CN100556545C - A kind of is the production method of the catalyst of active component with copper zinc - Google Patents
A kind of is the production method of the catalyst of active component with copper zinc Download PDFInfo
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- CN100556545C CN100556545C CNB2006100978749A CN200610097874A CN100556545C CN 100556545 C CN100556545 C CN 100556545C CN B2006100978749 A CNB2006100978749 A CN B2006100978749A CN 200610097874 A CN200610097874 A CN 200610097874A CN 100556545 C CN100556545 C CN 100556545C
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Abstract
The invention belongs to catalyst technical field, being specifically related to low bulk density copper zinc is the preparation method of the Cu-series catalyst of active component.By adopting the filtration of film circulation cleaning, spray drying granulation, two-sided chain-plate type far-infrared dryer calcining novel technique, replace decantation washing slip, plate compression in the existing production technology, roll, preparation semi-product material operations such as granulation, particle calcining, reduce labor intensity, reduce production costs, improve Catalyst Production serialization operation degree.
Description
Technical field:
The invention belongs to catalyst technical field, be specifically related to the preparation method of low bulk density Cu-series catalyst.
Background technology:
Present copper-zinc-aluminium System Catalyst preparation method is the soluble-salt mixed solution and the precipitating reagent reaction of copper, zinc, obtains copper, zinc precipitation, adds carrier again, makes catalyst through washing, filter, dry, grind operations such as material, granulation, roasting, moulding.Generally in the industrial production adopt co-precipitation, decantation washing slip, plate compression, roll, granulation, particle calcining, beat technology such as sheet moulding, manufactured copper series catalysts.The subject matter that this manufacturing process technology exists is: decantation washing slip, plate compression, and water consumption is big, cost is high, occurs easily running material, causes loss of material and environmental pollution; Roll, semi-product material preparation sections such as granulation, particle calcining, labour intensity is big, efficient is low, easily causes dust pollution because the material grinding compacting, the catalyst finished product bulk density that finally makes is higher.And technological process is long, and production cost is also high.
Summary of the invention:
The objective of the invention is to propose a kind of is the new preparation method of Cu-series catalyst of active component with copper zinc.Catalyst with the inventive method preparation has bulk density and higher intensity and activity and the heat endurance lower than the catalyst of conventional method preparation, can satisfy higher needs.Catalyst with the inventive method is produced has shortened technological process greatly, thereby has reduced production cost
The present invention is achieved in that by adopting the filtration of film circulation cleaning, spray drying granulation, far-infrared ray drying calcining novel technique, replace decantation washing slip in the existing production technology, roll, preparation semi-product material operations such as granulation, particle calcining, reduce labor intensity, reduce production costs, improve Catalyst Production serialization operation degree.Two-sided chain-plate type far-infrared dryer
Preparation method specifically of the present invention comprises batching co-precipitation, semi-product material preparation, beats the sheet molding procedure, it is characterized in that the semi-product material preparation section in turn includes the following steps: the filtration of film circulation cleaning, spray drying granulation, far-infrared dryer calcining.The material of film can be divided into it polysulfones, polyester, Nomex, polytetrafluoroethylene (PTFE), inorganic ceramic material film or metal micro-holes film etc.The membranous wall micropore that gathers can make different apertures as requested.Under pressure, slip is in the film flows inside, and by film, the macromolecular substances tunicle is held back and reached the purpose of separations, concentrated and purifying less than the small-molecule substance in membranous wall aperture.The type selecting of film need be determined according to slip granule size and characteristic.The preferred scheme of filtering the film circulation cleaning adopts shell and tube continuous filtration thickener.Spray-drying is to adopt atomizer that material liquid is separated into droplet, and obtains a kind of drying means of product with hot gas (air, nitrogen or overheated steam) dry droplet.Material liquid can be solution, emulsion, suspension, also can be that fused solution or cream are stuck with paste liquid.Dry products can be made into powdery, graininess, hollow ball or a shape as required.Material liquid of the present invention is that cream is stuck with paste liquid, and needing dried product is graininess.
Spray-dired committed step is the atomizing of liquid and the selection of nozzle.
The atomizer that feed liquid is separated into droplet is spray-dired critical component, and at present commonly used have 3 kinds of atomizers.
1) pneumatic atomizer adopt compressed air or steam with very high speed (〉=300m/s) from the nozzle ejection, the frictional force that speed difference produced by between gas-liquid two-phase makes feed liquid be split into droplet.
2) pressure atomizer makes liquid obtain high pressure with high-pressure pump, and highly pressurised liquid is during by nozzle, can change pressure into kinetic energy and is separated into droplet when spraying at a high speed.
3) the rotary atomizer feed liquid (is subjected to centrifugal action to throw away and atomize from plate edge at high speed rotating plate in the peripheral speed 90～160m/s).
The spray-drying of solution was finished in moment.For this reason, must increase its decentralization to greatest extent, promptly increase the surface area in the unit volume solution, could quicken to conduct heat and mass transport process.For example volume is 1m
3Solution, if it is dispersed into the spherical droplet that diameter is 10 μ m, compare before and after disperseing, surface area increases 1290 times, thereby has increased evaporating surface widely, has shortened drying time.
The far-infrared ray drying calcination process preferably adopts two-sided chain-plate type far-infrared dryer.This machine is a kind of high energy-conservation continuous drying and calcining equipment, adopts advanced far infrared drying technology and the two-sided carrying method of carrier bar.This machine divides upper, middle and lower three groups of two-sided carrier bar structure for conveying, and six layers of material come and go to be carried, every group of conveyor zones independence automatic constant-temperature control.Adopt ac motor speed control by variable frequency, promptly the transporting velocity of material is stepless adjustable, and can regulate arbitrarily drying time.
The specific embodiment:
Below in conjunction with embodiment the present invention is described in detail.
Embodiment 1
Use the inventive method on pilot-plant, to produce C307 type catalyst (Research Institute of Nanjing Chemical Industry Group, methanol synthesis catalyst), adopting the flushing of shell and tube continuous filtration thickener to record the wet cake solid content is 29.3%, carry out spray-drying (0.9 millimeter, 1.2 millimeters of injection diameters) after the laggard pressure spray dryer of 60 mesh sieves, directly carry out spray-drying, the particle and the powder that obtain are used two-sided chain-plate type far-infrared dryer drying respectively, and the products obtained therefrom numbering is respectively 1
#(0.9 millimeter of spray orifice), 2
#(1.2 millimeters of spray orifices), 3
#(powder).Compare check respectively, test result such as table 1, table 2, table 3 behind the material same period (05B-4) the economy-combat sheet shaped article with this batch materials and old explained hereafter.Test result shows: compare 1 with the 05B-4 sample
#With 2
#The bulk density of sample is on average low by 20.6%, and intensity on average exceeds 30.0%, heat-resisting before, the active mean height 5.0% respectively in heat-resisting back, more than 11.1%, illustrate that the inventive method is better than traditional handicraft.
Table 1 physical data
Table 2 pore-size distribution
Table 3 activity data (methanol yield/gml
-1h
-1)
| Numbering | Before heat-resisting | After heat-resisting |
| 05B-4 | 1.31 | 1.04 |
| 1 # | 1.38 | 1.16 |
| 2 # | 1.37 | 1.15 |
Testing conditions: gas composition CO (13～15) %, CO
2(3～5) %, H
2(55～65) %, N
2Surplus; Pressure 5.0MPa; 230 ℃ of temperature, air speed 1.0 * 10
4h
-1
Heat-resisting condition: 350 ℃ of temperature; Pressure is normal pressure; 20h.
Embodiment 2
Adopt the inventive method on pilot-plant, to produce 39 tons of DH021 type dehydrogenations (Research Institute of Nanjing Chemical Industry Group production, cyclohexanone catalyst by cyclohexanol dehydrogenation), with the performance test results such as the table 4 of the DH021 type dehydrogenation of old explained hereafter.By data in the table as seen, guaranteeing that catalyst bulk density has descended 7～8% under conversion ratio, selectivity and the situation that radially catalyst important performance such as anti-crushing power is constant.
Table 4 the inventive method is produced DH021 type catalyst and external GC250 type catalyst performance contrast
| Process | Bulk density kg/L | Anti-crushing power N/cm radially | Cyclohexanol conversion ratio % | Cyclohexanone selectivity % |
| Old technology | 1.55 | 234 | 49.39 | 99.1 |
| Old technology | 1.61 | 205 | 48.61 | 99.2 |
| The inventive method (6 batches of mean value) | 1.46 | 253 | 53.36 | 99.15 |
Active testing conditions: catalyst loading amount: former granularity (Ф 6 * 3 two ends convex surfaces) 50ml; Reaction temperature: 230 ℃; Reaction pressure: normal pressure; Raw material liq air speed: 0.6h
-1
From top embodiment situation, first effect is to have alleviated labour intensity, has shortened the production cycle greatly when improving Catalyst Production serialization level of operation, makes plant capacity improve 50%; It two is that the improvement of washing process can be saved deionization hot water at least 30%, avoid because of running the material loss that material (old technology is inclined and washed the problem that often has) causes, the spray-dired in addition fine powder rate of recovery is very high, not only alleviated labour intensity than the rolling of old technology, prilling, material loss has also reduced, and the old explained hereafter cost that compares of new technology decreases in a word; The most significant effect then is to reduce catalyst bulk density, can produce the more catalyst of polytypic according to the different demands of user, improve product adaptability.
Claims (5)
1, a kind of is the production method of the catalyst of active component with copper zinc, comprise batching co-precipitation, semi-product material preparation, beat the sheet molding procedure, it is characterized in that the semi-product material preparation section in turn includes the following steps: the filtration of film circulation cleaning, spray drying granulation, far-infrared ray drying calcining.
2, the production method of catalyst according to claim 1 is characterized in that the material of film in the filtration of film circulation cleaning is polysulfones, polyester, Nomex, polytetrafluoroethylene (PTFE), inorganic ceramic material film or metal micro-holes film.。
3, the production method of catalyst according to claim 1 and 2 is characterized in that the film circulation cleaning filters employing shell and tube continuous filtration thickener.
4, the production method of catalyst according to claim 1 is characterized in that the far-infrared ray drying calcination process adopts two-sided chain-plate type far-infrared dryer.
5, the production method of catalyst according to claim 1, the atomizer that it is characterized in that spray drying device in the spray drying granulation operation are pneumatic atomizer or pressure atomizer or rotary atomizer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100978749A CN100556545C (en) | 2006-11-17 | 2006-11-17 | A kind of is the production method of the catalyst of active component with copper zinc |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100978749A CN100556545C (en) | 2006-11-17 | 2006-11-17 | A kind of is the production method of the catalyst of active component with copper zinc |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101185905A CN101185905A (en) | 2008-05-28 |
| CN100556545C true CN100556545C (en) | 2009-11-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102233283B (en) * | 2010-05-04 | 2014-03-12 | 四川蜀泰化工科技有限公司 | Process for producing copper series catalyst by using primary energy |
| CN102343288B (en) * | 2011-08-17 | 2013-07-17 | 中国石油化工集团公司 | Preparation method of methanol synthesis catalyst |
| CN105728062A (en) * | 2014-12-11 | 2016-07-06 | 中国石油化工股份有限公司 | Production method for copper-zinc catalyst |
| CN113083311A (en) * | 2019-12-23 | 2021-07-09 | 中石化南京化工研究院有限公司 | Method for preparing carbon monoxide low-change catalyst by far infrared ray roasting |
| CN113634288B (en) * | 2021-08-13 | 2022-06-07 | 中山大学 | Method for continuously synthesizing monatomic catalyst in batches |
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Address after: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee after: SINOPEC NANJING CHEMICAL RESEARCH INSTITUTE Co.,Ltd. Address before: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee before: Nanhua Group Research Institute |