CN1394672A - Catalyst membrane separation method for heterogeneous suspension nano catalysis reaction - Google Patents
Catalyst membrane separation method for heterogeneous suspension nano catalysis reaction Download PDFInfo
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- CN1394672A CN1394672A CN 02137865 CN02137865A CN1394672A CN 1394672 A CN1394672 A CN 1394672A CN 02137865 CN02137865 CN 02137865 CN 02137865 A CN02137865 A CN 02137865A CN 1394672 A CN1394672 A CN 1394672A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 43
- 238000000926 separation method Methods 0.000 title claims abstract description 34
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 33
- 239000012528 membrane Substances 0.000 title claims abstract description 26
- 239000000725 suspension Substances 0.000 title claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 title claims description 23
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000007791 liquid phase Substances 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 11
- 239000011148 porous material Substances 0.000 claims abstract description 5
- 238000005086 pumping Methods 0.000 claims abstract description 4
- 239000011943 nanocatalyst Substances 0.000 claims description 35
- 239000007790 solid phase Substances 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 230000004044 response Effects 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims 1
- 238000007873 sieving Methods 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 description 6
- 238000011160 research Methods 0.000 description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 239000008187 granular material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 240000004859 Gamochaeta purpurea Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000009295 crossflow filtration Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011118 depth filtration Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
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Abstract
The present invention relates toa catalyst membrane separatino method for heterogeneous suspension state nano catalytic reaction. The catalyst separation process and catalytic reaction process are coupled into same system, a pump is used for continuously pumping material in the reactor still and feeding said material into inorganic membrane tube whose average pore diameter is 2-200 nano, and making it continuously circulate between reactor still and inorganic membrane tube, so that the liquid phase product can be continuously penetrated through the membrane tube, and can be separated, and the suspension catalyst is trapped in the membrane tube, and can be returned into reactor still with circualting liquor and can be recovered.
Description
(one) technical field
The present invention relates to the catalyst membrane separation method of a kind of separation method of nanocatalyst, particularly heterogeneous suspension nano catalysis reaction.
(2) background technology field
Nanocatalyst is because its particle is small, and specific area is big, and key attitude and the surface atom coordination not congruent characteristic different with granule interior on surface caused the increase of surface-active position, thereby is a kind of novel effective catalyst, be called as the 4th generation catalyst.Because this catalyst particle size≤10
-7Rice, have very thin uniform outer surface layer and special crystal structure, the surface state of its atom level can cause the variation of surface electronic state, and this good surface characteristic and unique electronic structure help absorbing the carrying out of absorption and surface chemical reaction, thereby nanocatalyst has light specific gravity, specific area is big, the reactivity height, selectivity is strong, long service life, outstanding advantage such as good operation performance, these character provide good prospect for its application at catalytic field.This catalyst is applicable to various types of chemical reactions, especially catalytic oxidation, reduction and cracking reaction all had advantages of high catalytic activity and good catalytic selectivity, caused domestic and international chemistry, chemical industry expert's great attention, its application will have an immense impact on to chemical industry, field of petrochemical industry, becomes the important high-tech sector that each developed country, each big petrochemical corporation (complex) competitively develop.Many developed countries all drop into great amount of manpower, financial resources are carried out the research of nano particle as high performance catalyst.For example the Nano ST of the Nano center of the U.S., Japan all classifies the research of nanocatalyst as the focus development project, and some achievements in research or transform to the practical stage.The basis and the application study of nanocatalyst are carried out in the also organizational strength energetically of many scientific research institutions of China, institution of higher learning, and have obtained certain achievement.But, at present both at home and abroad the research of nanocatalyst is also mainly concentrated on the evaluation etc. of preparation, finishing, sign and the reactivity worth of nanocatalyst, the research that separates the aspect with product with the closely-related suspension nano catalyst of commercial Application then seldom.
In the liquid phase heterogeneous catalytic reaction, the use of catalyst often is divided into two kinds of forms: support type, floating type.Though the separation of loaded catalyst is reclaimed the problem ratio and is easier to solve, when tiny catalyst granules loaded on the carrier, its active sites can obviously reduce, and this will reduce activity of such catalysts inevitably.It is undisputable fact that the catalytic activity of suspended state catalyst is higher than loaded catalyst.But the use of suspended state catalyst will relate to the separation problem of catalyst and product inevitably.Particularly after the catalyst granules nanometer, use methods such as traditional flotation, gravitational settling, centrifugal sedimentation, cake filtration, in-depth filtration all can not effectively the suspension nano catalyst to be separated fully with liquid-phase product, add in addition to react under the harsh conditions such as high temperature, high pressure of being everlasting and carry out, what relate to often is organic or the corrosivity system, and this just makes nanocatalyst very difficult with separating of product.Nanocatalyst can not separate fully and will cause two problems with product: a large amount of losses of expensive nanocatalyst and nanocatalyst be to the influence of target product quality, and this also is the main cause that nanocatalyst so far can not large-scale industrial application.
Therefore, how effectively separating and reclaim nanocatalyst, is the key and problem anxious to be solved of efficiently using nanocatalyst and nanocatalyst large-scale industrial application veritably.
(three) summary of the invention
The catalyst membrane separation method that the purpose of this invention is to provide a kind of heterogeneous suspension nano catalysis reaction; it can thoroughly separate liquid phase material with the solid phase nanocatalyst of suspension from the material of heterogeneous suspension nano catalysis reaction; avoid catalyst particles to sneak in the product; guarantee product purity, solved the suspension nano catalyst and easily run off, be difficult to separate a difficult problem that reclaims and influence product purity.
The inventive method is made up of catalytic reaction and catalyst separation two parts, catalytic reaction adopts the fine catalyst of average grain diameter 1nm～100nm, has a kind of liquid phase material that is in the reactant at least, other reactant can be liquid phase or gas phase, reactant and nanocatalyst add reactor and are mixed into the heterogeneous suspension system, and process conditions are routinely reacted; The invention is characterized in that separation process and catalytic reaction process with catalyst are coupled in the same system, promptly it is sent into and pass through inorganic film tube continuously by the material in the direct continuous drawing reactor of pump, the average pore size of inoranic membrane is 2～200 nanometers, material is under the conveying of pump, continuously between reactor and inorganic film tube assembly, circulate, utilize the screening principle of inorganic separating film, the solid phase nanocatalyst is trapped in the film pipe and constantly circulates with recycle stock, in this process, liquid-phase product continuously sees through the inoranic membrane outflow system, and the catalyst suspension that does not see through continuously returns reactor, thereby realizes Separation of Solid and Liquid.
In the inventive method, catalytic reaction can be to adopt to react the intermittent mode that afterwards separates earlier with the film separation process, also can adopt the mode of carrying out continuously simultaneously.Batch (-type) is to carry out after material circulation separation process question response still internal reaction finishes.Suspension is continuous enrichment along with the separation of liquid phase, and the solid phase weight content reaches at 0.1～15% o'clock in recycle stream, and material is thick paste, and flowability obviously reduces, and causes pump to extract resistance when excessive, the separation process termination of pumping that finishes.Catalyst has been recovered in the reactor, participates in next catalytic reaction again; Continous way is that the separation process of catalyst and the charging of reactor are carried out simultaneously continuously, promptly carry out catalytic reaction to the reactor continuous feed on one side, extracting on one side the material film that circulates from still separates, continuous separated and collected liquid-phase product, simultaneously constantly isolated catalyst is returned reactor, continue to participate in catalytic reaction.This method is by regulating the mean residence time that film sees through the rate of outflow control material in reactor of liquid.Continuity method is applicable to generally and need growing quantity-produced occasion in one period that separation process stops with the end of catalytic process.
The said inoranic membrane of the inventive method can be selected pottery, metallic material film or their composite material film, for example can select for use by α-Al
2O
3For supporting the zirconia ceramics film of body.
In sum, the present invention will react with separating to be coupled in the same device and finish, adopt inorganic separating film high temperature resistant, high pressure resistant, corrosion-resistant, anti-organic system to reclaim nanocatalyst, by with the integrated nano catalysis reaction process of inoranic membrane, nanocatalyst is separated fully with product, with the recovery fully of assurance nanocatalyst and the purity of target product.The present invention has solved the difficult problem that nanocatalyst separates recovery in the heterogeneous suspension nano catalysis reaction effectively, and this efficient use and industrialization promotion to nanocatalyst has realistic meaning.
(four) description of drawings
Accompanying drawing is the catalyst film piece-rate system flow chart of heterogeneous suspension nano catalysis reaction of the present invention.
(five) specific embodiment
Batch (-type) catalyst inoranic membrane separation process embodiment below in conjunction with accompanying drawing technological process explanation heterogeneous suspension nano catalysis reaction.
As shown in drawings: 1 is source of the gas, can control the pressure of nano catalysis reaction by the pressure-reducing valve on the steel cylinder 1.Stirred tank 4 has automatic speed regulation temperature controller 5, and conduit 3 leads to the reactor bottom, so that the gas, liquid, solid three-phase fully contacts.2-2 is an exhaust-valve.Discharge nozzle 6 is at the bottommost of reactor 4.Product pump 7 is used for convey materials.8 is the inorganic separating film assembly, in this example, adopts by α-Al
2O
3For supporting the zirconia ceramics membrane module of body.The average pore size of used film is relevant with the required catalyst grain size that separates, and separating average grain diameter as need is that then can to adopt average pore size be the inoranic membrane of 50nm for the nanocatalyst of 20nm.Stop valve 2-7 is used to regulate the pressure of recoil steam.9 is the product jar, is used to collect liquid-phase product.
A certain proportion of raw material and nanocatalyst are added in the autoclave 4.Feed earlier 3 atmospheric unstripped gas, shut off valve 2-1, and open exhaust-valve 2-2, drain unstripped gas and air, the step 4 above repeating time.After treating that air displacement finishes, by regulating on the steel cylinder 1 pressure-reducing valve, the pressure in the autoclave 4 is kept within the specific limits, open automatic speed regulation temperature controller 5, regulate suitable temperature and rotating speed, heterogeneous suspension nano catalysis reaction is normally carried out in reactor 4.When the flowmeter P on the reactor 4 shows that gas flow is zero, illustrate that reaction finishes.After reaction finished, shut off valve 2-1 opened exhaust-valve 2-2, unnecessary gas in the reactor 4 of draining, and close this valve.Open valve 2-3, valve 2-4, valve 2-5, valve 2-6, the liquid phase material in the still and the mixture of solid phase nanocatalyst enter inorganic separating film assembly 8 by pipeline 6 and pump 7.By control valve 2-4, valve 2-5 and valve 2-6, inoranic membrane 8 is operated, under suitable operating pressure and cross-flow velocity so that cross-flow filtration can successfully carry out.After aforesaid operations was finished, system carried out the separation removal process of nanocatalyst automatically, and Partial Liquid Phase sees through permeable membrane and discharges and be collected into the product jar 9 from the film pipe outside, and the nanocatalyst tunicle of solid phase is held back and returned in the reactor with concentrate.Along with liquid-solid continuous separation, solid phase enrichment gradually in the recycle stream, when the solid content of nanocatalyst in the recycle stream reached 12% (weight), separation process was finished, at this moment, termination of pumping 7, shut off valve 2-3, valve 2-4, valve 2-5, valve 2-6 again.Solid phase nanocatalyst after concentrating has been got back in the autoclave 4, so that continue to use during secondary response down.In above-mentioned Separation of Solid and Liquid process, according to circumstances the instantaneous unlatching Pressure Steam Valve 2-7 in timing or not timing ground carries out the instantaneous high pressure recoil to membrane module, pollutes with phase shift films.
Claims (4)
1, the catalyst membrane separation method of heterogeneous suspension nano catalysis reaction, form by catalytic reaction and catalyst separation two parts, catalytic reaction adopts the fine catalyst of average grain diameter 1nm～100nm, has a kind of liquid phase material that is in the reactant at least, reactant and nanocatalyst add reactor and are mixed into the heterogeneous suspension system, and process conditions are routinely reacted; It is characterized in that the separation process and the catalytic reaction process of catalyst are coupled in the same system, it is sent into and pass through inorganic film tube continuously by the material in the direct continuous drawing reactor of pump, the average pore size of inoranic membrane is 2～200 nanometers, material is under the conveying of pump, continuously between reactor and inorganic film tube assembly, circulate, utilize the sieving actoion of inorganic separating film, the solid phase nanocatalyst is trapped in the film pipe and constantly circulates with recycle stock, in this process, liquid-phase product continuously sees through the inoranic membrane outflow system, and the catalyst suspension that does not see through continuously returns reactor, realizes Separation of Solid and Liquid.
2, the catalyst membrane separation method of heterogeneous suspension nano catalysis reaction according to claim 1, it is characterized in that catalytic reaction and film separation process are step, be to carry out after material circulation separation process question response still internal reaction finishes, recycle stock is continuous enrichment along with the separation of liquid phase, the solid phase weight content reaches termination of pumping in 0.1～15% o'clock in recycle stock, separation finishes, and the catalyst that returns reactor participates in next catalytic reaction again.
3, the catalyst membrane separation method of heterogeneous suspension nano catalysis reaction according to claim 1, the separation process and the nano catalysis reaction in the reactor that it is characterized in that catalyst carry out simultaneously continuously, promptly carry out catalytic reaction to the reactor continuous feed on one side, extracting on one side the material film that circulates from still separates, continuous separated and collected liquid-phase product, simultaneously constantly isolated catalyst is returned reactor, continue to participate in catalytic reaction.
4,, it is characterized in that said inoranic membrane is pottery, metal or its composite material film according to the catalyst membrane separation method of claim 1 or 2 or 3 described heterogeneous suspension nano catalysis reactions.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021378657A CN1164355C (en) | 2002-07-01 | 2002-07-01 | Catalyst membrane separation method for heterogeneous suspension nano catalysis reaction |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021378657A CN1164355C (en) | 2002-07-01 | 2002-07-01 | Catalyst membrane separation method for heterogeneous suspension nano catalysis reaction |
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| Publication Number | Publication Date |
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| CN1394672A true CN1394672A (en) | 2003-02-05 |
| CN1164355C CN1164355C (en) | 2004-09-01 |
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|---|---|---|---|
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102151520A (en) * | 2010-12-21 | 2011-08-17 | 湘潭大学 | Gas-liquid-solid or liquid-solid heterogeneous catalytic reaction method |
| CN101348565B (en) * | 2008-05-30 | 2012-01-11 | 中化国际（苏州）新材料研发有限公司 | Purification process of oligo-ether containing heteropoly acid |
| CN102757305A (en) * | 2011-04-29 | 2012-10-31 | 岳阳昌德化工实业有限公司 | Method of oxidizing cyclohexane |
| CN102757303A (en) * | 2011-04-29 | 2012-10-31 | 岳阳昌德化工实业有限公司 | Method of oxidizing cyclohexane |
| CN102755862A (en) * | 2011-04-29 | 2012-10-31 | 岳阳昌德化工实业有限公司 | Equipment for oxidizing cyclohexane |
| WO2012146146A1 (en) * | 2011-04-29 | 2012-11-01 | 岳阳昌德化工实业有限公司 | Apparatus and method for oxidization of cyclohexane |
| CN104096388A (en) * | 2014-07-28 | 2014-10-15 | 湘潭大学 | Method used for directly separating catalyst from solid-liquid phase reacting system |
| US9555374B2 (en) | 2009-04-29 | 2017-01-31 | Basf Se | Method for conditioning catalysts by means of membrane filtration |
| CN110756120A (en) * | 2018-07-27 | 2020-02-07 | 上海凯鑫分离技术股份有限公司 | Continuous hydrogenation reaction device and reaction process |
-
2002
- 2002-07-01 CN CNB021378657A patent/CN1164355C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101348565B (en) * | 2008-05-30 | 2012-01-11 | 中化国际（苏州）新材料研发有限公司 | Purification process of oligo-ether containing heteropoly acid |
| US9555374B2 (en) | 2009-04-29 | 2017-01-31 | Basf Se | Method for conditioning catalysts by means of membrane filtration |
| CN102151520A (en) * | 2010-12-21 | 2011-08-17 | 湘潭大学 | Gas-liquid-solid or liquid-solid heterogeneous catalytic reaction method |
| CN102757305A (en) * | 2011-04-29 | 2012-10-31 | 岳阳昌德化工实业有限公司 | Method of oxidizing cyclohexane |
| CN102757303A (en) * | 2011-04-29 | 2012-10-31 | 岳阳昌德化工实业有限公司 | Method of oxidizing cyclohexane |
| CN102755862A (en) * | 2011-04-29 | 2012-10-31 | 岳阳昌德化工实业有限公司 | Equipment for oxidizing cyclohexane |
| WO2012146146A1 (en) * | 2011-04-29 | 2012-11-01 | 岳阳昌德化工实业有限公司 | Apparatus and method for oxidization of cyclohexane |
| CN104096388A (en) * | 2014-07-28 | 2014-10-15 | 湘潭大学 | Method used for directly separating catalyst from solid-liquid phase reacting system |
| CN104096388B (en) * | 2014-07-28 | 2015-11-04 | 湘潭大学 | A kind of method of direct separating catalyst from solid-liquid phase reaction system |
| CN110756120A (en) * | 2018-07-27 | 2020-02-07 | 上海凯鑫分离技术股份有限公司 | Continuous hydrogenation reaction device and reaction process |
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|---|---|
| CN1164355C (en) | 2004-09-01 |
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Owner name: JIANGSU JIUWU HIGH SCIENCE & TECHNOLOY CO., LTD. Free format text: FORMER OWNER: NANJING POLYTECHNIC UNIV. Effective date: 20080808 |
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