CN107848825A - The method for preparing the boehmite with specific crystallite - Google Patents
The method for preparing the boehmite with specific crystallite Download PDFInfo
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- CN107848825A CN107848825A CN201680032784.3A CN201680032784A CN107848825A CN 107848825 A CN107848825 A CN 107848825A CN 201680032784 A CN201680032784 A CN 201680032784A CN 107848825 A CN107848825 A CN 107848825A
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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
- C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/60—Compounds characterised by their crystallite size
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The present invention describes the method that alumina gel is prepared in single settling step, the settling step is included in water dissolved acid aluminum precursor in a manner of causing the pH of solution to be 0.5 to 5 at a temperature of 10 DEG C to 90 DEG C through the time of 2 to 60 minutes --- aluminium chloride, then at a temperature of 5 DEG C to 35 DEG C through the time of 5 minutes to 5 hours by adding alkaline precursor into the solution obtained --- sodium hydroxide, pH is adjusted into the pH in the range of to 7.5 to 9.5, to obtain suspension.
Description
Invention field
The present invention relates to the preparation of alumina gel or boehmite gel.Especially, the present invention relates to have by precipitation
The novel processing step of the alumina gel of small size crystallite.Obtain very small dimensions boehmite particle cause produce be different from compared with
The surface reaction of large scale particle（The exposure of different proportion and improved reactivity）.This will cause in dipping process not
Same activity phase is corresponding to the interaction of microporous surface and during being catalyzed such as such as hydrotreating or catalytic reforming
The improved reactivity of catalyst.
Especially, preparation in accordance with the present invention can be used for obtaining the alumina gel being made up of crystallite or boehmite coagulates
Glue, the crystallite have respectively 0.5 to 10 nm and 0.5 to 15 nm and preferably be respectively 0.5 to 2 nm and 0.5 to 3 nm and
Highly preferred is respectively 0.5 to 1.5 and 0.5 to 2.5 to pass through in crystal face [020] and [120] in X-ray diffraction
The size that Scherrer formula obtain.
Prior art
It is known in the art that many operation schemes are used to produce alumina gel.Especially, several patents describe
" sol-gel " preparation method.
Patent US 4 676 928 describes the method for producing the aluminum oxide that can be dispersed in water, including forms oxygen
The step of changing the water-borne dispersions of aluminium, add the step of acid is to produce the acid dispersion of the pH with 5 to 9, more than 70 DEG C
At a high temperature of curing one section be enough to make aluminum oxide be transformed into colloidal gel time the step of, be followed by dry acquisition the glue
The step of state gel.
The method that alumina gel is prepared by co-precipitation is also known in the prior art.
Thus, patent US 6 589 908 is described for example is used in temperature, pH and the flow bar fully controlled at two
The method that aluminum oxide is prepared in the step of aluminum precursor is precipitated under part.First step at a temperature of 25 DEG C to 60 DEG C, 3 to 10
Operated under pH and preferably under 3 to 4.5 and 7.5 to 10 pH.
The precursor is selected from aluminum nitrate, aluminium chloride combination sodium aluminate or sodium hydroxide combination acid aluminium salt.Precursor it is preferred
Combination is aluminum sulfate and sodium aluminate.Suspension is then heated to 50 DEG C to 90 DEG C of temperature.It is new that some are added into suspension
Fresh reagent, then washed, dried, be molded and calcined to form catalyst carrier.This method can be used for being aoxidized
Aluminium, the aluminum oxide be characterised by without macropore, being made up of less than 5% diameter more than 35 nm hole of total pore size volume,
High pore volume and the nm of two of which mode spacing 1 to 20 and main hole pattern more than 0.8 ml/g are more than average hole
The bimodal pore distribution in footpath.And undeclared crystallite dimension.
In addition, patent application WO2004/052534 A1, which are described, prepares urging comprising the carrier prepared by following steps
The method of agent：Co-precipitation（The co-precipitation of preferably sulfuric acid aluminium and sodium aluminate）, then by the gel drying obtained, extrude and forge
Burn.Silica can be added during or after co-precipitation.
More properly, the method for preparing alumina gel is this document describe, wherein in presence of water by sodium aluminate, hydrogen
The alkaline solution of sodium oxide molybdena or aluminium hydroxide is added in reactor.The acid solution of aluminum sulfate or aluminum nitrate is added simultaneously.It is excellent
Selection of land, at the end of acid adds, the pH of the reaction medium is 7 to 9, and temperature is maintained at 60-75 DEG C in mixed process,
Continue the time of 30 minutes to 30 minutes 1 hour.Mixing, extrusion, air drying then are imposed to the mixture（200℃）With
The step of heat treatment.Adjustment shaping makes it possible to obtain the characteristic of the carrier.
This method can be used for obtaining the alumina gel with specific pore distribution, but not refer to the size of crystallite.
It is also well known in the prior art to prepare alumina gel by precipitation.
Specifically, patent US 7 790 652 describes prepares the oxygen with very special distribution of pores by precipitating
Change alumina supporter, it can be used as the carrier of catalyst in the hydroconversion process of heavy hydrocarbon charge.
Using including forming aluminum oxide by mixing the first alkaline aqueous solution and the first acidic aqueous solution in a controlled manner
Dispersion first step method, alumina support is prepared in two settling steps, the acid solution and alkalescence are molten
At least one of liquid or its both include aluminium compound.Acid solution and alkaline solution are to cause dispersions obtained pH as 8
Ratio to 11 mixes.Acid solution and alkaline solution are also to cause the amount for producing the dispersion containing the desired amount of aluminum oxide to mix
Close；Especially, first step can be used for obtaining 25 based on the total amount of the aluminum oxide formed at the end of two settling steps
Weight % to 35 weight % aluminum oxide.First step operates at a temperature of 20 DEG C to 40 DEG C.When having formed the desired amount of oxidation
During aluminium, the temperature of suspension is brought up to 45 DEG C to 70 DEG C of temperature, then, then by making the suspension and the second alkalescence
The aqueous solution and the second acidic aqueous solution, which contact, imposes the second settling step to heated suspension, in described two solution extremely
Few one or its both include aluminium compound.Similarly, the ratio for passing through added acid solution and alkaline solution adjusts pH
Save to 8 to 10.5, and the surplus for the aluminum oxide to be formed in the second step is molten by the acid solution and alkalescence added
The amount supply of liquid.Second step operates at a temperature of 20 DEG C to 40 DEG C.The alumina gel being consequently formed includes at least 95%
Boehmite.Then in the case of not advance maturation stage, using method known to those skilled in the art by aluminum oxide
Gel filtration, washing and optionally drying, then will using method known to those skilled in the art to produce alumina powder
The alumina powder shaping, is then calcined to produce final alumina support.
The applicant makes it has now been found that in the case of not follow-up co-precipitation step in single settling step
The method of standby alumina gel generates the alumina gel with small crystallite, and it is specific that the single settling step includes dissolving
Acid aluminum precursor --- aluminium chloride, then adjust pH using specific alkaline precursor --- sodium hydroxide ---.
Especially, preparation in accordance with the present invention can be used for obtaining the alumina gel being made up of crystallite or boehmite coagulates
Glue, the size that the crystallite is obtained in X-ray diffraction in crystal face [020] and [120] by Scherrer formula are respectively
0.5 to 10 nm and 0.5 to 15 nm and preferably be respectively 0.5 to 2 nm and 0.5 to 3 nm and it is highly preferred be respectively 0.5 to
1.5 and 0.5 to 2.5.
X-ray diffraction on alumina gel and boehmite gel is carried out using conventional powders method and diffractometer.
Scherrer formula are the formula used in the X-ray diffraction on powder or Polycrystalline, and it is by diffraction maximum
Halfwidth is associated with crystallite dimension.It is described in detail in below with reference in document：Appl. Cryst. (1978). 11,
102-113, Scherrer after sixty years: A survey and some new results in the
Determination of crystallite size, J. I. Langford and A. J. C. Wilson.
Summary of the invention and invention advantage
The present invention relates to the method that alumina gel is prepared in single settling step, the settling step is included in water 10
DEG C to before dissolving acidic aluminum through the time of 2 to 60 minutes in a manner of causing the pH of solution to be 0.5 to 5 at a temperature of 90 DEG C
Body --- aluminium chloride, then pass through at a temperature of 5 DEG C to 35 DEG C through the time of 5 minutes to 5 hours into the solution obtained
Add alkaline precursor --- sodium hydroxide, pH is adjusted into the pH in the range of to 7.5 to 9.5, to obtain suspension.
Have it is one advantage of the present invention that providing and can be used for obtaining compared with the alumina gel prepared according to prior art
There is the preparation method of the alumina gel of the crystallite dimension of reduction, the alumina gel especially has the crystallite of small size.
Especially, an advantage of the invention that providing a kind of preparation method, it can be used for obtaining what is be made up of crystallite
Alumina gel or boehmite gel, the crystallite pass through Scherrer in X-ray diffraction in crystal face [020] and [120]
Formula obtain size be respectively 0.5 to 10 nm and 0.5 to 15 nm and preferably be respectively 0.5 to 2 nm and 0.5 to 3 nm and
Highly preferred is respectively 0.5 to 1.5 and 0.5 to 2.5.
Further advantage is that provide prepare with reduce crystallite dimension alumina gel method, its with
Prepare the conventional prior method of aluminum oxide（Such as Sol-gel type preparation method）Compared to being simplified and cost is relatively low, and
And it is that the method according to the invention only includes single settling step.
Invention description
According to the present invention, single settling step is included according to the method for preparing alumina gel of the present invention.
The settling step be included in water at 10 DEG C to 90 DEG C, preferably 10 DEG C to 80 DEG C, more preferably 10 DEG C to 75 DEG C and
Specific acid aluminum precursor --- aluminium chloride AlCl is even more preferably dissolved at a temperature of 15 DEG C to 70 DEG C3.The solution obtained
PH is 0.5 to 5, preferably 1 to 4, more preferably 1.5 to 3.5.The solution is stirred 2 to 60 minutes, preferably 5 to 30 minutes and more excellent
Select the time of 5 to 10 minutes.
Then it is small through 5 minutes to 5 at a temperature of 5 DEG C to 35 DEG C, preferably 10 DEG C to 30 DEG C and more preferably 10 DEG C to 25 DEG C
When, preferably 10 minutes to 5 hours, the time of more preferably 15 minutes to 2 hours, pass through specific alkaline precursor --- the hydrogen-oxygen of addition
Change sodium NaOH, by the pH regulations of the suspension obtained to the pH for being referred to as precipitation terminal pH, it is 7.5 to 9.5, preferably 7.5 to 9
More preferably 7.7 to 8.8.
Addition NaOH means can be with precipitating boehmite, and can obtain suspension.
Preferably, carried out in the case of being deposited in the absence of organic additive.
Preferably, the precipitation of alumina gel is carried out under agitation.
Preferably, the method according to the invention include for precipitate supplement step, and include be used for by
In aqueous reaction medium with least one alkaline precursor and at least one acidic precursor（In the alkaline precursor or acidic precursor
At least one includes aluminium）The subsequent step for contacting to be co-precipitated.
The selection of the specific precursor associated with selected temperature and pH conditions means to obtain and according to prior art
The alumina gel of preparation compares the alumina gel with the crystallite dimension reduced, and the aluminum oxide being particularly made up of crystallite coagulates
Glue or boehmite gel, the crystallite are obtained in X-ray diffraction in crystal face [020] and [120] by Scherrer formula
Size be respectively 0.5 to 10 nm and 0.5 to 15 nm and be preferably respectively 0.5 to 2 nm and 0.5 to 3 nm and highly preferred
Respectively 0.5 to 1.5 and 0.5 to 2.5.
Preferably, obtained at the end of also including filtering settling step according to the method for preparing alumina gel of the present invention
The step of suspension.
The filtration step is carried out using method known to those skilled in the art.
The filtration step is advantageously followed by least one using the aqueous solution（It is preferred that water）The washing step of progress, preferably one
Individual to three washing steps, the amount of sediment of the water with filtering are equal.
Obtained at the end of settling step, the subsequent optional step for being used to filter and at least one optional washing step
Alumina gel then advantageously for dry obtained from settling step suspension（It has optionally been filtered）The step of in
Dry to obtain powder, the drying steps at 120 DEG C or higher of temperature advantageous by drying or pass through spray drying
Or carried out by any other dry technology well known by persons skilled in the art.
It is described dry in the case of carrying out the drying steps by being dried at 120 DEG C or higher of temperature wherein
Dry step can be carried out advantageously in the baking oven closed and divulged information.Preferably, the drying steps are at 120 DEG C to 300 DEG C
At a temperature of, more preferably operated at a temperature of 150 DEG C to 250 DEG C.
In the case of carrying out the drying steps by being spray-dried wherein, make in the second settling step and then
The filter cake obtained at the end of filtration step turns into suspension again.The suspension is then according to original well known to those skilled in the art
Reason is ejected into the vertical cylindrical vessel contacted with stream of hot air in the form of fine drop with evaporation water.The powder obtained
It is entrained to by hot-fluid in cyclone separator, bag filter separates air with powder there.
Preferably, in the case of carrying out the drying steps by being spray-dried wherein, according to Asep Bayu
Dani Nandiyanto and Kikuo Okuyama publication, Advanced Powder Technology, 22,1-19,
Operation scheme described in 2011 carries out the spray drying.
The powder obtained at the end of drying steps then can be advantageously molded to obtain raw material.
Term " raw material " refers to the moulding material for not being subjected to any heat treatment step also.
Preferably, the forming step can be extruded, by being granulated, being molded by oil droplet by mixing（oil drop）Skill
Art passes through pill（pastillage）Come carry out.
Highly preferable, the forming step extrudes progress by mixing.
The shaping raw material obtained then can be optionally subjected to presence or absence of containing at most 60 volume % water
In the case of air stream, at a temperature of 500 DEG C to 1000 DEG C, walked through being advantageously the heat treatment of time of 2 to 10 hours
Suddenly.
Preferably, the heat treatment is carried out in the presence of air contained water logistics.
Preferably, the heat treatment step operates at a temperature of 540 DEG C to 850 DEG C.
Preferably, the heat treatment step operates the time of 2 hours to 10 hours.
The heat treatment step can be used for making boehmite be transformed into final aluminum oxide.
Can be optionally using any technology well known by persons skilled in the art at 50 DEG C to 120 before heat treatment step
It is dried at a temperature of DEG C.
The method according to the invention can be used for obtain optionally be in powder type alumina gel, its with according to prior art
The alumina gel of preparation is compared with the crystallite dimension reduced.
Especially, the alumina gel or boehmite gel obtained in powder form according to the present invention is made up of crystallite, institute
State the size that crystallite is obtained in X-ray diffraction in crystal face [020] and [120] by Scherrer formula be respectively 0.5 to
10 nm and 0.5 to 15 nm and preferably be respectively 0.5 to 2 nm and 0.5 to 3 nm and it is highly preferred be respectively 0.5 to 1.5 and
0.5 to 2.5.
The invention also relates to the alumina gel obtained by the preparation method of the present invention.
The present invention will be illustrated by the following examples now, the embodiment equal not structure under any circumstance in itself
Into limitation.
Embodiment：
Embodiment 1（Comparative example）：
Commercial alumina gel powder Pural SB3 are prepared by the hydrolysis-condensation of aluminium-alcohol salt using sol-gel route.
The size of obtained boehmite crystallite is measured using Scherrer methods：The size that use [020] measures=
3.1 ± 0.2 (nm)；Size=4.7 ± 0.3 (nm) for using [120] to measure.
Embodiment 2（Comparative example）：
Alumina gel is produced according to the preparation method of non-invention, is not the solidifying of embodiment 2 according to aspects of the present invention
The preparation method of glue is in two settling steps using the precursor of non-invention in 7 liters of reactors and with 5 liters of final suspension
Liquid is carried out.
The water being added in reactor is 3868 milliliters.
The final alumina concentration of target is 30 g/l.
For aluminum sulfate Al2(SO4)3With the first step of sodium aluminate NaAlOO co-precipitation at 30 DEG C and 9.3 pH
The lower time for carrying out 8 minutes.The concentration of aluminum precursor used is as follows：Al2(SO4)3=102 g/l（It is expressed as Al2O3）, and
NaAlOO=155 g/l（It is expressed as Al2O3）.It is stirred in whole building-up process under 350 rpm.
According to 1.80 alkali/sour weight than by adjust pH to 9.3 value in a manner of 19.6 ml/mins stream
Through 8 minutes by aluminum sulfate Al under amount2(SO4)3Solution be added continuously in sodium aluminate NaAlOO solution.The temperature of reaction medium
Degree is maintained at 30 DEG C.
Obtain the suspension containing precipitation of alumina thing.
The desired final concentrations of aluminum oxide are 30 g/l, therefore contain the sulfuric acid of the aluminium introduced in the first settling step
Aluminium Al2(SO4)3Flow with sodium aluminate NaAlOO precursors is respectively 19.6 ml/mins and 23.3 ml/mins.
Then the temperature of the suspension obtained is improved to 57 DEG C by 30 DEG C.
Then by adding concentration as 102 g/l（It is expressed as Al2O3）Aluminum sulfate Al2(SO4)3With concentration be 155 grams/
Rise（It is expressed as Al2O3）Sodium aluminate NaAlOO carry out the second step of the co-precipitation of the suspension for being obtained.Thus will
Aluminum sulfate Al2(SO4)3Solution under the flow of 12.8 ml/mins through being added continuously within 30 minutes the first heated precipitation
In the suspension obtained at the end of step, and according to 1.68 alkali/sour weight than in a manner of to adjust pH the value to 8.7
It is added in sodium aluminate NaAlOO solution.The temperature of reaction medium is maintained at 57 DEG C in second step.
Obtain the suspension containing precipitation of alumina thing.
The desired final concentrations of aluminum oxide are 30 g/l, therefore contain the sulfuric acid of the aluminium introduced in the second settling step
Aluminium Al2(SO4)3Flow with sodium aluminate NaAlOO precursors is respectively 12.8 ml/mins and 14.1 ml/mins.
Thus obtained suspension does not suffer from maturation stage.
Then the Bu Shi in sintering is passed through（Buchner）Water is replaced on type instrument to filter obtained suspension, and
The alumina gel obtained is washed 3 times at 70 DEG C with 5 liters of distilled water.Filtering and wash time are 4 hours.
The size of obtained boehmite crystallite is measured using Scherrer methods：The size that use [020] measures=
2.9 ± 0.2 (nm)；Size=4.1 ± 0.3 (nm) for using [120] to measure.
Embodiment 3（Comparative example）：
Alumina gel is prepared according to the synthetic method of non-invention, is not that alumina gel sinks according to aspects of the present invention
PH at the end of shallow lake is under the pH more than 9.5.
1/ Precipitating boehmite AlOOH
Enable to obtain the mode for the solution that pH is 0.5 through 5 in the beaker for making to be cooled with an ice bath at a temperature of 25 DEG C
Prepared by the time of minute contains 326 ml deionized waters and 135.6 grams of Aluminium chloride hexahydrates（AlCl3）Solution.
Then, under magnetic stirring, 67.5 grams of sodium hydroxides were added through 30 minutes（NaOH）To adjust pH.In end of synthesis
When the pH that reaches be 10.Temperature is maintained at 20 DEG C in whole step process.Make the filter with 320 milliliters of water in 3 liters of beakers
Cake, which is in, to suspend.
The sample of obtained sediment is taken out from reaction medium.The XRD of sediment（Fig. 1）Show, obtained in embodiment 3
The sediment of the really boehmite of the sediment obtained.
The size of obtained boehmite crystallite is measured using Scherrer methods：The size that use [020] measures=
2.1 ± 0.2 (nm)；Size=2.8 ± 0.3 (nm) for using [120] to measure.
Embodiment 4（Comparative example）：
Alumina gel is prepared according to the synthetic method of non-invention, because carrying out pH regulation at a temperature of 40 DEG C.
1/ Precipitating boehmite AlOOH
Enable to obtain the mode for the solution that pH is 0.5 through 5 in the beaker for making to be cooled with an ice bath at a temperature of 25 DEG C
Prepared by the time of minute contains 326 ml deionized waters and 135.6 grams of Aluminium chloride hexahydrates（AlCl3）Solution.
Then, under magnetic stirring, 67.5 grams of sodium hydroxides were added through 30 minutes（NaOH）To adjust pH.In end of synthesis
When the pH that reaches be 8.Temperature is maintained at 40 DEG C in whole step process.Make the filter cake with 320 milliliters of water in 3 liters of beakers
In suspension.
The sample of obtained sediment is taken out from reaction medium.The XRD of sediment（Fig. 2）Show, obtained in embodiment 4
The sediment of the really boehmite of the sediment obtained.
The size of obtained boehmite crystallite is measured using Scherrer methods：The size that use [020] measures=
1.9 ± 0.3 (nm)；Size=2.6 ± 0.2 (nm) for using [120] to measure.
Embodiment 5（According to the present invention）：
Alumina gel is prepared using according to the synthetic method of the present invention.
1/ Precipitating boehmite AlOOH
Enable to obtain the mode for the solution that pH is 0.5 through 5 in the beaker for making to be cooled with an ice bath at a temperature of 25 DEG C
Prepared by the time of minute contains 326 ml deionized waters and 135.6 grams of Aluminium chloride hexahydrates（AlCl3）Solution.
Then, under magnetic stirring, 67.5 grams of sodium hydroxides were added through 30 minutes（NaOH）To adjust pH.In end of synthesis
When the pH that reaches be 8.Temperature is maintained at 20 DEG C during whole settling step.Make this with 320 milliliters of water in 3 liters of beakers
Filter cake, which is in, to suspend.
The sample of obtained sediment is taken out from reaction medium.The XRD of sediment（Fig. 3）Show, obtained in embodiment 5
The sediment of the really boehmite of the sediment obtained.The boehmite precipitation thing obtained in embodiment 5 has low-crystallinity.
The size of obtained boehmite crystallite is measured using Scherrer methods：The size that use [020] measures=
0.6 ± 0.1 (nm)；Size=1.4 ± 0.1 (nm) for using [120] to measure.
Embodiment 6（According to the present invention）：
Alumina gel is prepared using according to the synthetic method of the present invention.
1/ Precipitating boehmite AlOOH
Enable to obtain the mode for the solution that pH is 0.5 through 5 in the beaker for making to be cooled with an ice bath at a temperature of 25 DEG C
Prepared by the time of minute contains 326 ml deionized waters and 135.6 grams of Aluminium chloride hexahydrates（AlCl3）Solution.
Then, under magnetic stirring, 67.5 grams of sodium hydroxides were added through 30 minutes（NaOH）To adjust pH.In end of synthesis
When the pH that reaches be 8.5.Temperature is maintained at 20 DEG C in whole step process.Make the filter with 320 milliliters of water in 3 liters of beakers
Cake, which is in, to suspend.
The sample of obtained sediment is taken out from reaction medium.The XRD of sediment（Fig. 4）Show, in embodiment 6
The sediment of the really boehmite of the sediment of acquisition.The boehmite precipitation thing obtained in embodiment 6 has low-crystallinity.
The size of obtained boehmite crystallite is measured using Scherrer methods：The size that use [020] measures=
0.9 ± 0.1 (nm)；Size=1.6 ± 0.2 (nm) for using [120] to measure.
Claims (11)
1. preparing the method for alumina gel in single settling step, the settling step is included in water at 10 DEG C to 90 DEG C
At a temperature of dissolve acid aluminum precursor through the time of 2 to 60 minutes in a manner of causing the pH of solution to be 0.5 to 5 --- chlorination
Aluminium, then at a temperature of 5 DEG C to 35 DEG C through the time of 5 minutes to 5 hours by adding alkalescence into the solution obtained before
Body --- sodium hydroxide, pH is adjusted into the pH in the range of to 7.5 to 9.5, to obtain suspension.
2. preparation method as claimed in claim 1, wherein at a temperature of 10 DEG C to 75 DEG C by the acidity of aluminium before
Body --- aluminium chloride AlCl3--- it is dissolved in water.
3. such as preparation method claimed, wherein aluminium chloride AlCl in claim 1 or claim 23Solution in water
PH be 1 to 4.
4. preparation method claimed in such as any one of claims 1 to 3, wherein being adjusted at a temperature of 10 DEG C to 30 DEG C
pH。
5. preparation method claimed in such as claim 4, wherein adjusting pH at a temperature of 10 DEG C to 25 DEG C.
6. preparation method claimed in such as any one of claim 1 to 5, wherein pH is adjusted in the range of to 7.7 to 8.8
PH.
7. such as preparation method claimed in any one of claim 1 to 6, wherein the method according to the invention does not include mending
Fill settling step.
8. preparation method claimed in such as any one of claim 1 to 7, wherein the preparation method also obtains including filtering
The step of suspension of autoprecipitation step.
9. such as preparation method claimed in any one of claim 1 to 8, obtained wherein the preparation method also includes drying
The step of suspension of the optional filtering of autoprecipitation step is to obtain powder, the drying steps pass through at 120 DEG C or higher
At a temperature of dry or carried out by being spray-dried.
10. preparation method claimed in such as claim 9, wherein the preparation method also includes the powder that will be obtained
The step of shaping.
11. preparation method claimed in such as claim 10, wherein the forming step is carried out by extruding.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR1555118A FR3037054B1 (en) | 2015-06-05 | 2015-06-05 | PROCESS FOR PREPARING A BOEHMITE PRESENTING SPECIAL CRYSTALLITES |
| FR1555118 | 2015-06-05 | ||
| PCT/EP2016/058821 WO2016192894A1 (en) | 2015-06-05 | 2016-04-21 | Method for preparing a boehmite having specific crystallites |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107848825A true CN107848825A (en) | 2018-03-27 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201680032784.3A Pending CN107848825A (en) | 2015-06-05 | 2016-04-21 | The method for preparing the boehmite with specific crystallite |
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| Country | Link |
|---|---|
| CN (1) | CN107848825A (en) |
| DE (1) | DE112016002510T5 (en) |
| FR (1) | FR3037054B1 (en) |
| WO (1) | WO2016192894A1 (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120289653A1 (en) * | 2004-09-07 | 2012-11-15 | Nissan Motor Co., Ltd. | Alumina particle composite, method of manufacturing the alumina particle composite, resin composition and method of manufacturing the resin composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4676928A (en) | 1986-01-30 | 1987-06-30 | Vista Chemical Company | Process for producing water dispersible alumina |
| US6589908B1 (en) | 2000-11-28 | 2003-07-08 | Shell Oil Company | Method of making alumina having bimodal pore structure, and catalysts made therefrom |
| CA2508605C (en) | 2002-12-06 | 2011-11-29 | Albemarle Netherlands B.V. | Heavy feed hpc process using a mixture of catalysts |
| US7790652B2 (en) | 2003-09-17 | 2010-09-07 | Shell Oil Company | Process and catalyst for the hydroconversion of a heavy hydrocarbon feedstock |
| RU2432318C1 (en) * | 2010-02-03 | 2011-10-27 | ООО "Компания Катахим" | Method of producing powdered aluminium hydroxide (versions) and aluminium oxide |
-
2015
- 2015-06-05 FR FR1555118A patent/FR3037054B1/en not_active Expired - Fee Related
-
2016
- 2016-04-21 CN CN201680032784.3A patent/CN107848825A/en active Pending
- 2016-04-21 WO PCT/EP2016/058821 patent/WO2016192894A1/en active Application Filing
- 2016-04-21 DE DE112016002510.6T patent/DE112016002510T5/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120289653A1 (en) * | 2004-09-07 | 2012-11-15 | Nissan Motor Co., Ltd. | Alumina particle composite, method of manufacturing the alumina particle composite, resin composition and method of manufacturing the resin composition |
Also Published As
| Publication number | Publication date |
|---|---|
| DE112016002510T5 (en) | 2018-03-29 |
| FR3037054B1 (en) | 2021-08-27 |
| WO2016192894A1 (en) | 2016-12-08 |
| FR3037054A1 (en) | 2016-12-09 |
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