CN202078904U - Device for preparing catalytic membrane - Google Patents
Device for preparing catalytic membrane Download PDFInfo
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- CN202078904U CN202078904U CN2011201436005U CN201120143600U CN202078904U CN 202078904 U CN202078904 U CN 202078904U CN 2011201436005 U CN2011201436005 U CN 2011201436005U CN 201120143600 U CN201120143600 U CN 201120143600U CN 202078904 U CN202078904 U CN 202078904U
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- membrane
- material liquid
- raw material
- catalytic
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- 239000012528 membrane Substances 0.000 title claims abstract description 120
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 87
- 239000007788 liquid Substances 0.000 claims abstract description 59
- 239000002994 raw material Substances 0.000 claims abstract description 50
- 238000007599 discharging Methods 0.000 claims description 30
- 230000008676 import Effects 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 230000002572 peristaltic effect Effects 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 abstract description 29
- 238000002360 preparation method Methods 0.000 abstract description 26
- 239000000243 solution Substances 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 11
- 238000006722 reduction reaction Methods 0.000 abstract description 10
- 239000003638 chemical reducing agent Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 108091006146 Channels Proteins 0.000 abstract 1
- 108090000862 Ion Channels Proteins 0.000 abstract 1
- 102000004310 Ion Channels Human genes 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 18
- 238000007598 dipping method Methods 0.000 description 17
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 16
- 239000008367 deionised water Substances 0.000 description 14
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 description 11
- 239000003054 catalyst Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 230000009467 reduction Effects 0.000 description 9
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 description 8
- 229910052763 palladium Inorganic materials 0.000 description 7
- 238000006555 catalytic reaction Methods 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 238000010531 catalytic reduction reaction Methods 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000011943 nanocatalyst Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 210000002808 connective tissue Anatomy 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 238000005470 impregnation Methods 0.000 description 3
- 238000011946 reduction process Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- OEHNVKBOQOXOJN-UHFFFAOYSA-N 2-(4-nitrophenyl)phenol Chemical compound OC1=CC=CC=C1C1=CC=C([N+]([O-])=O)C=C1 OEHNVKBOQOXOJN-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 230000001603 reducing effect Effects 0.000 description 2
- 238000009938 salting Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002457 bidirectional effect Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000002803 maceration Methods 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The utility model relates to a device of preparation catalytic membrane belongs to preparation catalytic membrane equipment technical field. The device consists of a membrane component, a pump and a raw material liquid tank. The method comprises the steps of preparing a catalytic membrane by using the device, fixing a ceramic membrane tube in a membrane assembly of the device, pumping a salt solution containing a catalytic active component into the membrane assembly of the device by a pump, enabling the solution to flow through membrane channels from the outer surface (or inner tube) of the ceramic membrane tube and enter the inner tube (or outer surface), enabling the active component to be attached to the surface and the channels of the membrane, and preparing the catalytic membrane by adopting chemical reduction. The utility model discloses the device of preparation catalytic membrane is simple, and operation process is simple and convenient, and the catalytic membrane performance of preparation is excellent.
Description
Technical field
The utility model relates to a kind of device for preparing catalytic membrane, belongs to preparation catalytic membrane equipment technical field.
Background technology
Chemical reaction is the core of chemical industry, and about 90% chemical process is relevant with catalytic reaction.Catalyst is the key and the core of catalysis technique, and the engineering and the technology of relevant catalysis played very important supporting role.Nanocatalyst shows excellent catalytic performance because its grain diameter is little, and specific area is big, blemish, causes people's extensive concern.
Nanocatalyst can be divided into suspended state and support type in the liquid-phase catalysis reaction.It is reported that the catalyst efficient of suspended state will be higher than loaded catalyst, but the problem that exists small catalyst particles to separate with the product difficulty.Catalyst not only causes catalyst loss if can not thoroughly separate with product, also influences product quality.For solving this type of problem, the researcher has designed and developed catalysis-ceramic membrane separation coupling technology.Patent CN02137865.7 discloses a kind of membrane separating method, can solve the difficult problem that nanocatalyst separates recovery in the heterogeneous suspension nano catalysis reaction effectively.But because nanocatalyst produces pollution on the absorption and the reaction pair film surface on film surface, cause catalytic efficiency to descend, membrane flux reduces, and then influences catalytic reaction.As if on the surface that catalyst activity component is supported on film or in the immersion fenestra, constitute catalytic membrane, the bottleneck problem that can avoid tiny catalyst to separate with product.
Catalytic membrane preparation normally loads on palladium, platinum, nickel isoreactivity component on the surface of film in (catalyst or be evenly distributed on the film or be attached on the perforated membrane supporter with the form of film with particle form) or the immersion fenestra by surface impregnation, ion-exchange, organometallic chemistry vapor deposition methods such as (MOCVD).Adopt the catalytic membrane of method for preparing, the catalyst basic load is in the film surface with high specific surface area, and is difficult to be attached to the film surface of low specific surface area or enter into fenestra.Desalination, 2002,144,411 reports adopt ion-exchange at asymmetric ceramic membrane (α-Al
2O
3Supporter, top layer γ-Al
2O
3, thickness 1.8 μ m) and preparation palladium catalytic membrane, palladium only is carried on γ-Al
2O
3, and α-Al
2O
3Non-loaded.
If the flow of solution of forcing to contain catalytic active component then can make active component be deposited in the duct through film surface and duct, increase the load capacity of catalyst in ceramic membrane surface and duct, promote the catalytic performance of catalytic membrane.
Summary of the invention
The purpose of this utility model is that a kind of device for preparing catalytic membrane is provided in order to improve the deficiencies in the prior art, the utility model is to force will contain the flow of solution of catalytic active component through film surface and duct in specific device, improve the load capacity of active component and the catalytic efficiency of catalytic membrane, and can use this device that the catalytic performance of catalytic membrane is characterized.
The technical solution of the utility model is: a kind of device for preparing catalytic membrane, by membrane module, pump and raw material liquid bath are formed: wherein membrane module is made up of interior pipe and outer tube, place ceramic-film tube in the interior pipe, and with sealing ring and upper cover, sealing ring and low head seal respectively, the downside of interior pipe and upside have charging aperture and discharging opening, the low head bottom has charging aperture, the upper cover top has discharging opening, the downside of outer tube and upside have water-bath or oil bath import and water-bath or oil bath import export, raw material liquid bath peripheral hardware has water-bath or oil bath insulation jacket, the downside of chuck and upside have water-bath or oil bath import and water-bath or oil bath outlet, raw material liquid bath top is provided with three holes, and raw material liquid bath downside is provided with raw material liquid bath discharging opening; Wherein: the water-bath of raw material liquid bath or oil bath outlet link to each other with the water-bath or the oil bath import of the downside of outer tube; The discharging opening of raw material liquid bath links to each other with pump, and pump connection traffic meter is divided into two branch roads afterwards: first branch road is connected with valve K, and valve K is connected with the charging aperture G of interior pipe, and upper cover discharging opening I is connected with the raw material liquid bath by valve L; Second branch road is connected with valve J, and valve J is connected with low head charging aperture F, and the discharging opening H of interior pipe is connected with the raw material liquid bath by valve M.
Above-mentioned material liquid trench bottom is provided with stirrer; Raw material liquid bath top is provided with three holes, and wherein the hole of the right and left is a feed cycle liquid mouth, and middle hole is used for the laying temperature meter.
The method of utilizing the utility model device to prepare catalytic membrane is: will contain the salting liquid circular flow of catalytic active component through ceramic membrane with pump, active component is adsorbed in ceramic-film tube surface and the duct, this process is the impregnation stage of ceramic-film tube, prepare catalytic membrane again behind reducing loaded active salt component in ceramic-film tube surface and duct, its concrete steps are:
A. at first valve K and L are opened, valve-off M and J, start pump, the catalytic active component salting liquid that is placed in the raw material liquid bath is squeezed into the annular space that interior pipe charging aperture G enters interior pipe and ceramic-film tube, flow through the then duct of ceramic-film tube enters into the interior pipe hollow part of ceramic-film tube, gets back in the raw material liquid bath by upper cover discharging opening I;
Perhaps be: at first open valve M and J, valve-off K and L, catalytic activity salt component solution enters into the interior pipe hollow part of ceramic-film tube by low head charging aperture F, flow through then the duct of ceramic-film tube enter in the annular space of pipe and ceramic membrane outer wall, get back in the raw material liquid bath by interior pipe discharging opening H;
B. press A. process identical operations step, circulate reductant solution, the reducing activity component is cleaned whole pipeline and catalytic membrane then with anhydrating.
Preferred above-mentioned pump adopts peristaltic pump or centrifugal pump charging, and by regulating the rotating speed control rate of flow of fluid of pump, wherein the discharging flow velocity is 0.01L/min～0.5L/min.Described ceramic-film tube is pellumina, zirconium oxide film, silicon oxide film or oxidation titanium film; The average pore size of ceramic-film tube is 2nm～10 μ m.
Preferred above-mentioned active salt component is nickel, palladium, platinum, rhodium or ruthenium, and its concentration is between 0.01mol/L～1mol/L.The dip time of preferred described impregnation stage is 1～100h; Dipping temperature is-20 ℃～100 ℃.Preferred described reductant solution is a hydrazine hydrate, and its concentration is between 0.01mol/L～1mol/L; The temperature of reductant solution is at-20 ℃～100 ℃; Recovery time is at 1～50h.Catalytic membrane washed with de-ionized water 1-10 time that preferred for preparation is good.
The catalytic membrane of the utility model preparation can adopt this device to carry out catalytic performance and characterize:
Take by weighing the 2.5g p-nitrophenol and add in the raw material liquid bath, add the 20ml absolute ethyl alcohol,, add the 480ml deionized water again, be configured to the p-nitrophenyl phenol solution of 500ml with the magnetic stirrer dissolving.Take by weighing the 2.0g sodium borohydride, join in the p-nitrophenyl phenol solution, treat that not having gas substantially emits after, open valve K, L valve-off J, M, start peristaltic pump, material liquid is by interior pipe charging aperture G, pipe hollow part in the catalytic membrane of flowing through duct enters, I flows back to the raw material liquid bath by the upper cover discharging opening.In reaction, by the content of real time sample monitoring p-nitrophenol, entire reaction was carried out 60 minutes altogether, and preceding 20 minutes every sampling in 5 minutes once, and back 40 minutes every sampling in 10 minutes once.By content of p-nitrophenol in the high performance liquid chromatography test sample, calculate its conversion ratio and estimate the catalytic membrane performance.
Beneficial effect:
1. the utility model adopts compulsory measure circulation maceration extract, compare with the dipping method of routine overcome steeping liq since the surface tension in ceramic membrane duct may not permeation ceramic membrane defective, the active salt component can be carried in the fenestra road.
2. preparation catalytic membrane device of the present utility model is practical, and the ceramic membrane that can adopt different structure is that supporter prepares catalytic membrane, as symmetric membrane, adventitia or inner membrance.
Description of drawings
Fig. 1 is preparation catalytic membrane device schematic diagram; 1-stirrer wherein, 2-raw material liquid bath, 3-insulation jacket, 4-thermometer, pipe in the 5-ceramic-film tube, 6-, 7-outer tube, 8-upper cover, 9-sealing ring, 10-membrane module, 11-sealing ring, 12-flowmeter, 13-low head, 14-peristaltic pump; Water-bath of A-insulation jacket or oil bath import, water-bath of B-insulation jacket or oil bath outlet, water-bath of C-membrane module or oil bath import, water-bath of D-membrane module or oil bath outlet, the outlet of E-raw material liquid bath, F-low head charging aperture, I-upper cover discharging opening, G-membrane module charging aperture, H-membrane module discharging opening, K, J, L, M-valve
The specific embodiment
Embodiment 1: the device of preparation catalytic membrane
Shown in figure (1), this device is mainly by membrane module 10, pump 14 and raw material liquid bath 2 are formed: wherein membrane module 10 is made up of interior pipe 6 and outer tube 7, place ceramic-film tubes 5 in the interior pipe 6, and with sealing ring 9 and upper cover 8, sealing ring 11 seals respectively with low head 13, the downside and the upside of interior pipe 6 have charging aperture G and discharging opening H, low head 13 bottoms have charging aperture F, upper cover 8 tops have discharging opening I, the downside of outer tube 7 and upside have water-bath or oil bath import C and water-bath or oil bath import export D, raw material liquid bath 2 outer water-bath or the oil bath insulation jacket 3 of being provided with, the downside of chuck and upside have water-bath or oil bath import A and water-bath or oil bath outlet B, raw material liquid bath top is provided with three holes, and raw material liquid bath downside is provided with raw material liquid bath discharging opening E; Wherein: the water-bath of raw material liquid bath or oil bath outlet B link to each other with the water-bath or the oil bath import C of the downside of outer tube 7; The discharging opening E of raw material liquid bath links to each other with pump 14, and pump 14 connection traffic meters 12 are divided into two branch roads afterwards: first branch road is connected with valve K, and valve K is connected with the charging aperture G of interior pipe, and upper cover discharging opening I is connected with the raw material liquid bath by valve L; Second branch road is connected with valve J, and valve J is connected with low head charging aperture F, and the discharging opening H of interior pipe 6 is connected with the raw material liquid bath by valve M.
The raw material liquid bath adopts special glass container, this glass container external diameter 13cm, and wall thickness 0.7cm, high 15cm has three circular ports on the top seal cover, and wherein the hole of the right and left is used for feed cycle liquid, and middle hole is used for the laying temperature meter.The lower right of glass container has the discharging opening that external diameter is 9mm, the outside of whole glass container is provided with an insulation jacket, the annular space of this insulation jacket and glass container is 1cm, and it is 8mm that the lower left of this chuck and upper right side have external diameter, and internal diameter is water-bath import and the outlet of 5mm.
Membrane module adopts stainless steel to make, and whole membrane module is long to be 18cm, and the external diameter of outer tube is 28mm, and internal diameter is 27mm, and the external diameter of interior pipe is 14mm, and internal diameter is 13mm, and the outer wall spacing of the inwall of outer tube and interior pipe is 7mm.The charging aperture on interior pipe and the last low head and the external diameter of discharging opening are 12mm, and internal diameter is 9mm, and the water-bath import of outer tube and outlet external diameter are 8mm, and internal diameter is 5mm.Membrane module has two end sockets up and down.
In this device, BT00-100M type peristaltic pump is adopted in charging, the pump driver adopts YZ1515X, the agitating device of raw material liquid bath adopts 79-2 bidirectional magnetic force heating stirrer, constant temperature water bath adopts the thermostatic water-circulator bath groove, and all pipelines connect the corrosion resistant NORPRENE Chemical pipe connection of all adopting external import.
Embodiment 2:Pd/Al
2O
3The preparation of catalytic membrane
(length 18cm, external diameter are 12mm, and wall thickness is 2mm, symmetric membrane, materials A l with deionized water cleaning ceramic film pipe before the experiment
2O
3, membrane aperture 3 μ m), airing is standby.
(1) dipping: palladium/acetone soln of configuration 150mL 0.02mol/L is in the raw material liquid bath, ceramic-film tube is put in the interior pipe 6 of membrane module 10 fixing, make by pump 14 among the annular space of interior pipe 6 that dipping solution squeezes into membrane module and ceramic-film tube 5, in the outer surface passing hole channel inflow ceramic membrane of ceramic membrane, manage the hollow part, and return raw material liquid bath 2 through upper cover discharging opening I, the palladium active component is attached in film surface and the duct, and dipping carries out 18h, 0 ℃ of control temperature.
(2) reduction: the hydrazine hydrate solution of configuration 150mL 0.1mol/L, solvent adopts deionized water, reduces according to above-mentioned identical operations, and the control reduction temperature is that 0 ℃, recovery time are 4h.The catalytic ceramics film that taking-up prepares spends deionised water 4 times, dries stand-by naturally.
The catalytic membrane for preparing is numbered A
Adopt the identical raw material with preparation catalytic membrane A, ceramic membrane is statically placed in the test tube in dipping, the reduction process, does not use forced flow, and the preparation catalytic membrane is numbered B.
Catalytic membrane A, the B for preparing is used for the catalytic reduction p-nitrophenol prepares the para-aminophenol test, adopt the content of p-nitrophenol in the timing sampling analysis material liquid, calculate the catalytic performance that its conversion ratio is estimated catalytic membrane, its result is as shown in the table.Can find that the catalytic performance of catalytic membrane A obviously is better than catalytic membrane B, illustrate that device and method of the present utility model can prepare the catalytic membrane of excellent performance.
Embodiment 3:Pd/ZrO
2The preparation of catalytic membrane
(length 18cm, external diameter are 12mm, and wall thickness is 2mm, adventitia, film material ZrO with deionized water cleaning ceramic film pipe before the experiment
2, membrane aperture 200nm), airing is standby.
(1) dipping: palladium/acetone soln of preparation 150mL 0.01mol/L is in the raw material liquid bath, ceramic-film tube is put in the interior pipe of membrane module fixing, by pump dipping solution is squeezed among the annular space of the interior pipe of membrane module and ceramic-film tube, and in the outer surface passing hole channel inflow ceramic membrane of ceramic membrane, manage the hollow part, I returns the raw material liquid bath from the upper cover discharging opening, dipping carries out 6h, 20 ℃ of control temperature.
(2) reduction: the hydrazine hydrate solution of configuration 150mL 0.08mol/L, solvent adopts deionized water, reduces according to above-mentioned identical operations, and the control reduction temperature is that 10 ℃, recovery time are 2h.The catalytic ceramics film that taking-up prepares spends deionised water 8 times, dries stand-by naturally.
The catalytic membrane for preparing is numbered C
Adopt the identical raw material with preparation catalytic membrane C, ceramic membrane is statically placed in the test tube in dipping, the reduction process, does not use forced flow, and the preparation catalytic membrane is numbered D.
Catalytic membrane C, the D for preparing is used for the catalytic reduction p-nitrophenol prepares the para-aminophenol test, the conversion ratio that adopts real time sample to analyze the p-nitrophenol in the material liquid is estimated the catalytic performance of catalytic membrane.Its result is as shown in the table.Can find that the catalytic performance of catalytic membrane C obviously is better than catalytic membrane D.
Embodiment 4:Ni/Al
2O
3The preparation of catalytic membrane
(length 18cm, external diameter are 12mm, and wall thickness is 2mm, symmetric membrane, materials A l with deionized water cleaning ceramic film pipe before the experiment
2O
3, membrane aperture 3 μ m), airing is standby.
(1) dipping: nickel nitrate/aqueous solution of preparation 150mL 0.1mol/L is in the raw material liquid bath, ceramic-film tube is put in the interior pipe of membrane module fixing, by pump dipping solution is squeezed in the membrane module ceramic membrane and managed the hollow part, flow into the annular space of interior pipe and ceramic membrane from the interior pipe hollow part passing hole channel of ceramic-film tube, discharging opening H by interior pipe returns the raw material liquid bath, the nickel active component is attached in film surface and the duct, and dipping carries out 60h, 30 ℃ of control temperature.
(2) reduction: the hydrazine hydrate solution of configuration 150mL 0.6mol/L, solvent adopts deionized water, reduces according to above-mentioned identical operations, and the control reduction temperature is that 20 ℃, recovery time are 30h.The catalytic ceramics film that taking-up prepares spends deionised water 6 times, dries stand-by naturally.
(3) catalytic membrane is numbered E
Adopt the identical raw material with preparation catalytic membrane E, ceramic membrane is statically placed in the test tube in dipping, the reduction process, does not use forced flow, and the preparation catalytic membrane is numbered F.
Catalytic membrane E, the F for preparing is used for the catalytic reduction p-nitrophenol prepares the para-aminophenol test, the conversion ratio that adopts real time sample to analyze the p-nitrophenol in the material liquid is estimated the catalytic performance of catalytic membrane.Its result is as shown in the table.Can find that the catalytic performance of catalytic membrane E obviously is better than catalytic membrane F.
Embodiment 5:Ni/ZrO
2The preparation of catalytic membrane
(length 18cm, external diameter are 12mm, and wall thickness is 2mm, adventitia, film material ZrO with deionized water cleaning ceramic film pipe before the experiment
2, membrane aperture 200nm), airing is standby.
(1) dipping: nickel nitrate/aqueous solution of preparation 150mL 0.04mol/L is in the raw material liquid bath, ceramic-film tube is put in the interior pipe of membrane module fixing, by pump dipping solution is squeezed in the membrane module ceramic membrane and managed the hollow part, flow into the annular space of interior pipe and ceramic membrane from the interior pipe hollow part passing hole channel of ceramic-film tube, discharging opening H by interior pipe returns the raw material liquid bath, the nickel active component is attached in film surface and the duct, and dipping carries out 12h, 40 ℃ of control temperature.
(2) reduction: the hydrazine hydrate solution of configuration 150mL 0.4mol/L, solvent adopts deionized water, reduces according to above-mentioned identical operations, and the control reduction temperature is that 30 ℃, recovery time are 20h.。The catalytic ceramics film that taking-up prepares spends deionised water 8 times, dries stand-by naturally.
The catalytic membrane for preparing is numbered G
Comparative Examples adopts the catalytic membrane of conventional immersion reduction method preparation to be numbered H.
Catalytic membrane G, the H for preparing is used for the catalytic reduction p-nitrophenol prepares the para-aminophenol test, the conversion ratio that adopts real time sample to analyze the p-nitrophenol in the material liquid is estimated the catalytic performance of catalytic membrane.Its result is as shown in the table.Can find that the catalytic performance of catalytic membrane G obviously is better than catalytic membrane H.
Claims (3)
1. device for preparing catalytic membrane, by membrane module (10), pump (14) and raw material liquid bath (2) are formed: wherein membrane module (10) is made up of interior pipe (6) and outer tube (7), place ceramic-film tube (5) in the interior pipe (6), and with sealing ring (9) and upper cover (8), sealing ring (11) seals respectively with low head (13), the downside and the upside of interior pipe (6) have charging aperture (G) and discharging opening (H), low head (13) bottom has charging aperture (F), upper cover (8) top has discharging opening (I), the downside of outer tube (7) and upside have water-bath or oil bath import (C) and water-bath or oil bath import export (D), outer water-bath or the oil bath insulation jacket (3) of being provided with of raw material liquid bath (2), the downside of chuck and upside have water-bath or oil bath import (A) and water-bath or oil bath outlet (B), raw material liquid bath top is provided with three holes, and raw material liquid bath downside is provided with raw material liquid bath discharging opening (E); Wherein: the water-bath of raw material liquid bath or oil bath outlet (B) link to each other with the water-bath or the oil bath import (C) of the downside of outer tube (7); The discharging opening of raw material liquid bath (E) links to each other with pump (14), pump (14) connection traffic meter (12), be divided into two branch roads afterwards: first branch road is connected with valve (K), and valve (K) is connected with the charging aperture (G) of interior pipe, and upper cover discharging opening (I) is connected with the raw material liquid bath by valve (L); Second branch road is connected with valve (J), and valve (J) is connected with low head charging aperture (F), and the discharging opening (H) of interior pipe (6) is connected with the raw material liquid bath by valve (M).
2. device according to claim 1 is characterized in that described pump (14) is peristaltic pump or centrifugal pump.
3. device according to claim 1 is characterized in that described material liquid trench bottom is provided with stirrer (1); Raw material liquid bath top is provided with three holes, and wherein the hole of the right and left is a feed cycle liquid mouth, and middle hole is used for laying temperature meter (4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011201436005U CN202078904U (en) | 2011-05-09 | 2011-05-09 | Device for preparing catalytic membrane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011201436005U CN202078904U (en) | 2011-05-09 | 2011-05-09 | Device for preparing catalytic membrane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN202078904U true CN202078904U (en) | 2011-12-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011201436005U Expired - Lifetime CN202078904U (en) | 2011-05-09 | 2011-05-09 | Device for preparing catalytic membrane |
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| Country | Link |
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| CN (1) | CN202078904U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102274757A (en) * | 2011-05-09 | 2011-12-14 | 南京工业大学 | Device and method for preparing catalytic membrane |
-
2011
- 2011-05-09 CN CN2011201436005U patent/CN202078904U/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102274757A (en) * | 2011-05-09 | 2011-12-14 | 南京工业大学 | Device and method for preparing catalytic membrane |
| CN102274757B (en) * | 2011-05-09 | 2013-10-30 | 南京工业大学 | Device and method for preparing catalytic membrane |
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