CN104338563A - Preparation technology for hydrogenation catalyst carrier and method for controlling pore diameter - Google Patents
Preparation technology for hydrogenation catalyst carrier and method for controlling pore diameter Download PDFInfo
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- CN104338563A CN104338563A CN201310343680.2A CN201310343680A CN104338563A CN 104338563 A CN104338563 A CN 104338563A CN 201310343680 A CN201310343680 A CN 201310343680A CN 104338563 A CN104338563 A CN 104338563A
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Abstract
The invention provides a preparation technology for a hydrogenation catalyst carrier and a method for controlling pore diameter. The preparation technology is characterized by comprising the following steps: a neutralization reaction process, a gel preparation process, drying and a roasting process. In order to relatively well control the pore diameter of the catalyst carrier, the following technical scheme is employed: adding an acidic solution in a controlled way and controlling the flow velocity during neutralization; in the gel forming process, controlling the addition speed of ammonia water according to the gel pH value of 7.5-9.5, so as to enable the pH value to be regularly swung; in the washing process, getting a sample and instantly filtering, adding ammonia water with the concentration of 7-8% for adjusting the pH value of a washing solution, enabling the pH value to be continuously increased by performing washing for six times, and stopping until the Cl content in the filtrate is zero. The superiority comprises that the pore size of the catalyst carrier can be relatively accurately controlled during production and satisfies demands of different consumers.
Description
(1) technical field
The present invention relates to a kind of technology of preparing of catalyst carrier, particularly a kind of preparation technology of catalyst carrier for hydrgenating and the method to pore size control.
(2) background technology
The preparation method describing general general catalyst carrier more in patent document in the past, at present in the actual use of catalyst carrier, because the field of its application is different, client proposes various different demand for the aperture of catalyst carrier, in order to control the size in catalyst carrier aperture more exactly, need to compare whole preparation process to control accurately, how to realize in process of production the control of catalyst carrier pore size Here it is our problem that will solve.
(3) summary of the invention
For solving the problem, the invention discloses a kind of preparation technology of catalyst carrier for hydrgenating and the method to pore size control, the method especially proposes the method to catalyst carrier pore size control while describing preparation technology.
Technical scheme provided by the invention is: the preparation technology of catalyst carrier for hydrgenating and the method to pore size control, is characterized in that it comprises the following steps:
1), neutralization reaction process
Get containing aluminum ions acidic aqueous solution (Al
2(SO
4)
3, AlCl
3or Al (NO
3)
3) aqueous solution, with Al
2o
3meter concentration is 2-10g/100ml) and containing aluminum ions alkaline aqueous solution (NaAlO
2or KAlO
2, with Al
2o
3meter concentration is 10-30g/100ml) or not containing aluminum ions alkaline aqueous solution (NH
4oH or NaOH, with NH
3meter concentration is 9-15g/100ml) add in the water purification under stirring simultaneously, carry out neutralization reaction;
Neutralization reaction time 0.5-3 hour; Neutral temperature 60-80 DEG C, in and PH7.5-9.0, in and slurries in Al
2o
3content is 2-10g/100ml;
2), gel process is prepared
Conventional water-soluble polymer polyethylene glycol and PEO, concentration 10%-38%, can make Al
2o
3pore volume is from 0.50m l/g to 1.44m l/g;
1. aging
Before ageing, aqueous silicate solution (Na is added
2siO
3the aqueous solution, SiO
2content is 1-10g/100ml, SiO
2addition accounts for carrier 0.1-5w%), Si-Al is combined and carries out aging again and filter;
At the aluminium hydroxide hydrogel that the aging neutralization of 30-85 DEG C, PH6-10 condition generates, ageing time 0.25-8 hour, Al in slurries
2o
3content is 5-9g/100ml, then filters;
2. wash
Washing aluminum hydroxide hydrogel, wash temperature 30-85 DEG C, control PH, to remove impurity SO
4 2-, Cl
-, Na
+;
Aluminium hydroxide hydrogel after washing, (phosphoric acid or ammonium phosphate salt, P addition is the 0.5-5w% of carrier can to add appropriate phosphorus-containing compound when needing.)；
3) dry, roasting process
Aluminum hydroxide filter cake or slurries after washing, or aluminum hydroxide filter cake after phosphorating or slurries, dry at 50-150 DEG C, make dry glue powder Al
2o
3content is greater than 70w%;
Dried dry glue, 300-700 DEG C of roasting, is converted into Y-Al
2o
3, or low SiO
2stable Y-Al
2o
3, or P
2o
5-Al
2o
3or SiO
2-P
2o
5-Al
2o
3.
Method as above, is characterized in that: add water in a reservoir in N-process, stir under be warming up to 60-80 DEG C, divide flow velocity to add acid solution with 45-60ml/.
Method as above, it is characterized in that: in plastic process, will add speed according to plastic pH value 7.5-9.5 control ammoniacal liquor is 30-60ml/m, control constant flow, constant to ensure pH value, temperature then allows to fluctuate in 60-80 DEG C, stops charging after one hour, stir, PH will realize regular swing.
Method as above, is characterized in that: in washing process, filters immediately after sampling, slurry should be preheating to more than 70C, uses water 5L, after filter cake adds washing container at every turn, need add 7-8% ammoniacal liquor to regulate the pH value of cleaning solution, in six washings, pH value is constantly risen progressively, its value is 7.5-10, stir half an hour at the specified temperature at every turn, then suction filtration, cyclic washing, filter 6 times, in filtrate, Cl is zero.
Superiority of the present invention is: the size that can control catalyst carrier aperture in process of production more exactly, meets the demand of different client.
(4) detailed description of the invention
The preparation technology of a kind of catalyst carrier for hydrgenating described above and the method to pore size control, is characterized in that it comprises the following steps:
1), neutralization reaction process
Get containing aluminum ions acidic aqueous solution (Al
2(SO
4)
3the aqueous solution, with Al
2o
3meter concentration is 6g/100ml) and containing aluminum ions alkaline aqueous solution NaAlO
2with Al
2o
3meter concentration is that 12g/100ml adds in the water purification under stirring simultaneously, carries out neutralization reaction;
3 hours neutralization reaction time; Neutral temperature 68 DEG C, in and PH7.8 ± 0.2, in and slurries in Al
2o
3content is 9g/100ml;
2), gel is prepared
Conventional water-soluble polymer polyethylene glycol and PEO, concentration 20%, can make Al
2o
3pore volume reaches 0.7 ± 0.05m l/g;
1. ageing process
At 65 DEG C, the aluminium hydroxide hydrogel that the aging neutralization of PH6-10 condition generates, ageing time 0.5 hour, in slurries, Al2O3 content is 9g/100ml, then filters;
2. wash
Washing aluminum hydroxide hydrogel, wash temperature 60 DEG C, control PH, to remove impurity SO
4 2-, Cl
-, Na
+;
3) dry, roasting process
After washing, dry at aluminum hydroxide filter cake 120 DEG C, make dry glue powder Al
2o
3content is greater than 70w%;
Dried dry glue, 550 DEG C of roastings, is converted into Y-Al
2o
3.
Method as above, it is characterized in that adding water in a reservoir in N-process, stir under be warming up to 68 DEG C, divide flow velocity to add aluminum sulfate solution with 45ml/.
Method as above, it is characterized in that in plastic process, will according to plastic pH value 7.8 ± 0.2, it is that 35ml/ divides that control sodium aluminate adds speed, controls constant flow, to ensure that pH value is constant, temperature then allows to fluctuate in 60-80 DEG C, stop charging after one hour, stir, PH will realize regular swing.
Method as above, it is characterized in that filtering immediately after sampling in washing process, slurry should be preheating to more than 60C, each water 5L, after filter cake adds washing container, need add 7-8% ammoniacal liquor to regulate the pH value of cleaning solution, in six washings, pH value is constantly risen progressively, and its value is 8.2, stirs half an hour at the specified temperature at every turn, suction filtration again, cyclic washing, filter 6 times, in filtrate, Cl is zero.
Claims (4)
1. the preparation technology of catalyst carrier for hydrgenating and the method to pore size control, is characterized in that it comprises the following steps:
1), neutralization reaction process
Get containing aluminum ions acidic aqueous solution (Al
2(SO
4)
3, AlCl
3or Al (NO
3)
3) aqueous solution, with Al
2o
3meter concentration is 2-10g/100ml) and containing aluminum ions alkaline aqueous solution (NaAlO
2or KAlO
2, with Al
2o
3meter concentration is 10-30g/100ml) or not containing aluminum ions alkaline aqueous solution (NH
4oH or NaOH, with NH
3meter concentration is 9-15g/100ml) add in the water purification under stirring simultaneously, carry out neutralization reaction;
Neutralization reaction time 0.5-3 hour; Neutral temperature 60-80 DEG C, in and PH7.5-9.0, in and slurries in Al
2o
3content is 2-10g/100ml;
2), gel process is prepared
Conventional water-soluble polymer polyethylene glycol and PEO, concentration 10%-38%, can make Al
2o
3pore volume is from 0.50m l/g to 1.44m l/g;
1. aging
Before ageing, aqueous silicate solution (Na is added
2siO
3the aqueous solution, SiO
2content is 1-10g/100ml, SiO
2addition accounts for carrier 0.1-5w%), Si-Al is combined and carries out aging again and filter;
At the aluminium hydroxide hydrogel that the aging neutralization of 30-85 DEG C, PH6-10 condition generates, ageing time 0.25-8 hour, Al in slurries
2o
3content is 5-9g/100ml, then filters;
2. wash
Washing aluminum hydroxide hydrogel, wash temperature 30-85 DEG C, control PH, to remove impurity SO
4 2-, Cl
-, Na
+;
Aluminium hydroxide hydrogel after washing, (phosphoric acid or ammonium phosphate salt, P addition is the 0.5-5w% of carrier can to add appropriate phosphorus-containing compound when needing.)；
3) dry, roasting process
Aluminum hydroxide filter cake or slurries after washing, or aluminum hydroxide filter cake after phosphorating or slurries, dry at 50-150 DEG C, make dry glue powder Al
2o
3content is greater than 70w%;
Dried dry glue, 300-700 DEG C of roasting, is converted into Y-Al
2o
3, or low SiO
2stable Y-Al
2o
3, or P
2o
5-Al
2o
3or SiO
2-P
2o
5-Al
2o
3.
2. according to the preparation technology of catalyst carrier for hydrgenating according to claim 1 and the method to pore size control, it is characterized in that adding water in a reservoir in N-process, stir under be warming up to 60-80 DEG C, divide flow velocity to add acid solution with 45-60ml/.
3. according to the preparation technology of catalyst carrier for hydrgenating according to claim 1 and the method to pore size control, it is characterized in that in plastic process, will add speed according to plastic pH value 7.5-9.5 control ammoniacal liquor is 30-60ml/m, control constant flow, constant to ensure pH value, temperature then allows to fluctuate in 60-80 DEG C, stops charging after one hour, stir, PH will realize regular swing.
4., according to the preparation technology of catalyst carrier for hydrgenating according to claim 1 and the method to pore size control, it is characterized in that, in washing process, filtering immediately after sampling, slurry should be preheating to more than 70 DEG C, uses water 5L, after filter cake adds washing container at every turn, need add 7-8% ammoniacal liquor to regulate the pH value of cleaning solution, in six washings, pH value is constantly risen progressively, its value is 7.5-10, stir half an hour at the specified temperature at every turn, then suction filtration, cyclic washing, filter 6 times, in filtrate, Cl is zero.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310343680.2A CN104338563A (en) | 2013-08-02 | 2013-08-02 | Preparation technology for hydrogenation catalyst carrier and method for controlling pore diameter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310343680.2A CN104338563A (en) | 2013-08-02 | 2013-08-02 | Preparation technology for hydrogenation catalyst carrier and method for controlling pore diameter |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104338563A true CN104338563A (en) | 2015-02-11 |
Family
ID=52495509
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|---|---|---|---|
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1141821A (en) * | 1994-06-29 | 1997-02-05 | 中国石油化工总公司抚顺石油化工研究院 | Process for preparation of hydrogenating catalyst carrier |
| CN1425612A (en) * | 2003-01-16 | 2003-06-25 | 厦门大学 | Process for preparing active aluminium oxide |
| CN102120597A (en) * | 2011-01-14 | 2011-07-13 | 北京工商大学 | Preparation method of high-purity boehmite |
| CN102259900A (en) * | 2010-05-24 | 2011-11-30 | 中国石油化工股份有限公司 | Hydrated alumina and preparation method thereof |
| CN102730724A (en) * | 2012-05-31 | 2012-10-17 | 江苏晶晶新材料有限公司 | Preparation process for large pore volume and light bulk density activated alumina |
-
2013
- 2013-08-02 CN CN201310343680.2A patent/CN104338563A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1141821A (en) * | 1994-06-29 | 1997-02-05 | 中国石油化工总公司抚顺石油化工研究院 | Process for preparation of hydrogenating catalyst carrier |
| CN1425612A (en) * | 2003-01-16 | 2003-06-25 | 厦门大学 | Process for preparing active aluminium oxide |
| CN102259900A (en) * | 2010-05-24 | 2011-11-30 | 中国石油化工股份有限公司 | Hydrated alumina and preparation method thereof |
| CN102120597A (en) * | 2011-01-14 | 2011-07-13 | 北京工商大学 | Preparation method of high-purity boehmite |
| CN102730724A (en) * | 2012-05-31 | 2012-10-17 | 江苏晶晶新材料有限公司 | Preparation process for large pore volume and light bulk density activated alumina |
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Application publication date: 20150211 |
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