CN104338488A - Automatic control production and preparation technology for hydrogenation catalyst carrier - Google Patents
Automatic control production and preparation technology for hydrogenation catalyst carrier Download PDFInfo
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- CN104338488A CN104338488A CN201310343699.7A CN201310343699A CN104338488A CN 104338488 A CN104338488 A CN 104338488A CN 201310343699 A CN201310343699 A CN 201310343699A CN 104338488 A CN104338488 A CN 104338488A
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- catalyst carrier
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- control device
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
- B01J21/04—Alumina
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
- B01J2523/30—Constitutive chemical elements of heterogeneous catalysts of Group III (IIIA or IIIB) of the Periodic Table
- B01J2523/31—Aluminium
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Catalysts (AREA)
Abstract
The invention provides an automatic control production and a preparation technology for a hydrogenation catalyst carrier. The automatic control production for the hydrogenation catalyst carrier comprises a kettle body and a control center, and the control center is composed of a temperature and pressure controller, a stirring controller, a left electromagnetic feeding system, a right electromagnetic feeding system and a sampling controller. The preparation technology for the hydrogenation catalyst carrier 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 during neutralization; and 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. The superiority comprises that the reaction apparatus is operated by the automatic control center, 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 process units and technology of catalyst carrier, particularly a kind of automatic production control device of catalyst carrier for hydrgenating and preparation technology.
(2) background technology
Due to the pore size of catalyst carrier will be controlled in catalyst support preparation process, and last output the pore size of catalyst carrier and the preparation condition of whole production in reaction temperature, solution reaction concentration, solution pH value, agitating mode all relevant.The reaction condition key element that more importantly common most of chemical reaction relies on is a steady state value, and the reaction condition key element relied in catalyst support preparation process is a cyclically-varying value.If we control repeatedly to sample by full manual mode, charging repeatedly, repeatedly stir to do and extremely bother like this, and are difficult to the accuracy of Control release.Inventing a kind of controllable reaction still makes whole reaction all can be controlled by control centre, one of our invention problem that Here it is.In addition, 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 another problem that will solve.
(3) summary of the invention
The object of the present invention is to provide a kind of automatic production control device and preparation technology of catalyst carrier for hydrgenating; The automatic production control device of hydrogen catalyst carrier will enter heat, go out heat pipe, multiple feed pipe, sampler, agitator, add decompressor and will all control by control centre is unified, ensure the accurate operation of chemical reaction; The preparation technology of catalyst carrier for hydrgenating, provides preparation technology in detail, especially proposes the method to catalyst carrier pore size control.
A kind of automatic production control device of catalyst carrier for hydrgenating, comprise kettle, kettle is provided with into heat pipe, goes out heat pipe, motor, decelerator, feed pipe, safety valve, pressurization gas relief line, agitator, the discharging mouth of pipe, it is characterized in that: kettle forcing pipe is provided with and adds pressure electromagnetic valve, enter heat pipe and be provided with heating electromagnetic valve, they are connected with temperature pressure controller jointly; The motor of kettle is provided with electric machine control system, and electric machine control system is connected with mixing control device; The feed pipe on the left side is provided with left electromagnetism feeding system, the feed pipe on the right is provided with right electromagnetism feeding system, they respectively connected left and right feed system controller; Sampler is provided with sampler electromagnetic pump, sampler electromagnetic pump is connected to sampling controller; Temperature pressure controller, mixing control device, left and right electromagnetism feeding system and sampling controller form control centre jointly.
A preparation technology for catalyst carrier for hydrgenating, 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 A1 (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/100m1) 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/100m1;
2), gel process is prepared
Conventional water-soluble polymer polyethylene glycol and PEO, concentration 10%-38%, can make Al
2o
3pore volume is from 0.50m1/g to 1.44m1/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/100m1, 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, 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/.
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, 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, C1 is zero.
Superiority of the present invention is: the automatic production control device of catalyst carrier for hydrgenating will enter heat, go out heat pipe, multiple feed pipe, sampler, agitator, add decompressor and all control by control centre is unified, facilitate the cyclically-varying of realization response condition element, ensure the accurate operation of chemical reaction; The preparation technology of catalyst carrier for hydrgenating, can control the size in catalyst carrier aperture in process of production more exactly, meet the demand of different client.
(4) detailed description of the invention
A kind of automatic production control device of catalyst carrier for hydrgenating, comprise kettle, kettle is provided with into heat pipe, goes out heat pipe, motor, decelerator, feed pipe, safety valve, pressurization gas relief line, agitator, the discharging mouth of pipe, it is characterized in that: kettle forcing pipe is provided with and adds pressure electromagnetic valve, enter heat pipe and be provided with heating electromagnetic valve, they are connected with temperature pressure controller jointly; The motor of kettle is provided with electric machine control system, and electric machine control system is connected with mixing control device; The feed pipe on the left side is provided with left electromagnetism feeding system, the feed pipe on the right is provided with right electromagnetism feeding system, they respectively connected left and right feed system controller; Sampler is provided with sampler electromagnetic pump, sampler electromagnetic pump is connected to sampling controller; Temperature pressure controller, mixing control device, left and right electromagnetism feeding system and sampling controller form control centre jointly.
A preparation technology for catalyst carrier for hydrgenating, 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 ± 0.05m1/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 (5)
1. the automatic production control device of a catalyst carrier for hydrgenating, comprise kettle, kettle is provided with into heat pipe, goes out heat pipe, motor, decelerator, feed pipe, safety valve, pressurization gas relief line, agitator, the discharging mouth of pipe, it is characterized in that: kettle forcing pipe is provided with and adds pressure electromagnetic valve, enter heat pipe and be provided with heating electromagnetic valve, they are connected with temperature pressure controller jointly; The motor of kettle is provided with electric machine control system, and electric machine control system is connected with mixing control device; The feed pipe on the left side is provided with left electromagnetism feeding system, the feed pipe on the right is provided with right electromagnetism feeding system, they respectively connected left and right feed system controller; Sampler is provided with sampler electromagnetic pump, sampler electromagnetic pump is connected to sampling controller; Temperature pressure controller, mixing control device, left and right electromagnetism feeding system and sampling controller form control centre jointly.
2. a preparation technology for catalyst carrier for hydrgenating, is characterized in that it comprises the following steps:
1), neutralization reaction process
Get containing aluminum ions acidic aqueous solution (A1
2(SO
4)
3, AlCl
3or A1 (NO
3)
3) aqueous solution, with Al
2o
3meter concentration is 2-10g/100m1) 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 0.50m1/g to 1.44m1/g;
1. aging
Before ageing, aqueous silicate solution (Na is added
2siO
3the aqueous solution, SiO
2content is 1-10g/100m1, 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/100m1, 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.
3. according to automatic production control device and the preparation technology of catalyst carrier for hydrgenating according to claim 1, 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 45-60m1/.
4. according to automatic production control device and the preparation technology of catalyst carrier for hydrgenating according to claim 1, it is characterized in that in plastic process, will add speed according to plastic pH value 7.5-9.5 control ammoniacal liquor is 30-60m1/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.
5., according to automatic production control device and the preparation technology of catalyst carrier for hydrgenating according to claim 1, 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 |
|---|---|---|---|
| CN201310343699.7A CN104338488A (en) | 2013-08-02 | 2013-08-02 | Automatic control production and preparation technology for hydrogenation catalyst carrier |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310343699.7A CN104338488A (en) | 2013-08-02 | 2013-08-02 | Automatic control production and preparation technology for hydrogenation catalyst carrier |
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| Publication Number | Publication Date |
|---|---|
| CN104338488A true CN104338488A (en) | 2015-02-11 |
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ID=52495435
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|---|---|---|---|
| CN201310343699.7A Pending CN104338488A (en) | 2013-08-02 | 2013-08-02 | Automatic control production and preparation technology for hydrogenation catalyst carrier |
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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 |
| JP2002028491A (en) * | 2000-07-12 | 2002-01-29 | Catalysts & Chem Ind Co Ltd | Formed catalyst for hydrogenation treatment and producing method thereof |
| CN2915247Y (en) * | 2006-06-29 | 2007-06-27 | 上海保兴生物设备工程有限公司 | Self controlled reactor for solid liquid reaction and separation |
| CN102399330A (en) * | 2010-09-15 | 2012-04-04 | 中国石油天然气股份有限公司 | Preparation method of high-purity modified silica gel carrier |
| 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 CN201310343699.7A patent/CN104338488A/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 |
| JP2002028491A (en) * | 2000-07-12 | 2002-01-29 | Catalysts & Chem Ind Co Ltd | Formed catalyst for hydrogenation treatment and producing method thereof |
| CN2915247Y (en) * | 2006-06-29 | 2007-06-27 | 上海保兴生物设备工程有限公司 | Self controlled reactor for solid liquid reaction and separation |
| CN102399330A (en) * | 2010-09-15 | 2012-04-04 | 中国石油天然气股份有限公司 | Preparation method of high-purity modified silica gel carrier |
| 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 |