CN105233883A - Vacuum coater used for loading porous ceramics material surface with photocatalysis membrane and method - Google Patents

Vacuum coater used for loading porous ceramics material surface with photocatalysis membrane and method Download PDF

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Publication number
CN105233883A
CN105233883A CN201510588362.1A CN201510588362A CN105233883A CN 105233883 A CN105233883 A CN 105233883A CN 201510588362 A CN201510588362 A CN 201510588362A CN 105233883 A CN105233883 A CN 105233883A
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China
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tank body
fluid reservoir
reacting tank
pipe
valve
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CN201510588362.1A
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王沛芳
饶磊
王超
侯俊
钱进
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Hohai University HHU
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Hohai University HHU
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Abstract

The invention discloses a vacuum coater used for loading a porous ceramics material surface with a photocatalysis membrane and a method. The apparatus comprises a reaction tank body, a liquid storage tank, a liquid elevating pipe, a vacuum pumping pipe, a quartz exhaust pipe, a drying air-inlet pipe, a forcing pipe and a bracing frame. The advantages comprise that 1) a plating liquid can effectively penetrate into all open pores, and prepared porous ceramics possesses relatively high film covering rate; 2) the thickness uniformity of the coated film in the pore of the porous ceramics is guaranteed, and also the apparatus is applicable to porous ceramic substrates with different pore diameter and porosity; 3) the apparatus helps to improve the thickness of the substrate surface loaded film and the film adhesion strength, and possesses relatively high production efficiency; 4) the apparatus is beneficial for improving the composition uniformity of the plating liquid, and further helping to obtain a coated layer with uniform compositions on the porous ceramics substrate surface; and 5) the apparatus is simple in structure, convenient to operate and suitable for large-scale production.

Description

For porous ceramic film material area load photocatalysis membrana vacuum coater and method
Technical field
What the present invention relates to is a kind of vacuum coater for porous ceramic film material area load photocatalysis membrana and method, belongs to composite formed technical field.
Background technology
In recent years, because enterprise's production technology falls behind, managerial skills are lower and supplies consumption is high, cause the pollutant discharge amount of unit product too high; Urban population growth excessive velocities simultaneously, industry is concentrated, and the development speed of municipal sewage system and sewage treatment facility is very slow.These are main, odjective cause makes the water environment of China in continuous deterioration.The water pollutions that traditional pollutant (COD, BOD), eutrophication composition and all kinds of toxic chemical substance cause all is increasing year by year, the urban waters of current China more than 90% is seriously polluted, the water source, key cities of nearly 50% does not meet drinking water standard, and environmental pollution improvement has become modern society and faced and one of major issue urgently to be resolved hurrily.Therefore, researcher is seeking efficient, eco-friendly pollutant treatment technology always and is threatening with response environment.
Photocatalysis technology is that the one found the seventies in last century is efficient, clean, pollutant treatment technology thoroughly, has developed the multiple semi-conducting material with photocatalytic effect at present, wherein nano-TiO 2powder has high, the fast light burn into of chemical stability and is insoluble in the advantage such as water and nontoxicity, and the compound that in water body, some are difficult to degrade, under light radiation condition, can pass through TiO 2photocatalysis be degraded to H 2o and CO 2, therefore TiO 2nano powder photocatalyst edman degradation Edman is a kind of water treatment new technology having application prospect.Load method is by TiO 2nanometer powder is fixed on a certain carrier prepares supported titanium 2catalysis material, this material solid-liquor separation in water treatment is comparatively easy, reuses more for convenience.In order to improve the contact area of catalytic membrane material and sewage, carrier many employings porous material, as silica gel, zeolite, glass fibre, porous ceramics etc.Wherein porous ceramics be a kind of in Prof. Du Yucang, body containing communicating with each other in a large number or the ceramic material of closed pore, because it has, specific area is large, be shaped convenient, the advantage such as cost is low, pollution-free, is a kind of widely used environmental protection carrier.
The film plating process generally adopted at present has dip-coating method, direct spraying method etc., due to the three-dimensional porous structure that porous ceramic film material has, and aperture is less, adopt above method plating solution can only be coated in the skin of porous ceramic bodies, and cannot penetrate in the hole of ceramic body, thus cause can only in the outer load of porous ceramics nano-TiO 2film, and inside does not have, this just reduces this kind of supported titanium greatly 2effective usable floor area of catalysis material, especially for the porous ceramic filler block that volume is larger, its nano-TiO 2the load area of film is lower, and this also hinders porous ceramic matrix nano-TiO greatly 2promoting the use of of catalysis material.Therefore develop a kind of apparatus and method being applicable to porous ceramic film material area load photocatalysis membrana, prepare the porous ceramics catalysis material with higher film coverage rate, to photocatalysis technology applying in water environment treatment, there is positive meaning.
Summary of the invention
The present invention proposes a kind of vacuum coater for porous ceramic film material area load photocatalysis membrana and method, its object is intended to prepared porous ceramic matrix nano-photocatalyst material and has that loaded film thickness is even, coverage rate is high, in conjunction with the advantage such as firm, be applicable to the surrounding purifying materials such as large-scale production porous ceramic matrix nano-photo catalytic filling block.
Technical solution of the present invention: for the vacuum coater of porous ceramic film material area load photocatalysis membrana, its structure comprises retort device, fluid reservoir, stalk, vacuum exhaust pipe, quartzy blast pipe, dries air inlet pipe, forcing pipe and bracing or strutting arrangement.Described retort is hollow vessel, is fixed on bracing frame; The epicoele cross section of retort is square, and cavity of resorption is infundibulate, and its top is provided with end cap and tank body can be sealed, and bottom is connected with stalk; Reacting tank body inside is provided with liner plate, and porous ceramics block is fixed between two blocks of liner plates; Described vacuum exhaust pipe and quartzy blast pipe are installed on end cap top; Described oven dry air inlet pipe is installed on retort cavity of resorption sidewall; Described fluid reservoir is cylindrical enclosure tank body, is installed on below retort, and plating solution is stored in tank, and stalk is inserted in tank by fluid reservoir top through hole, and fluid reservoir top is also provided with feed tube and forcing pipe, and bottom is provided with discharging tube.
The present invention has following beneficial effect:
1) plating solution slowly infiltrates through in porous ceramics block under vacuum, ceramic block endoporus is negative pressure state, and the penetrating power of plating solution is strong, and without gas block effect in hole, plating solution can effectively penetrate in all opening holes, and prepared porous ceramics has higher film coverage rate;
2) plating solution passes through stalk under malleation acting in conjunction in negative pressure of vacuum and fluid reservoir, from bottom to top be drawn in retort, liquid level rises steadily, plating solution can be made with suitable flow velocity by porous ceramics block by the positive pressure pressure in adjustment fluid reservoir, the uniformity of porous ceramics inner bore coating film thickness can be ensured, be also applicable to the porous ceramic matrices suitable with different pore size and porosity simultaneously;
3) the present invention can carry out plating and dry the alternate cycles of two processes and operate, thus realization is plated the multi-pass of porous ceramic film material, with the adhesive strength of the thickness and film that improve matrix surface loaded film, has higher production efficiency;
4) the present invention in the course of the work, and plating solution is in flow regime always, is conducive to the uniformity improving composition in plating solution, thus obtains the coating of uniform composition in porous ceramic matrix surface;
5) originally put structure simple, easy to operate, be suitable for producing in enormous quantities.
Accompanying drawing explanation
Accompanying drawing 1 is the front view inhaling plating appts for porous ceramic film material area load photocatalysis membrana vacuum;
Accompanying drawing 2 is left views of Fig. 1;
Accompanying drawing 3 is liner plate schematic diagrames.
In figure 1 is bracing frame, 2, and are end caps, 3 are vacuum exhaust pipes, 4 are epicoeles, 5 are quartzy blast pipes, 6 are silica gel sealing rings, 7 are sealing bolts, 8 are reacting tank bodies, 9 are limit ribs, 10 are liner plates, 11 are cavity of resorptions, 12 are forcing pipes, 13 are sealing rings, 14 are fluid reservoirs, 15 are plating solutions, 16 are stalks, 17 are bases, 18 to be feed tubes, 19 be that to dry air inlet pipe, 20 are porous ceramics blocks, 21 are discharging tubes, 22 are lining frames, 23 is lining nets.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, technical solution of the present invention is described in further detail.
As shown in drawings, for the vacuum coater of porous ceramic film material area load photocatalysis membrana, its structure comprises reacting tank body 8, fluid reservoir 14, stalk 16, vacuum exhaust pipe 3, quartzy blast pipe 5, dries air inlet pipe 19, forcing pipe 12 and bracing or strutting arrangement, wherein
Drying air inlet pipe 19 is fixed on the cavity of resorption sidewall of reacting tank body 8, dries air inlet pipe 19 one end and is communicated with reacting tank body 8, dries air inlet pipe 19 other end and is provided with valve, for being connected with hot-air pump;
Fluid reservoir 14 center offers through hole, for being connected with stalk 16; The upper end of described stalk 16 is by compact siro spinning technology bottom screw thread and reacting tank body 8, and the lower end of stalk 16 is inserted into fluid reservoir 14 inside by fluid reservoir 14 top through hole, and forcing pipe 12 is fixed at fluid reservoir 14 top,
Vacuum exhaust pipe 3, quartzy blast pipe 5 are fixed on end cap 2, and 2 ~ 3cm in one end intercalation reaction tank body 8 of vacuum exhaust pipe 3, quartzy blast pipe 5, the other end of vacuum exhaust pipe 3, quartzy blast pipe 5 is positioned at outside reacting tank body 8.
Described reacting tank body 8 is the stainless steel hollow vessel of a upper opening, and tank body epicoele cross section is square, and cavity of resorption is infundibulate, and reacting tank body 8 upper end open is provided with flange, and tank body thickness is 10mm.
The outer middle side part of described reacting tank body 8 is also provided with limit rib 9, and reacting tank body 8 can be vertically placed on bracing frame 1, and bracing frame 1 is connected with base 17;
Described end cap 2 is square corrosion resistant plate, and thickness is 15mm, and outside the flange of the length of side and reacting tank body 8 upper end, appearance is same; End cap 2 is fixed on the upper end of reacting tank body 8 by four sealing bolts 7, is also provided with silica gel sealing ring 6 between end cap 2 and reacting tank body 8;
Appearance etc. outside the interior length of side of described reacting tank body 8 and liner plate 10, liner plate 10 comprises lining frame 22 and lining net 23, and lining frame 22 be square-shaped frame, and wherein serve as a contrast net 23 and be fixed in the middle part of lining frame 22, employing 5 ~ 10 object stainless (steel) wires are made;
Described two blocks of liner plates 10 are secured by bolts in the epicoele 4 of reacting tank body 8, closely stack porous ceramics block 20 between two blocks of liner plates 10;
Vacuum exhaust pipe 3 end is provided with valve for connecting vacuum air pump;
Quartz blast pipe 5 end is provided with valve for controlling the discharge of reacting tank body 8 internal gas, and meanwhile, quartzy blast pipe is rising the effect also with level monitoring in liquid process.
Described fluid reservoir 14 of stating is for cylindrical enclosure tank body, and tank base is also connected with discharging tube 21.
Described stalk 16 is the stainless steel tube of an internal diameter 3 ~ 4cm, stalk 16 distance from bottom fluid reservoir 14 inner chamber bottom surface 3 ~ 5cm; Fluid reservoir 14 through hole position is also provided with sealing ring 13, to ensure the air-tightness that stalk 16 is connected with fluid reservoir 14.
Feed tube 18 is fixed at described fluid reservoir 14 top, and 2 ~ 3cm in fluid reservoir 14 is inserted in feed tube 18 one end, and feed tube 18 other end is positioned at outside fluid reservoir 14, and end is provided with valve; Feed tube 18 is for supplementing the plating solution in fluid reservoir 14.
Described forcing pipe 12 is fixed on fluid reservoir 14 top, for three-way pipeline, 2 ~ 3cm in fluid reservoir 14 is inserted in fluid reservoir 14 lower end, and fluid reservoir 14 one end is provided with air intake valve for connecting compressed air pump, and fluid reservoir 14 other end is provided with drain tap for letting out except the pressure in fluid reservoir 14.
Bottom described fluid reservoir 14, sidewall fixes discharging tube 21, discharging tube 21 one end is communicated with fluid reservoir 14, discharging tube 21 other end is provided with valve, and discharging tube 21 tube cavity lower limb distance fluid reservoir 14 inner chamber bottom surface 0 ~ 0.5cm, so that the plating solution 15 in fluid reservoir 14 is all discharged.
For porous ceramic film material area load photocatalysis membrana Vacuum Deposition electroplating method, comprise three phases: (1) preparatory stage: first prepare plating solution (component volume ratio is: tetraethyl titanate: ethanol: water: diethanol amine: acetic acid=1:4.5:2:0.6:0.02), close discharging tube 21 valve, join in fluid reservoir 14 by feed tube 18 by plating solution, plating solution liquid level is lower than fluid reservoir 14 top 5 ~ 10cm.By tightly packed for porous ceramics block 20 to be coated in the epicoele 4 of reacting tank body 8, and be fixed with two blocks of liner plates 10, with end cap 2 by sealing suitable for reading for reacting tank body 8;
(2) vacuum plating operation: close feed tube 18 valve, discharging tube 21 valve, the air intake valve of forcing pipe 12 and drain tap, dry air inlet pipe 18 valve and quartzy blast pipe 5 valve, open vacuum exhaust pipe 3 valve, vacuumize in reacting tank body 8, when in reacting tank body 8, vacuum reaches 0.1 ~ 0.2MPa, close vacuum exhaust pipe 3 valve, the air intake valve of slow unlatching forcing pipe 12, compressed air is introduced above the plating solution of fluid reservoir 14, under the negative pressure of plating solution 15 in retort 8 and the positive pressure in fluid reservoir 14, entered in reacting tank body 8 by stalk 16 and plating is carried out to porous ceramics block, the liquid level in reacting tank body 8 is monitored by quartzy blast pipe 5, when plating solution liquid level exceedes end cap 2, close the air intake valve of forcing pipe 12, plating solution liquid level will keep present level, leave standstill 5 ~ 10 minutes.Open the drain tap of forcing pipe 12 and blast pipe 5 valve, the plating solution in reacting tank body 8 will be flow back in fluid reservoir 14 by stalk 16, and leave standstill and within 30 minutes, be beneficial to the absorption of plating solution on ceramic matrix surface;
(3) drying operation: close feed tube 18 valve, discharging tube 21 valve, the air intake valve of forcing pipe 12 and drain tap and vacuum exhaust pipe 3 valve, open and dry air inlet pipe 18 valve and quartzy blast pipe 5 valve, the hot-air of 60 ~ 80 DEG C is blown in the cavity of resorption 11 of retort 8 by drying air inlet pipe 18, hot-air is by being discharged by quartzy blast pipe 5 after porous ceramics block, dry after 10 ~ 15 minutes and close oven dry air inlet pipe 18 valve and quartzy blast pipe 5 valve, leave standstill cooling 30 minutes.Repeat above-mentioned vacuum plating operation and drying operation 2 ~ 4 times, can complete the plated film work of porous ceramics block 20, unnecessary plating solution is discharged by discharging tube 21.Can obtain after the porous ceramics block 20 of plated film is taken out combine firmly, area load photocatalysis membrana porous ceramics catalysis material that coverage rate is higher.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.

Claims (7)

1. for a vacuum coater for porous ceramic film material area load photocatalysis membrana, it is characterized in that: comprise reacting tank body, fluid reservoir, stalk, vacuum exhaust pipe, quartzy blast pipe, dry air inlet pipe, forcing pipe and bracing frame; Wherein reacting tank body is hollow vessel, is fixed on bracing frame; The epicoele cross section of reacting tank body is square, and the cavity of resorption of reacting tank body is infundibulate, and reacting tank body top is provided with end cap for sealed shell of tank, is connected bottom reacting tank body with stalk; Reacting tank body inside is provided with liner plate, and porous ceramics block is fixed between two blocks of liner plates; Described vacuum exhaust pipe and quartzy blast pipe are installed on end cap top; Described oven dry air inlet pipe is installed on reacting tank body cavity of resorption sidewall; Described fluid reservoir is cylindrical enclosure tank body, is installed on below retort, and plating solution is stored in tank, and stalk is inserted in tank by fluid reservoir top through hole, and fluid reservoir top is also provided with feed tube and forcing pipe, and bottom is provided with discharging tube.
2. a kind of vacuum coater for porous ceramic film material area load photocatalysis membrana according to claim 1, it is characterized in that: described retort upper end open is provided with flange, end cap is fixed on the upper end of reacting tank body by four sealing bolts, is also provided with silica gel sealing ring between end cap and reacting tank body; The outer middle side part of reacting tank body is also provided with limit rib, and reacting tank body can be vertically placed on bracing frame.
3. a kind of vacuum coater for porous ceramic film material area load photocatalysis membrana according to claim 1, is characterized in that: described liner plate comprises lining frame and lining net, and lining frame is square-shaped frame, the inner edge appearance etc. of the outer length of side of lining frame and reacting tank body; Lining net is fixed in the middle part of lining frame, adopts 5 ~ 10 object stainless (steel) wires to make; Described two blocks of liner plates are secured by bolts in the epicoele of reacting tank body, and described porous ceramics block compact reactor is put between two blocks of liner plates.
4. a kind of vacuum coater for porous ceramic film material area load photocatalysis membrana according to claim 1, it is characterized in that: described fluid reservoir is cylindrical enclosure tank body, tank body top is connected with feed tube and forcing pipe, and center also offers through hole, for being connected with stalk; Tank base is also connected with discharging tube.
5. a kind of vacuum for porous ceramic film material area load photocatalysis membrana according to claim 1 inhales plating appts and method, it is characterized in that: described stalk is the stainless steel tube of an internal diameter 3 ~ 4cm, stalk upper end is by compact siro spinning technology bottom screw thread and reacting tank body, stalk lower end is inserted into fluid reservoir inside by the through hole at fluid reservoir top, stalk distance from bottom storage tank interior bottom surface 3 ~ 5cm; Fluid reservoir through hole position is also provided with sealing ring, to ensure stalk and the tank connected air-tightness of liquid storage.
6. a kind of vacuum coater for porous ceramic film material area load photocatalysis membrana according to claim 1 and method, it is characterized in that: described forcing pipe is fixed on fluid reservoir top, for three-way pipe, 2 ~ 3cm in fluid reservoir is inserted in forcing pipe lower end, forcing pipe one end is provided with air intake valve for connecting compressed air pump, and the forcing pipe other end is provided with drain tap for letting out except the pressure in fluid reservoir.
7. a kind of vacuum coating method for porous ceramic film material area load photocatalysis membrana as claimed in claim 1, is characterized in that being divided into three phases:
(1) preparatory stage: first prepare plating solution (component volume ratio is: tetraethyl titanate: ethanol: water: diethanol amine: acetic acid=1:4.5:2:0.6:0.02), close discharging tube valve, join in fluid reservoir by feed tube by plating solution, plating solution liquid level is lower than fluid reservoir top 5 ~ 10cm; By tightly packed for porous ceramics block to be coated in the epicoele of reacting tank body, and be fixed with two blocks of liner plates, with end cap by sealing suitable for reading for reacting tank body;
(2) vacuum plating operation: close feed tube valve, discharging tube valve, the air intake valve of forcing pipe and drain tap, dry air inlet pipe valve and quartzy exhaust valve, open vacuum suction tube valve, vacuumize in reacting tank body, when in reacting tank body, vacuum reaches 0.1 ~ 0.2MPa, close vacuum suction tube valve, the air intake valve of slow unlatching forcing pipe, compressed air is introduced above the plating solution of fluid reservoir, under the negative pressure of plating solution in reacting tank body and the positive pressure in fluid reservoir, entered in reacting tank body body by stalk and plating is carried out to porous ceramics block, by the liquid level in quartzy blast pipe monitoring reacting tank body, when plating solution liquid level exceedes end cap, close the air intake valve of forcing pipe, plating solution liquid level will keep present level, leave standstill 5 ~ 10 minutes, open the drain tap of forcing pipe and exhaust valve, the plating solution in reacting tank body will be flow back in fluid reservoir by stalk, and leave standstill and within 30 minutes, be beneficial to the absorption of plating solution on ceramic matrix surface,
(3) drying operation: close feed tube valve, discharging tube valve, the air intake valve of forcing pipe and drain tap and vacuum suction tube valve, open and dry air inlet pipe valve and quartzy exhaust valve, the hot-air of 60 ~ 80 DEG C is blown in the cavity of resorption of reacting tank body by drying air inlet pipe, hot-air is by being discharged by quartzy blast pipe after porous ceramics block, dry after 10 ~ 15 minutes and close oven dry air inlet pipe valve and quartzy exhaust valve, leave standstill cooling 30 minutes; Repeat above-mentioned vacuum plating operation and drying operation 2 ~ 4 times, can complete the plated film work of porous ceramics block, unnecessary plating solution is discharged by discharging tube; Can obtain after the porous ceramics block of plated film is taken out combine firmly, area load photocatalysis membrana porous ceramics catalysis material that coverage rate is high.
CN201510588362.1A 2015-09-16 2015-09-16 Vacuum coater used for loading porous ceramics material surface with photocatalysis membrane and method Pending CN105233883A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113564591A (en) * 2021-08-03 2021-10-29 江苏鹏举半导体设备技术有限公司 Porous gas flow distribution plate film coating system
CN114227882A (en) * 2021-12-29 2022-03-25 华中科技大学 Infiltration post-treatment device for large-size additive manufacturing ceramic blank

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6130661A (en) * 1984-07-19 1986-02-12 Matsushita Electric Ind Co Ltd Coating forming device
CN1660508A (en) * 2004-02-24 2005-08-31 中国科学院生态环境研究中心 Method and equipment for coating slurry layer on cellular carrier of ceramics

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6130661A (en) * 1984-07-19 1986-02-12 Matsushita Electric Ind Co Ltd Coating forming device
CN1660508A (en) * 2004-02-24 2005-08-31 中国科学院生态环境研究中心 Method and equipment for coating slurry layer on cellular carrier of ceramics

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113564591A (en) * 2021-08-03 2021-10-29 江苏鹏举半导体设备技术有限公司 Porous gas flow distribution plate film coating system
CN113564591B (en) * 2021-08-03 2022-08-09 江苏鹏举半导体设备技术有限公司 Porous gas flow distribution plate film coating system
CN114227882A (en) * 2021-12-29 2022-03-25 华中科技大学 Infiltration post-treatment device for large-size additive manufacturing ceramic blank

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Application publication date: 20160113