonium hydroxide, concentration for the treatment of 0.2%, temperature 40
DEG C, processing time 4h；
7) gel after above-mentioned ammonia treatment is subjected to drying and processing twice, first drying temperature is 90 DEG C, and drying time is
12h, secondary drying temperature are 400 DEG C, and drying time 4h obtains Alusil.
By detection, in the Alusil obtained by the present embodiment, Al2O3Mass content be 3.5%, SiO2Mass content
For 91.5%, pore volume 0.65mL/g, specific surface area 510m2/ g, compression strength 106N.
Embodiment two
A kind of preparation method of Alusil of the present invention, comprises the following steps：
1) aluminium salt and sulfuric acid are taken, is mixed, is added water, the acid solution of aluminium salt is made, the mass concentration for making aluminium salt is 12%, sulfuric acid
Mass concentration be 10.5%；Sodium silicate is taken, adds in water, the sodium silicate solution that mass concentration is 14.5% is made；
2) sodium silicate solution obtained by step 1) is added in the acid solution obtained by step 1), sodium silicate solution and acid solution
Volume ratio be 18:7, it is placed in reactor, carries out solgel reaction, temperature is 31 DEG C, reaction pressure 0.36Mpa, instead
PH value after answering is 7.0, and at the end of reaction, the pH value of water is 9.0 in receiver, and the temperature of water is 40 DEG C, obtains gel, gel
Balling-up distance is 1m；
3) above-mentioned gained gel is subjected to burin-in process, temperature is 45 DEG C, ageing time 4h；
4) gel after above-mentioned aging is swapped into acid treatment, the mass concentration of exchanged acid is 2.5%, and treatment temperature is
40 DEG C, processing time 2h, wherein, exchanged acid is aluminum sulfate；
5) by above-mentioned exchanged acid, treated that gel is washed, and temperature is 50 DEG C, and washing terminal is that pH value is 6.0, water
Wash rear 1500 Ω cm of gel specific resistance；
6) by after above-mentioned washing gel carry out ammonia treatment, all ammonia be ammonium hydrogen carbonate, concentration for the treatment of 0.4%, temperature
For 60 DEG C, processing time 5h；
7) gel after above-mentioned ammonia treatment is subjected to drying and processing twice, first drying temperature is 100 DEG C, and drying time is
For 24 hours, secondary drying temperature is 200 DEG C, and drying time 12h obtains Alusil.
By detection, in the Alusil obtained by the present embodiment, Al2O3Mass content be 4.5%, SiO2Mass content
For 89.5%, pore volume 0.76mL/g, specific surface area 488m2/ g, compression strength 84N.
Embodiment three
A kind of preparation method of Alusil of the present invention, comprises the following steps：
1) aluminium salt and sulfuric acid are taken, is mixed, is added water, the acid solution of aluminium salt is made, the mass concentration for making aluminium salt is 13%, sulfuric acid
Mass concentration be 19%；Sodium silicate is taken, adds in water, the sodium silicate solution that mass concentration is 18.5% is made；
2) sodium silicate solution obtained by step 1) is added in the acid solution obtained by step 1), sodium silicate solution and acid solution
Volume ratio be 16:6, it is placed in reactor, carries out solgel reaction, temperature is 28 DEG C, reaction pressure 0.36Mpa, instead
PH value after answering is 3.5, and at the end of reaction, the pH value of water is 6.0 in receiver, and the temperature of water is 20 DEG C, obtains gel, gel
Balling-up distance is 2m；
3) above-mentioned gained gel is subjected to burin-in process, temperature is 35 DEG C, and ageing time is for 24 hours；
4) gel after above-mentioned aging is swapped into acid treatment, the mass concentration of exchanged acid is 1.5%, and treatment temperature is
50 DEG C, processing time 4h, wherein, exchanged acid is oxalic acid；
5) by above-mentioned exchanged acid, treated that gel is washed, and temperature is 60 DEG C, and washing terminal is that pH value is 5.8, water
Wash rear 1000 Ω cm of gel specific resistance；
6) gel after above-mentioned washing is subjected to ammonia treatment, all ammonia are ammonium chloride, and concentration for the treatment of 0.8%, temperature is
40 DEG C, processing time 6h；
7) gel after above-mentioned ammonia treatment is subjected to drying and processing twice, first drying temperature is 120 DEG C, and drying time is
36h, secondary drying temperature are 300 DEG C, and drying time 2h obtains Alusil.
By detection, in the Alusil obtained by the present embodiment, Al2O3Mass content be 4.7%, SiO2Mass content
For 88.5%, pore volume 0.82mL/g, specific surface area 458m2/ g, compression strength 65N.
Compared with prior art, the beneficial effects of the invention are as follows：In the Alusil of the present invention, SiO2Content is high, Al2O3Contain
Measure adjustable, silica alumina ratio adjustable range is wide, skeleton structure and even intensity, large pore volume, large specific surface area, and compression strength is high, skeleton
Structure and pore structure are stablized, and good product quality, big pore volume and specific surface area and high compressive strength are taken into account, can be widely applied to urge
The fields such as agent and catalyst carrier, adsorbing separation and system with molecular sieve for preparing be standby；The preparation process is simple, easy to operate, it is easy to accomplish
Industrialization.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modifications, equivalent replacements and improvements are made should all be included in the protection scope of the present invention god.
Claims (10)
1. a kind of Alusil, it is characterised in that：In the Alusil, Al2O3Mass content be 3-8%, SiO2Mass content
Not less than 82%；
The specific surface area of the Alusil is 300-550m2/ g, pore volume 0.6-1.0mL/g, compression strength are not less than 50N.
2. Alusil according to claim 1, it is characterised in that：
The pore volume of the Alusil is 0.7-0.9mL/g, pore size 6-10nm.
3. the preparation method of Alusil according to claim 1 or 2, it is characterised in that：Comprise the following steps：
1) aluminium salt and raw material acid are taken, is mixed, is added water, the acid solution of aluminium salt is made, makes the mass concentration of aluminium salt for 1-20%, raw material
The mass concentration of acid is 5-45%；Sodium silicate is taken, adds in water, the sodium silicate solution that mass concentration is 5-25% is made；
2) sodium silicate solution obtained by step 1) is added in the acid solution obtained by step 1), sodium silicate solution and acid solution
Volume ratio is 15-18:5-7 carries out solgel reaction, reaction pressure 0.05-1.5MPa, after reaction at 15-45 DEG C
PH value is 2.5-8.5, obtains gel；
3) by the gel obtained by step 1), aging exchanges acid treatment, washing, and ammonia treatment dries, obtains Alusil.
4. the preparation method of Alusil according to claim 3, it is characterised in that：
The balling-up distance of gel obtained by the step 1) is 1-3m, in the receiver into row buffering after reaction, water in receiver
PH value for 6.0-9.0, the temperature of water is 20-40 DEG C in receiver.
5. the preparation method of Alusil according to claim 3, it is characterised in that：
In the step 2), during ammonia treatment, ammonia used is appointing in ammonium hydroxide, ammonium chloride, ammonium sulfate, ammonium carbonate or ammonium hydrogen carbonate
Meaning is one or more of, concentration for the treatment of 0.05-1.5%, and treatment temperature is 20-90 DEG C, processing time 1-12h；
Preferably：Ammonia used is ammonium hydroxide, and concentration for the treatment of 0.1-1%, treatment temperature is 40-80 DEG C, processing time 4-8h.
6. the preparation method of Alusil according to claim 3, it is characterised in that：
In the step 1), the mass concentration of sodium silicate is 10-20%, and the mass concentration of aluminium salt is 5-15%, the matter of raw material acid
Amount concentration is 10-30%, and the pH value after reaction is 3.5-7.5.
7. the preparation method of Alusil according to claim 3, it is characterised in that：
In the step 2), during aging, temperature is 25-85 DEG C, time 0.5-50h；Preferably：Temperature is 30-60 DEG C, the time
For 2-35h.
8. the preparation method of Alusil according to claim 3, it is characterised in that：
In the step 2), when exchanging acid treatment, exchanged acid is hydrochloric acid, sulfuric acid, aluminum nitrate, nitric acid, aluminum sulfate, oxalic acid or lemon
Any one or a few in acid, the mass concentration of exchanged acid is 0.05-10%, and treatment temperature is 30-100 DEG C, processing time
For 1-12h；
Preferably：The mixed acid that exchanged acid is sulfuric acid, oxalic acid and aluminum sulfate form, the mass concentration of exchanged acid is 0.1-5%, is located
It is 30-60 DEG C to manage temperature, processing time 2-6h.
9. the preparation method of Alusil according to claim 3, it is characterised in that：
In the step 2), during washing, temperature is 20-90 DEG C, washes the pH value of terminal as 4.5-7.0, the gel ratio after washing
Resistance is not less than 1000 Ω cm；
Preferably：Temperature is 30-60 DEG C, washes the pH value 5.0-6.5 of terminal.
10. the preparation method of Alusil according to claim 3, it is characterised in that：
In the step 2), during drying, temperature is 80-400 DEG C, time 12-48h；
Preferably：Using stoving process twice, the temperature of drying is 80-200 DEG C, time 10-36h for the first time, second of baking
Dry temperature is 200-400 DEG C, time 2-12h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711421111.XA CN108046280B (en) | 2017-12-25 | 2017-12-25 | Silica-alumina gel and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711421111.XA CN108046280B (en) | 2017-12-25 | 2017-12-25 | Silica-alumina gel and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108046280A true CN108046280A (en) | 2018-05-18 |
| CN108046280B CN108046280B (en) | 2020-11-27 |
Family
ID=62131702
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711421111.XA Active CN108046280B (en) | 2017-12-25 | 2017-12-25 | Silica-alumina gel and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108046280B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5011667A (en) * | 1988-09-08 | 1991-04-30 | Engelhard Corporation | Self-bound sodium chabazite aggregates and methods for preparation thereof |
| CN1206020A (en) * | 1997-07-21 | 1999-01-27 | 青岛海洋化工集团公司 | Guanulated gelatinized silica-alumina product and its production process |
| CN105819884A (en) * | 2016-03-10 | 2016-08-03 | 青岛海洋化工有限公司 | Waterproof alumina-silica gel particle product and production method thereof |
| CN106140286A (en) * | 2015-03-27 | 2016-11-23 | 中国石油化工股份有限公司 | The preparation method of carrier of hydrocracking catalyst |
-
2017
- 2017-12-25 CN CN201711421111.XA patent/CN108046280B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5011667A (en) * | 1988-09-08 | 1991-04-30 | Engelhard Corporation | Self-bound sodium chabazite aggregates and methods for preparation thereof |
| CN1206020A (en) * | 1997-07-21 | 1999-01-27 | 青岛海洋化工集团公司 | Guanulated gelatinized silica-alumina product and its production process |
| CN106140286A (en) * | 2015-03-27 | 2016-11-23 | 中国石油化工股份有限公司 | The preparation method of carrier of hydrocracking catalyst |
| CN105819884A (en) * | 2016-03-10 | 2016-08-03 | 青岛海洋化工有限公司 | Waterproof alumina-silica gel particle product and production method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 天津化工研究院等，: "《无机盐工业手册（第二版）下册》", 31 January 2000 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108046280B (en) | 2020-11-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105819457A (en) | Preparation method and applications of silica aerogel | |
| CN107640777A (en) | A kind of method for preparing big/mesoporous zeolite molecular sieve of crystal seed induction | |
| CN103172082B (en) | Preparation method of mesoporous-containing Y-shaped molecular sieve | |
| CN101053819B (en) | Method for producing variable-pressure adsorption silica gel | |
| CN104445261A (en) | Preparation method of microporous/mesoporous composite ZSM-5 molecular sieve | |
| CN109775716A (en) | A kind of multi-stage porous Y type molecular sieve and preparation method thereof rich in L acid | |
| CN103771429A (en) | Method using co-template agent to synthesizing porous spherical silica | |
| CN115594193B (en) | High-hydrophobicity mesoporous Y-type molecular sieve and preparation method thereof | |
| CN104016369B (en) | A kind of method utilizing kaolin synthesizing high-stability ordered mesoporous material Al-SBA-15 | |
| CN104211080A (en) | Preparation method for Fe isomorphously substituted ZSM-22 molecular sieve | |
| CN102464326B (en) | Method for synthesizing high-silicon mordenite | |
| CN108046280A (en) | A kind of Alusil and preparation method thereof | |
| CN106477591B (en) | A kind of preparation method of PE dividing plates silica | |
| CN108439427A (en) | A kind of method that fabricated in situ is rich in mesoporous NaY molecular sieve | |
| CN102786064B (en) | Hydrocracking catalyst carrier and preparation method thereof | |
| CN107840349A (en) | The preparation method of the nanometer multi-stage porous aggregations of ZSM 5 | |
| CN105712374A (en) | Preparation method of hollow USY molecular sieve | |
| CN101760242A (en) | Continuous stripping process and device for chlorinated paraffin | |
| CN106608642B (en) | A kind of mesopore molecular sieve and preparation method thereof | |
| CN106927477B (en) | A kind of preparation method of mesoporous Y type molecular sieve | |
| CN103318912B (en) | Preparation method of sodium alginate-xanthan gum modified nano A zeolite assembly | |
| CN112808296A (en) | Catalyst containing Y-type molecular sieve and preparation method thereof | |
| CN106345513B (en) | A kind of mesoporous Si-Al material and its preparation method and application | |
| CN110203937A (en) | A kind of synthetic method of the orderly super-microporous silicon dioxide of cubic phase | |
| CN106927480A (en) | A kind of method of modifying of Y type molecular sieve |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |