CN105983444A - Preparation method of aluminum oxide carrier - Google Patents
Preparation method of aluminum oxide carrier Download PDFInfo
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- CN105983444A CN105983444A CN201510041352.6A CN201510041352A CN105983444A CN 105983444 A CN105983444 A CN 105983444A CN 201510041352 A CN201510041352 A CN 201510041352A CN 105983444 A CN105983444 A CN 105983444A
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Abstract
A preparation method of an aluminum oxide carrier includes the steps of: 1) kneading and shaping step: adding water, a peptizer and an extrusion aid to dry pseudo-boehmite colloid powder, fully kneading and shaping the mixture, and drying the mixture to obtain granules; 2) pre-roasting step: pre-roasting the granules formed in the step 1) at a certain temperature; 3) spraying step: spraying an acid or an acid solution or spraying water and the acid or the acid solution on the pre-roasted granules according to saturated water absorption rate of the granules, and allowing the granules to stand for a certain time at room temperature; and 4) high-temperature roasting step: drying the granules treated in the step 3) and then roasting the granules at a high temperature to obtain the aluminum oxide carrier.
Description
Technical field
The present invention relates to the preparation method of a kind of alumina support, particularly to one at mink cell focus hydrogenation
The carrying alumina preparation of reason catalyst.
Background technology
The inferior heavy oil such as impurity content such as wax tailings, residual oil is higher, it usually needs through hydrotreating (as
Residual hydrogenation) impurity such as sulfur of removing wherein most, in order to produce through follow-up processing (such as catalytic cracking)
Go out oil product and the industrial chemicals such as the vapour of cleaning, diesel oil.Containing substantial amounts of colloid and drip in the inferior heavy oil such as residual oil
Blue or green matter, moieties molecular weight is big, structure is complicated for this, and diffusion difficulty, therefore it is required that catalyst has excellent
Pore passage structure, to improve de-impurity activity and the stability of catalyst.
Owing to the pore structure of catalyst has important impact to its performance, therefore for mink cell focus hydrotreating
Catalyst, needs have unobstructed duct and bigger pore volume.Duct is unobstructed is conducive to macromole in mink cell focus
The diffusion of hydrocarbons and reaction, thus improve the reactivity of catalyst；Avoid metal deposit or anti-simultaneously
Coking is answered to cause the blocking of catalyst aperture to cause rapid catalyst deactivation, to improve the activity stabilized of catalyst
Property.Therefore the catalyst for hydroprocessing of heavy oil that a duct is unobstructed, will have good reactivity and work
Property stability.
In order to improve the pore volume of alumina support and obtain unimpeded duct, current commonly used addition expanding agent
Method, such as the United States Patent (USP) of Publication No. US4448896 disclose with a kind of boehmite be
Raw material, and add carbon powder as expanding agent, through kneading, extrusion, is dried and roasting obtains alumina support.
Its shortcoming is: add a small amount of carbon powder, then be easily formed " ink bottle " type hole；Add too much carbon powder,
Support strength is then caused substantially to reduce.
Publication No. US4066574, discloses one in the United States Patent (USP) of US4113661 and US4341625
Plant the preparation method of alumina support, i.e. in Alpha-alumina monohydrate, be initially charged aqueous solution of nitric acid, fully
Add a certain amount of ammonia spirit after effect, reach to expand the purpose of carrier pore volume.Although the method is permissible
Play reaming effect, but carrier hole diameter is single distribution by particle exterior surface to center, be unfavorable for maximizing
Ground plays the effect of granule surfaces externally and internally.
To sum up, the method for prior art also exists reaming poor effect, the single distribution of Carrier diameters, duct
The openst, easily block, and the problem that the arbitrarily regulation of duct shape cannot be carried out as desired.
Summary of the invention
The technical purpose of the present invention is to provide the preparation method of a kind of alumina support, to solve prior art
Present in reaming poor effect, the single distribution of Carrier diameters, duct is the openst, easily blocks, and
The problem that cannot carry out the arbitrarily regulation of duct shape as desired.
For reaching above-mentioned purpose, the invention provides the preparation method of a kind of alumina support, described preparation method
Comprise the following steps:
Kneading and compacting step: add water, peptizer and extrusion aid in boehmite dry glue powder, the most mixed
Pinch molding and be dried, generating particulate matter；
Preroast step: the described particulate matter of gained in described kneading and compacting step is carried out at a certain temperature
Preroast；
Spraying step: to gained in described preroast step to described particulate matter uniformly to spray concentration continuous
The acid increased or acid solution, or successively shower water and acid or acid solution, or spray concentration by low to
After high two or more acid or acid solution, described particulate matter is stood 0.5～3 hour in room temperature；
High temperature firing steps: the particulate matter of gained in described spraying step is dried rear high-temperature roasting,
To final described alumina support.
The preparation method of above-mentioned alumina support, adds in forming process described in described kneading and compacting step
Auxiliary agent.
The preparation method of above-mentioned alumina support, cylindrically shaped or be special-shaped after described particulate matter molding,
Described abnormal shape includes: Herba Trifolii Pratentis, Herba Galii Bungei or butterfly.
The preparation method of above-mentioned alumina support, the baking temperature in described kneading and compacting step is 90～150
DEG C, drying time is 1～3 hour.
The preparation method of above-mentioned alumina support, the treatment temperature in described preroast step is 200～450
DEG C, the process time is 1～8 hour.
The preparation method of above-mentioned alumina support, in described preroast step, treatment temperature optimum is 250～400
DEG C, processing time optimal is 2～5 hours.
The preparation method of above-mentioned alumina support, it is characterised in that in described spraying step while spray,
Continuously adjust the concentration of acid or acid solution.
The preparation method of above-mentioned alumina support, it is characterised in that in described spraying step, first spray is certain
The water of amount, the two or more acid more from low to high of spray acid or acid solution or concentration or acid solution.
The preparation method of above-mentioned alumina support, it is characterised in that in described spraying step, spray concentration by
Low paramount two or more acid or acid solution.
The preparation method of above-mentioned alumina support, it is characterised in that in described spraying step, described particulate matter
0.5～3 hour is stood in room temperature.
The preparation method of above-mentioned alumina support, described in described spraying step acid or acid solution be nitric acid or
Acetic acid and solution thereof.
The preparation method of above-mentioned alumina support, described extrusion aid be Sesbania cannabina (Retz.) Pers. powder, starch, polyvinyl alcohol,
One or more in methylcellulose；
The preparation method of above-mentioned alumina support, described auxiliary agent is the elements such as phosphorus, boron, fluorine, silicon, titanium, zirconium
Compound in one or more.
The preparation method of above-mentioned alumina support, described in described high temperature firing steps, drying condition is
90～150 DEG C are dried 1～3 hour, and roasting condition is 600～1000 DEG C of roastings 1～8 hours.
The preparation method of above-mentioned alumina support, the average channel diameter of described alumina support is along carrier granular
Radially being gradually increased from center to outer surface, described duct is open trumpet type pore passage structure.
The preparation method of above-mentioned alumina support, described alumina support from granular center to grain diameter
The average pore diameter of 50% is little compared to from the average pore diameter of grain diameter 80% to particle surface
1～12nm.
The preparation method of above-mentioned alumina support, the pore volume of described alumina support is 0.72～0.73mL.g-1,
The specific surface area of described alumina support is 201～212m2.g-1, the average pore diameter of described alumina support
It is 13.6～14.5nm.
Compared with existing catalyst carrier preparation method, having the beneficial effects that of the inventive method: reaming effect
Good, carrier hole diameter is open distribution, and duct is open, is not easily blocked, and can random adjustment hole on demand
Road shape.
Accompanying drawing explanation
Fig. 1 is the preparation method schematic flow sheet of alumina support of the present invention.
Wherein, reference:
S1～S4: specific embodiment of the invention step
Detailed description of the invention
Obviously, the many modifications and variations that those skilled in the art are done based on spirit of the invention belong to this
Bright protection domain.
The inventive method is characterized by: 1) first aluminium oxide precursor is shaped and is dried；2) to molding
Dried material carries out preroast at a temperature of 200-450 DEG C；3) with acid or the acid solution spray of variable concentrations
Drenching, room temperature stands 0.5-3 hour；4) again the material after acid treatment is dried and roasting.
The preparation method of a kind of alumina support of the inventive method, the method includes molding dried
Aluminium oxide precursor carries out preroast, and the solution being gradually increased by acid concentration processes, after room temperature stands
Being dried and roasting, wherein pre-calcination temperature is 200-450 DEG C, and the acid treatment time is 0.5-3 hour, roasting
Temperature is 600-1000 DEG C, and roasting time is 1-8 hour.Its average hole of alumina support that the present invention provides
Diameter along carrier granular radially from center to outer surface in being gradually increased, aperture compared with big, duct is open, diffusion
Function admirable, can use as catalyst carrier particularly catalyst for hydroprocessing of heavy oil carrier.
The principle that the present invention makes carrier duct unimpeded is: to the particulate matter after shaping and drying by its saturated water absorption
Spray acid or acid solution or shower water and acid or acid solution.Spray while, continuously adjust acid or
The concentration of acid solution；Or first spray a certain amount of water, then spray acid or acid solution or concentration are by as little as
High two or more acid or acid solution；Or spray concentration two or more acid from low to high or acidity
Solution.Due to the effect of capillary pressure, make acid or acid solution by the successively entrance from low to high of its concentration
Grain thing duct, finally making solution acid concentration in particulate matter duct is increase tendency by granular center to outer surface.
By the effect between acid or acid solution and boehmite, the bore dia in duct is made to be expanded.Due to
The difference of acid solutions, causes its reaming effect different, finally makes carrier duct from granular center to appearance
Face, in being gradually increased trend, forms open " trumpet type " pore passage structure, so that the pore volume of carrier increases
Greatly, duct is open.
As it is shown in figure 1, the preparation method of a kind of alumina support, described preparation method comprises the following steps:
Kneading and compacting step S1: add water, peptizer and extrusion aid in boehmite dry glue powder, fill
Divide kneading and compacting and be dried, generating particulate matter；Auxiliary agent is added in forming process；
Preroast step S2: the particulate matter of gained in kneading and compacting step S1 is carried out pre-at a certain temperature
Roasting；
Spraying step S3: to gained in preroast step S2 to particulate matter uniformly spray concentration and increase continuously
The acid added or acid solution, or successively shower water and sour or acid solution, or spray concentration is from low to high
Two or more acid or acid solution after, by particulate matter room temperature stand 0.5～3 hour；
High temperature firing steps S4: the particulate matter of gained in spraying step S3 is dried rear high-temperature roasting,
Obtain final alumina support.
Combine shown in Fig. 1 below by way of specific embodiment, the flow process of detailed description the inventive method:
The one of alumina support is prepared as follows:
(1), weigh boehmite dry glue powder, add peptizer and extrusion aid, abundant kneading aftershaping.
The most different auxiliary agents can be added as required in forming process；
(2), it is dried 1～3 hour at 90～150 DEG C by (1) gained material；
(3), processed 2～5 hours at 200～450 DEG C by (2) gained material；
(4) acid or the acid solution that concentration increases continuously, to dried particulate matter is uniformly sprayed, or first
Rear shower water and sour or acid solution, or the two or more acid or acid molten that spray concentration is from low to high
Liquid, room temperature stands 0.5～3 hour；
(5), being dried 1～3 hour at 90～150 DEG C, gained material is little in 600～1000 DEG C of roastings 1～8
Time.
Using acid or acid solution in the specific embodiment of the invention is nitric acid or acetic acid and solution thereof.
The extrusion aid used in the specific embodiment of the invention is Sesbania cannabina (Retz.) Pers. powder, starch, polyvinyl alcohol, Methyl cellulose
One or more in element.Described auxiliary agent can be the change of the elements such as phosphorus, boron, fluorine, silicon, titanium, zirconium
One or more in compound.
The shape using alumina support in the specific embodiment of the invention can change according to different requirements
Become.Carrying alumina body formed after the most cylindrically shaped or be abnormal shape, abnormal shape includes: Herba Trifolii Pratentis, Herba Galii Bungei or
Butterfly, but the specific embodiment of the invention is not limited thereto.
Alumina support in the specific embodiment of the invention, can be used as catalyst carrier for hydrgenating, is particularly well-suited to weight
Matter oil hydrogenating treatment catalyst carrier.
Inventive feature is further illustrated below with embodiment and comparative example.
Embodiment 1
Weigh the boehmite dry glue powder 500g that Shandong Zibo ten thousand continuous heavy rain Chemical Co., Ltd. produces, add clean
Water, sesbania powder, acetic acid, after abundant kneading, banded extruder is extruded into the cylinder of a diameter of 2.0mm.
It is dried 2.0 hours at 120 DEG C, processes 3 hours at 300 DEG C.Take particulate matter after 100g processes, will
64.0g deionized water uniformly sprays to gained alumina support with the speed of 30mL/ minute, shower water same
Time in aforementioned deionized water, be uniformly added into glacial acetic acid 16.0g with the speed of 4.0g/ minute.It is sprayed to particulate matter
After saturated water absorption, room temperature stands 1.0 hours.It is dried 2.0 hours at 120 DEG C, 750 DEG C of roastings 3.0
Hour, obtaining carrier A, its character is shown in Table 1.
Embodiment 2
Taking aforementioned boehmite dry glue powder 500g, method same as in Example 1 carries out extrusion and is dried,
Process 3 hours at 250 DEG C.Take particulate matter after 100g processes, be 10.0wt%'s by 48.0g concentration
Acetum uniformly sprays on material, is finally uniformly sprayed by the acetum that 32.0g concentration is 15.0wt%
Pour on gained material.Room temperature stands 1.0 hours.Method same as in Example 1 is dried and roasting,
Carrier B, its character is shown in Table 1.
Embodiment 3
Taking aforementioned boehmite dry glue powder 500g, method same as in Example 1 carries out extrusion and is dried also
Process.Take particulate matter after 100g processes, 56.0g deionized water is uniformly sprayed on gained material, with
After the acetum that 24.0g concentration is 10.0wt% is uniformly sprayed on material.Room temperature stands 1.0 hours.
Method same as in Example 1 is dried and roasting, obtains support C, and its character is shown in Table 1.
Embodiment 4
Taking aforementioned boehmite dry glue powder 500g, method same as in Example 1 carries out extrusion and is dried,
Process 2 hours at 450 DEG C.Take particulate matter after 100g processes, 56.0g deionized water is uniformly sprayed
On gained material, subsequently the acetum that 24.0g concentration is 10.0wt% is uniformly sprayed on material.Room
Gentle and quiet put 2.0 hours.Method same as in Example 1 is dried and roasting, obtains carrier D, and its character is shown in Table
1。
Embodiment 5
Taking aforementioned boehmite dry glue powder 500g, method same as in Example 1 carries out extrusion and is dried also
Process.Take particulate matter after 100g processes, 56.0g deionized water is uniformly sprayed on gained material, with
After the acetum that 24.0g concentration is 10.0wt% is uniformly sprayed on material.Room temperature stands 2.0 hours.
Being dried 2.0 hours at 120 DEG C, 850 DEG C of roastings 3.0 hours, obtain carrier E, its character is shown in Table 1.
Comparative example 1
Taking aforementioned boehmite dry glue powder 500g, method same as in Example 1 carries out extrusion, 120
DEG C being dried after 2.0 hours roasting 3 hours at 750 DEG C, obtain carrier F, its character is shown in Table 1.
Comparative example 2
Taking aforementioned boehmite dry glue powder 500g, method same as in Example 1 carries out extrusion and is dried also
Process.Take particulate matter after 100g processes, the acetum that 80.0g concentration is 10.0wt% is uniformly sprayed
On material.Room temperature stands 1.0 hours.Method same as in Example 1 is dried and roasting, obtains carrier G,
Its character is shown in Table 1.
Table 1 support
Refer to the average pore diameter of a carrier part
Refer to that on carrier cross section, the certain point distance away from carrier granular center accounts for the hundred of its cross sectional radius
Proportion by subtraction
As shown in Table 1, carrier A, B, C, D and E of the present invention, pore volume is relatively big, has from granule
The heart to outer surface is the open pore passage structure of increase tendency；And comparison vehicle E pore volume is little, pore passage structure list
One, although comparison vehicle F has bigger pore volume, but pore passage structure is single.
Have been shown that the detailed embodiment of the present invention above, it is therefore apparent that those skilled in the art is not disobeying
On the premise of the back of the body present invention, part modifications and changes can be carried out；The content mentioned in described above and accompanying drawing
It is only used as illustrative case, is not limitation of the present invention；There is technical characteristic described in the invention
Filter, each fall within the protection domain of patent of the present invention.
Claims (17)
1. the preparation method of an alumina support, it is characterised in that comprise the following steps:
Kneading and compacting step: add water, peptizer and extrusion aid in boehmite dry glue powder, the most mixed
Pinch molding and be dried, generating particulate matter；
Preroast step: the described particulate matter of gained in described kneading and compacting step is carried out at a certain temperature
Preroast；
Spraying step: to the particulate matter after preroast, by the saturated water absorption spray acid of described particulate matter
Or acid solution or shower water and acid or acid solution, described particulate matter is stood a period of time in room temperature；
High temperature firing steps: the particulate matter of gained in described spraying step is dried rear high-temperature roasting,
To final described alumina support.
The preparation method of alumina support the most according to claim 1, it is characterised in that described mixed
Pinch and forming process adds described in forming step auxiliary agent.
The preparation method of alumina support the most according to claim 1, it is characterised in that described granule
After thing molding cylindrically shaped or be special-shaped, described abnormal shape includes: Herba Trifolii Pratentis, Herba Galii Bungei or butterfly.
The preparation method of alumina support the most according to claim 1, it is characterised in that described kneading
Baking temperature in forming step is 90～150 DEG C, and drying time is 1～3 hour.
The preparation method of alumina support the most according to claim 1, it is characterised in that described prebake
The treatment temperature burnt in step is 200～450 DEG C, and the process time is 1～8 hour.
The preparation method of alumina support the most according to claim 5, it is characterised in that described prebake
Burning treatment temperature optimum in step is 250～400 DEG C, and processing time optimal is 2～5 hours.
The preparation method of alumina support the most according to claim 1, it is characterised in that described spray
In step while spray, continuously adjust the concentration of acid or acid solution.
The preparation method of alumina support the most according to claim 1, it is characterised in that described spray
In step, first spray a certain amount of water, then spray acid or acid solution or concentration from low to high two or more
Acid or acid solution.
The preparation method of alumina support the most according to claim 1, it is characterised in that described spray
In step, spray concentration two or more acid from low to high or acid solution.
The preparation method of alumina support the most according to claim 1, it is characterised in that described spray
In step, described particulate matter stands 0.5～3 hour in room temperature.
The preparation method of 11. alumina supports according to claim 1, it is characterised in that described spray
Acid or acid solution described in step are nitric acid or acetic acid and solution thereof.
The preparation method of 12. alumina supports according to claim 1, it is characterised in that described helps
Crowded agent is one or more in Sesbania cannabina (Retz.) Pers. powder, starch, polyvinyl alcohol, methylcellulose.
The preparation method of 13. alumina supports according to claim 2, it is characterised in that described auxiliary agent
For one or more in the compound of the elements such as phosphorus, boron, fluorine, silicon, titanium, zirconium.
The preparation method of 14. alumina supports according to claim 1, it is characterised in that described high temperature
Drying condition described in calcination steps is 90～150 DEG C and is dried 1～3 hour, and roasting condition is 600～1000 DEG C
Roasting 1～8 hours.
The preparation method of 15. alumina supports according to claim 1, it is characterised in that described oxidation
The average channel diameter of alumina supporter is radially gradually increased along carrier granular from center to outer surface, and described duct is
Open trumpet type pore passage structure.
The preparation method of 16. alumina supports according to claim 1, it is characterised in that described oxidation
Alumina supporter from granular center to the average pore diameter of grain diameter 50%, compared to from grain diameter 80%
Average pore diameter little 1～12nm to particle surface.
17. the preparation method of alumina support according to claim 1, it is characterised in that described oxidation
The pore volume of alumina supporter is 0.72～0.73mL.g-1, and the specific surface area of described alumina support is
201～212m2.g-1, the average pore diameter of described alumina support is 13.6～14.5nm.
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| CN107983405A (en) * | 2016-10-26 | 2018-05-04 | 中国石油化工股份有限公司 | A kind of preparation method of hydrogenation catalyst |
| CN107983326A (en) * | 2016-10-26 | 2018-05-04 | 中国石油化工股份有限公司 | A kind of preparation method of hydrogenation catalyst shaping carrier |
| CN111939885A (en) * | 2020-07-30 | 2020-11-17 | 上海氯碱化工股份有限公司 | Pore diameter adjustable alumina carrier and preparation method thereof |
| CN112044445A (en) * | 2020-08-25 | 2020-12-08 | 上海氯碱化工股份有限公司 | Catalyst for preparing chlorine by catalytic oxidation of hydrogen chloride and preparation method and application thereof |
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| CN111939885A (en) * | 2020-07-30 | 2020-11-17 | 上海氯碱化工股份有限公司 | Pore diameter adjustable alumina carrier and preparation method thereof |
| CN112044445A (en) * | 2020-08-25 | 2020-12-08 | 上海氯碱化工股份有限公司 | Catalyst for preparing chlorine by catalytic oxidation of hydrogen chloride and preparation method and application thereof |
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Application publication date: 20161005 |