CN106629795B - A kind of preparation method of high single water diaspore - Google Patents
A kind of preparation method of high single water diaspore Download PDFInfo
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- CN106629795B CN106629795B CN201610891887.7A CN201610891887A CN106629795B CN 106629795 B CN106629795 B CN 106629795B CN 201610891887 A CN201610891887 A CN 201610891887A CN 106629795 B CN106629795 B CN 106629795B
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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
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
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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 proposes a kind of preparation method of high single water diaspore, preparation step are as follows: (1) refines, (2) aquation, (3) divide alcohol, and alcohol is steamed in (4) aging, and (5) are dry, and high single water diaspore is made.The advantages that water diaspore product that the present invention makes has impurity content low, pore distribution concentration, and product is stablized.Preparation process environmental protection, three-waste free discharge, obtained product can be applied to reforming catalyst and catalyst carrier for hydrgenating.
Description
Technical field
The invention belongs to catalyst material field, specially a kind of preparation method of high single water diaspore.
Background technique
One water diaspore, also referred to as false boehmite are that a kind of particle is tiny, crystallization is imperfect, with thin fold piece
A kind of aluminium hydroxide of layer is thixotropy gel containing aquosity, has the characteristics that specific surface height, Kong Rong great.It can be used as production to urge
The raw material of agent carrier, activated alumina also serves as the molding adhesive and alcohol of molecular sieve, silicate refractory material product etc.
It is dehydrated ethylene and the catalyst of ethylene oxide processed etc..Product γ-the Al roasted between 400-700 DEG C2O3It is widely used as catalyst load
Body, catalyst and adsorbent etc.；Calcining can obtain nanoscale γ-Al between 1100-1200 DEG C2O3, be widely used as coating additive,
High-grade ceramic, the effective catalyst of petrochemical industry, submicron/nanometer grade grinding-material and polishing material, cosmetics filler and nothing
Machine membrane material etc..
The method of one water diaspore of domestic production at present is mainly carbonizatin method and the precipitation method and aluminium alcoholates method, using carbonizatin method and
The product impurity of the precipitation method existing water diaspore production technology production is higher, can several apertures are inhomogenous, crystal phase purity is low, produce
Product are unstable.It is all to need to be added catalyst progress using low-carbon alcohols such as isopropanol at present when preparing diaspore using aluminium alcoholates method
Reaction, causes equipment to corrode, and causes filtration drying difficult, and there are safety problems for low-carbon alcohols, and recycling is difficult, increased costs, therefore
For catalytic reforming and add the single water diaspore of height of hydrogen always from external import, comes out always without production domesticization product.
Summary of the invention
The invention aims to overcome the deficiencies in the prior art, and high-purity alcohol can be obtained with distillation purifying using low-carbon aluminium alcoholates
Aluminium, higher alcohols and low-carbon aluminium alcoholates can carry out displacement reaction, and the higher alcohols recycling obtained after higher alcohols aluminum water solution is easy, and prepare
A kind of impurity content is low, pore distribution concentration, single crystal phase material.
In order to solve the above technical problems, a kind of high single water diaspore of the present invention, is prepared using following steps:
(1) aluminium alcoholates is prepared,
(2) hydration reaction,
(3) divide alcohol,
(4) alcohol is steamed in aging,
(5) it filters, is dried to obtain high single water diaspore.
Step (1) is that four-hole boiling flask is added in low-carbon aluminium alcoholates and higher alcohols, is heated to reflux after a certain period of time, and alcohol is steamed in decompression,
When flowing out to water segregator there is no liquid, reaction is completed, and obtains high-carbon aluminium alcoholates.Wherein, higher alcohols can be in C5-C10 alcohol
One or more, low-carbon aluminium alcoholates are any one of C2-C4；The molar ratio of higher alcohols and low-carbon aluminium alcoholates is 1-5: 1.Higher alcohols with
Low-carbon alcohols reactive aluminum temperature is at 70-140 DEG C；Reaction time 2-7h, decompression steam low-carbon alcohols, depressurize 50-80 DEG C of temperature, obtain height
Carbon aluminium alcoholates.
Step (2) is that deionized water and aluminum sulfate, the molar ratio of aluminum sulfate additional amount and deionized water are added in flask
It is 0.001-0.003: 1, after being warming up to 80 degree, starts that high-carbon aluminium alcoholates, deionized water and aluminium alcoholates are added dropwise into deionized water solution
Molar ratio be 3-10: 1, while be added dropwise while stir.The temperature of hydration reaction is 60-100 DEG C, reaction time 20-120min；Water
Solution reaction generates hydroxyl diaspore.
Step (3) is that the alcohol for generating hydration reaction is extracted out, reusable after processing.
Step (4) is that deionized water is added again in flask, carries out aging, the deionization of addition to hydroxyl diaspore
Water and the molar ratio of hydroxyl diaspore are 40-300: 1, and the temperature of aging is 60-100 DEG C, time 30-900min, aging
Distillation separates remaining alcohol simultaneously.
Step (5) is that nonionic surfactant solution is added to be filtered the substance of aging, the surface-active of addition
The molar ratio of dosage and diaspore is 0.0001-0.001: 1, and strainer mesh number 300-500, filter cake is obtained in 120 DEG C of crushed after being dried
To high single water diaspore.Filtered water can be recycled after treatment.
The advantage of the invention is that not avoiding the corrosion and final production of flask using catalyst such as mercury salt and aluminium chloride
The filtration difficulty of object, low-carbon aluminium alcoholates can be widely available, high-purity can be obtained by the methods of distillation, higher alcohols have insoluble
In the water the advantages of, post-processing is simple, preparation process environmental protection, three-waste free discharge.One water diaspore product of production contains with impurity
Measure low, the advantages that pore distribution concentration, crystal phase is single, and product is stablized；Obtained product can be widely applied to reforming catalyst and add
Hydrogen catalyst carrier.
Specific embodiment
Embodiments of the present invention are further described below with reference to embodiment.
Embodiment 1:
Four-hole boiling flask is added in 20.4 grams of aluminium isopropoxides, 30.6 grams of n-hexyl alcohols, is heated to reflux 4h, alcohol is steamed in decompression.To dividing water
When device is flowed out there is no liquid, reaction is completed, and obtains n-hexyl alcohol aluminium.18mL deionized water is added in the four-hole boiling flask with stirring
With 0.4g aluminum sulfate, after being warming up to 80 degree, start to stir, while n-hexyl alcohol aluminium, reaction time being added dropwise into deionized water solution
For 30min；The n-hexyl alcohol for extracting hydrolysis out, obtains hydroxyl diaspore.100mL deionized water and 0.07g are added in flask
OP-10 is warming up to 85 DEG C, and aging is filtered after 12 hours.Filter cake obtains high single water diaspore in 120 DEG C of crushed after being dried.
Embodiment 2:
Four-hole boiling flask is added in 20.4 grams of aluminium isopropoxides, 40 grams of n-octyl alcohols, is heated to reflux 4h, alcohol is steamed in decompression.To water segregator
There is no when liquid outflow, reaction is completed, and n-octyl alcohol aluminium is obtained.With stirring four-hole boiling flask in be added 18mL deionized water and
0.4g aluminum sulfate after being warming up to 80 degree, starts to stir, while the dropwise addition n-octyl alcohol aluminium into deionized water solution, reaction time are
30min；It extracts hydrolysis n-octyl alcohol out, obtains hydroxyl diaspore.The heating of 100mL deionized water and 0.07g are added in flask
TX-10, until 85 DEG C, aging is filtered after 12 hours.Filter cake obtains high single water diaspore in 120 DEG C of crushed after being dried.
Embodiment 3:
Four-hole boiling flask is added in 20.4 grams of aluminium isopropoxides, 40 grams of isooctanol, is heated to reflux 4h, alcohol is steamed in decompression.To water segregator
There is no when liquid outflow, reaction is completed, and isooctanol aluminium is obtained.With stirring four-hole boiling flask in be added 18mL deionized water and
0.4g aluminum sulfate after being warming up to 80 degree, starts to stir, while the dropwise addition n-hexyl alcohol aluminium into deionized water solution, reaction time are
30min；It extracts hydrolysis isooctanol out, obtains hydroxyl diaspore.100mL deionized water and 0.03g AEO9 are added in flask,
85 DEG C are warming up to, aging is filtered after 12 hours.Filter cake obtains high single water diaspore in 120 DEG C of crushed after being dried.
Embodiment 4:
Four-hole boiling flask is added in 25 grams of Tributyl aluminates, 30.6 grams of n-hexyl alcohols, is heated to reflux 4h, alcohol is steamed in decompression.To water segregator
There is no when liquid outflow, reaction is completed, and n-hexyl alcohol aluminium alcoholates is obtained.18mL deionized water is added in the four-hole boiling flask with stirring
With 0.4g aluminum sulfate, after being warming up to 80 degree, start to stir, while n-hexyl alcohol aluminium, reaction time being added dropwise into deionized water solution
For 30min；It extracts hydrolysis n-hexyl alcohol out, obtains hydroxyl diaspore.200mL deionized water and 0.007g OP- are added in flask
10,85 DEG C are warming up to, aging is filtered after 12 hours.Filter cake obtains high single water diaspore in 120 DEG C of crushed after being dried.
Embodiment 5:
Four-hole boiling flask is added in 25 grams of Tributyl aluminates, 48 grams of Decanols, is heated to reflux 4h, alcohol is steamed in decompression.Not to water segregator
When having liquid outflow again, reaction is completed, and obtains Decanol aluminium.With stirring four-hole boiling flask in be added 18mL deionized water and
0.4g aluminum sulfate after being warming up to 80 degree, starts to stir, while the dropwise addition n-hexyl alcohol aluminium into deionized water solution, reaction time are
30min；It extracts hydrolysis Decanol out, obtains hydroxyl diaspore.100mL deionized water and 0.005g OP- are added in flask
10,85 DEG C are warming up to, aging is filtered after 12 hours.Filter cake obtains high single water diaspore in 120 DEG C of crushed after being dried.
Embodiment 6:
Four-hole boiling flask is added in 20.4 grams of aluminium isopropoxides, 30.6 grams of n-hexyl alcohols, is heated to reflux 4h, alcohol is steamed in decompression.To dividing water
When device is flowed out there is no liquid, reaction is completed, and obtains n-hexyl alcohol aluminium alcoholates.18mL deionization is added in the four-hole boiling flask with stirring
Water and 0.4g aluminum sulfate after being warming up to 80 degree, start to stir, while n-hexyl alcohol aluminium being added dropwise into deionized water solution, when reaction
Between be 30min；It extracts hydrolysis n-hexyl alcohol out, obtains hydroxyl diaspore.150mL deionized water and 0.008g are added in flask
AEO7 is warming up to 85 DEG C, and aging is filtered after 12 hours.Filter cake obtains high single water diaspore in 120 DEG C of crushed after being dried.It is high
Single water diaspore impurity content and pore structure data are referring to table 1.
Table 1
Claims (5)
1. a kind of high single water diaspore preparation method, which is characterized in that preparation step are as follows:
(1) refine, (2) aquation, (3) divide alcohol, and alcohol is steamed in (4) aging, and (5) filtering is dry, and high single water diaspore is made；Wherein
Step (1) alcoholization is the realization that flowed back in reaction flask by low-carbon aluminium alcoholates and higher alcohols；The low-carbon aluminium alcoholates is in C2-C4
One kind, higher alcohols are one or more of C5-C10 alcohol；The molar ratio of higher alcohols and low-carbon aluminium alcoholates is 1-5: 1；Higher alcohols
With low-carbon alcohols reactive aluminum temperature at 70-140 DEG C；Decompression is carried out under reaction time 2-8h, 10~100mmHg and steams low-carbon alcohols, is steamed
50-80 DEG C of temperature is evaporated, high-carbon aluminium alcoholates is obtained；Step (2) are as follows: deionized water and aluminum sulfate are added in flask, aluminum sulfate is added
The molar ratio of amount and deionized water is 0.001-0.003: 1；The additional amount of deionized water and the molar ratio of aluminium alcoholates are 1-3: 1, are risen
Temperature to after 80 degree starts that aluminium alcoholates is added dropwise into deionized water solution, stirs when being added dropwise；The temperature of hydration reaction is 60-100
DEG C, reaction time 20-120min；Hydration reaction generates hydroxyl diaspore；Step (4) are as follows: in flask again be added go from
Sub- water carries out aging to hydroxyl diaspore, and the amount of deionized water of addition and the molar ratio of diaspore are 40-300: 1, the temperature of aging
Degree is 60-100 DEG C, time 30-900min, and aging is distilled simultaneously separates remaining alcohol.
2. preparation method according to claim 1, which is characterized in that higher alcohols water content < 0.2%.
3. preparation method according to claim 1, which is characterized in that step (3) are as follows: the alcohol for generating hydration reaction is taken out
Out.
4. preparation method according to claim 1, which is characterized in that step (5) are as follows: it is living that surface is added in substance after toward aging
Property agent solution, the amount of surfactant of addition and the molar ratio of diaspore are 0.0001-0.001: 1, to the object of aging after stirring
Matter is filtered, and filter cake obtains high single water diaspore in 120 DEG C of crushed after being dried.
5. the preparation method according to claim 4, which is characterized in that the surfactant is nonionic surfactant
OP-10, AEO7, AEO9, TX-10.
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