CN103752186B - A kind of preparation method of ceramic super-filtering film - Google Patents
A kind of preparation method of ceramic super-filtering film Download PDFInfo
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- CN103752186B CN103752186B CN201410036726.0A CN201410036726A CN103752186B CN 103752186 B CN103752186 B CN 103752186B CN 201410036726 A CN201410036726 A CN 201410036726A CN 103752186 B CN103752186 B CN 103752186B
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Abstract
The present invention relates to a kind of preparation method of ceramic super-filtering film, specifically the porous ceramics particulate selective laser sintering and moulding technology obtained through sol-gel, sintering, grinding is carried out rapid shaping, the ceramic super-filtering film of preparation difformity, stereochemical structure, thickness.This invention preparation method is simple, molding cycle is short, various shapes, practicality, the ceramic super-filtering film rejection obtained is large, and pore size distribution range 10-100nm, under the operating condition of 0.1Mpa, water flux is 100-200L/m
3h, is with a wide range of applications.
Description
Technical field
The present invention relates to a kind of UF membrane field, be specifically related to a kind of preparation method of ceramic super-filtering film.
Background technology
Milipore filter is a kind of for taking differential static pressure as motive force, carries out the membrane technology be separated according to the difference of relative molecular mass.The distinctive micropore of milipore filter can effectively detention bacterium, most of virus, colloid and mud, reaches separation, classification, purifying, concentrated object.Nowadays extensive use is obtained in industry and sphere of life, for separating of, concentrated, purifying biological goods, in pharmaceutical products and food industry, also for the terminal processes in blood treatment, desalinization, wastewater treatment, drink water purifying and ultra-pure water preparation.
Inorganic Ultrafiltration Membrane particularly inorganic ceramic ultra-filtering film owing to having, the advantage such as mechanical resistance is strong, high temperature resistant, corrosion-resistant, chemical-resistant reagent is widely used in UF membrane field.The large multiplex particles sintering legal system of current ceramic super-filtering film is for basement membrane, and with sol-gel process preparation feedback layer, the supporter of porous all to be used as carrier preparing in Ceramic excessive filtration membrane process, and the shape of carrier is all unified fixing, arbitrarily can not change along with needs of production, complicated planform also cannot be shaping, thus limit the scope of application of ceramic super-filtering film.
China Patent Publication No. CN102743979A discloses a kind of preparation method of zirconia ceramic ultrafiltration film, the present invention prepares Zirconium oxalate sol by chemical coprecipitation, low temperature calcination method is adopted to prepare the Zirconium powder of easily dispersion, then grinding distribution is carried out, add coalescents subsequently, drying control agent, defoamer obtain coating liquid, this coating liquid is applied on porous ceramic film support, zirconia ceramic ultrafiltration film rete is obtained through super-dry, sintering, reduce energy consumption, improve the cost performance of milipore filter.
China Patent Publication No. CN101791524A discloses a kind of unsymmetric structure ceramic super-filtering film and preparation method thereof, the present invention by one dimension fibre shape dispersion of materials in colloidal sol, abundant mixing, add dispersant, thickener, defoamer be mixed with preparation liquid, film on porous supporting body, transition zone is formed after drying, at transition zone surface coating colloidal sol preparation liquid, wet film is dried, dries, roasting, namely Temperature fall obtains unsymmetric structure ceramic super-filtering film, and this ceramic super-filtering film has water flux advantage greatly.
China Patent Publication No. CN1686920A discloses a kind of preparation method of ceramic micro filter film, nano-scale oxide is scattered in by dispersant, thickener, defoamer and anticorrisive agent mixed aqueous solution by this method, even formation coating liquid, add template again, with obtained coating liquid film on porous metals or porous ceramic support, and after drying at wet film, drying, process removes polymer template agent, finally carry out roasting shaping, obtain ceramic microfiltration membrane.
Above-mentioned patent is all the preparation method of ceramic super-filtering film, have employed different formulas and preparation method, obtain the ceramic super-filtering film of excellent performance, but all employ the carrier of porous supporting body as film, thus the milipore filter of preparation has, and shape is single, molding cycle is grown, the defect of milipore filter forming method backwardness, be unfavorable for the needs of ceramic super-filtering film in actual production process, limit the application and development of ceramic super-filtering film.
Summary of the invention
The defect single for current ceramic super-filtering film shape, difficult forming, molding cycle are long, propose a kind of preparation method of ceramic super-filtering film, for achieving the above object, the porous ceramics particulate selective laser sintering and moulding technology obtained through sol-gel, sintering, grinding is carried out rapid shaping process by the present invention, be prepared into the ceramic super-filtering film of various space structure, forming method is simple, and practical, water flux is large.
The concrete preparation process of the preparation method of a kind of ceramic super-filtering film of the present invention is as follows:
1) the colloidal solid 70-80 parts by weight solvent of 10-20 weight portion is dissolved at normal temperatures while stirring, mixing speed 50-80r/min, allow colloidal solid form homogeneous, the stable colloidal sol of dispersion in a solvent;
2) colloidal sol step 1) obtained joins in planetary ball mill together with the pore creating material of 2-5 weight portion, fully grind under the speed conditions of 300-350r/min, disperse, mix 20-30min after discharging, carry out suction filtration and obtain mixture;
3) by step 2) mixture that obtains puts into high temperature sintering furnace, and at the temperature of 600-800 DEG C, sinter 1-2h, discharging after normal temperature cooling, then grind with planetary ball mill, then sieve, obtain porous ceramics particulate;
4) according to the needs of practical condition, the requirement of ceramic super-filtering film on thickness, shape, space structure is analyzed, utilizes computer to set up mathematical model, write performing a programme and the order of three-dimensional fast shaping;
5) porous ceramics particulate step 3) obtained joins in the hopper of powder sintered laser fast shaping machine, with computer steps for importing 4) performing a programme that writes and order, powder sintered laser fast shaping machine carries out three-dimensional fast shaping under the automatic control of computer, the ceramic super-filtering film of obtained difformity, stereochemical structure, thickness.
The concrete preparation process 1 of above-mentioned a kind of ceramic super-filtering film) in, described colloidal solid is one or more in aluminium oxide, titanium oxide, zirconia, silica sol; Described solvent is deionized water; One or both in the nano-calcium carbonate of described pore creating material to be diameter be 10-100nm, nano-calcium carbonate magnesium.
The concrete preparation process 2 of above-mentioned a kind of ceramic super-filtering film) in, described sieving was 2000-5000 object sieve.
The concrete preparation process 3 of above-mentioned a kind of ceramic super-filtering film) in, described powder sintered laser fast shaping machine adopts selective laser sintering and moulding technology, namely adopt CO2 laser instrument by the 3-D graphic that computer designs, under control of the computer, the principle of the printing dusty material sinter molding of the one deck be coated with on the table, it is the one in the main former of three-dimensional fast shaping technology, primarily of scanning system, laser control system, heating element heater, moulding cylinder, feeding system, moving component, cooling system, kinetic control system, software systems form.
The present invention utilizes the principle of selective laser sintering and moulding technology in rapid shaping, the porous ceramics particulate selective laser sintering and moulding technology obtained through sol-gel, sintering, grinding is carried out forming processes, make the ceramic super-filtering film of various space structure, forming method is simple, molding cycle is short, practical, the rejection of this ceramic super-filtering film is large, pore size distribution range 10-100nm, under the operating condition of 0.1Mpa, water flux is 100-200L/m
3h.
The feature that the present invention gives prominence to is:
1, the present invention adopts three-dimensional fast shaping technology, makes that ceramic super-filtering film convenient formation, molding cycle are short, various shapes, meets the demand to the various shape of ceramic super-filtering film and structure.
2, the present invention does not need mould, greatly improves the production efficiency of ceramic super-filtering film, has widened range of application.
3, production process of the present invention is simple, and easy to operate, production cost is low, is easy to suitability for industrialized production, and range of application is more extensive.
The technological process of production of the present invention is shown in Figure of description 1.
Detailed description of the invention
Below by way of detailed description of the invention, the present invention is described in further detail, but this should be interpreted as scope of the present invention is only limitted to following example.When not departing from said method thought of the present invention, the various replacement made according to ordinary skill knowledge and customary means or change, all should be within the scope of the present invention.
embodiment 1
1) the alumina gel particle of 10 weight portions is dissolved at normal temperatures while stirring by 70 parts by weight of deionized water, mixing speed 50r/min, allow colloidal solid form homogeneous, the stable colloidal sol of dispersion in a solvent;
2) colloidal sol step 1) obtained joins in planetary ball mill together with the nano-calcium carbonate of 2 weight portions, fully grind under the speed conditions of 300r/min, disperse, mix 20min after discharging, carry out suction filtration and obtain mixture;
3) by step 2) mixture that obtains puts into high temperature sintering furnace, and at the temperature of 600 DEG C, sinter 1h, discharging after normal temperature cooling, then grind with planetary ball mill, then cross 2000 mesh sieves, obtain porous ceramics particulate;
4) according to the needs of practical condition, the requirement of ceramic super-filtering film on thickness, shape, space structure is analyzed, utilizes computer to set up mathematical model, write performing a programme and the order of three-dimensional fast shaping;
5) porous ceramics particulate step 3) obtained joins in the hopper of powder sintered laser fast shaping machine, with computer steps for importing 4) performing a programme that writes and order, powder sintered laser fast shaping machine carries out three-dimensional fast shaping under the automatic control of computer, the ceramic super-filtering film of obtained difformity, stereochemical structure, thickness.
embodiment 2
1) the alumina gel particle of 15 weight portions is dissolved at normal temperatures while stirring by 80 parts by weight of deionized water, mixing speed 60r/min, allow colloidal solid form homogeneous, the stable colloidal sol of dispersion in a solvent;
2) colloidal sol step 1) obtained joins in planetary ball mill together with the nano-calcium carbonate magnesium of 3 weight portions, fully grind under the speed conditions of 300r/min, disperse, mix 20min after discharging, carry out suction filtration and obtain mixture;
3) by step 2) mixture that obtains puts into high temperature sintering furnace, and at the temperature of 700 DEG C, sinter 1h, discharging after normal temperature cooling, then grind with planetary ball mill, then cross 2000 mesh sieves, obtain porous ceramics particulate;
4) according to the needs of practical condition, the requirement of ceramic super-filtering film on thickness, shape, space structure is analyzed, utilizes computer to set up mathematical model, write performing a programme and the order of three-dimensional fast shaping;
5) porous ceramics particulate step 3) obtained joins in the hopper of powder sintered laser fast shaping machine, with computer steps for importing 4) performing a programme that writes and order, powder sintered laser fast shaping machine carries out three-dimensional fast shaping under the automatic control of computer, the ceramic super-filtering film of obtained difformity, stereochemical structure, thickness.
embodiment 3
1) the alumina gel particle of 10 weight portions is dissolved at normal temperatures while stirring by 80 parts by weight of deionized water, mixing speed 70r/min, allow colloidal solid form homogeneous, the stable colloidal sol of dispersion in a solvent;
2) colloidal sol step 1) obtained joins in planetary ball mill together with the nano-calcium carbonate of 4 weight portions, fully grind under the speed conditions of 350r/min, disperse, mix 30min after discharging, carry out suction filtration and obtain mixture;
3) by step 2) mixture that obtains puts into high temperature sintering furnace, and at the temperature of 800 DEG C, sinter 1.5h, discharging after normal temperature cooling, then grind with planetary ball mill, then cross 3000 mesh sieves, obtain porous ceramics particulate;
4) according to the needs of practical condition, the requirement of ceramic super-filtering film on thickness, shape, space structure is analyzed, utilizes computer to set up mathematical model, write performing a programme and the order of three-dimensional fast shaping;
5) porous ceramics particulate step 3) obtained joins in the hopper of powder sintered laser fast shaping machine, with computer steps for importing 4) performing a programme that writes and order, powder sintered laser fast shaping machine carries out three-dimensional fast shaping under the automatic control of computer, the ceramic super-filtering film of obtained difformity, stereochemical structure, thickness.
embodiment 4
1) the alumina gel particle of 20 weight portions is dissolved at normal temperatures while stirring by 80 parts by weight of deionized water, mixing speed 80r/min, allow colloidal solid form homogeneous, the stable colloidal sol of dispersion in a solvent;
2) colloidal sol step 1) obtained joins in planetary ball mill together with the nano-calcium carbonate magnesium of 5 weight portions, fully grind under the speed conditions of 350r/min, disperse, mix 30min after discharging, carry out suction filtration and obtain mixture;
3) by step 2) mixture that obtains puts into high temperature sintering furnace, and at the temperature of 700 DEG C, sinter 2h, discharging after normal temperature cooling, then grind with planetary ball mill, then cross 5000 mesh sieves, obtain porous ceramics particulate;
4) according to the needs of practical condition, the requirement of ceramic super-filtering film on thickness, shape, space structure is analyzed, utilizes computer to set up mathematical model, write performing a programme and the order of three-dimensional fast shaping;
5) porous ceramics particulate step 3) obtained joins in the hopper of powder sintered laser fast shaping machine, with computer steps for importing 4) performing a programme that writes and order, powder sintered laser fast shaping machine carries out three-dimensional fast shaping under the automatic control of computer, the ceramic super-filtering film of obtained difformity, stereochemical structure, thickness.
embodiment 5
1) the alumina gel particle of 15 weight portions is dissolved at normal temperatures while stirring by 75 parts by weight of deionized water, mixing speed 70r/min, allow colloidal solid form homogeneous, the stable colloidal sol of dispersion in a solvent;
2) colloidal sol step 1) obtained joins in planetary ball mill together with the nano-calcium carbonate of 4 weight portions, fully grind under the speed conditions of 300r/min, disperse, mix 25min after discharging, carry out suction filtration and obtain mixture;
3) by step 2) mixture that obtains puts into high temperature sintering furnace, and at the temperature of 700 DEG C, sinter 2h, discharging after normal temperature cooling, then grind with planetary ball mill, then cross 4000 mesh sieves, obtain porous ceramics particulate;
4) according to the needs of practical condition, the requirement of ceramic super-filtering film on thickness, shape, space structure is analyzed, utilizes computer to set up mathematical model, write performing a programme and the order of three-dimensional fast shaping;
5) porous ceramics particulate step 3) obtained joins in the hopper of powder sintered laser fast shaping machine, with computer steps for importing 4) performing a programme that writes and order, powder sintered laser fast shaping machine carries out three-dimensional fast shaping under the automatic control of computer, the ceramic super-filtering film of obtained difformity, stereochemical structure, thickness.
Claims (4)
1. a preparation method for ceramic super-filtering film, is characterized in that concrete preparation method is as follows:
1) the colloidal solid 70-80 parts by weight solvent of 10-20 weight portion is dissolved at normal temperatures while stirring, mixing speed 50-80r/min, allow colloidal solid form homogeneous, the stable colloidal sol of dispersion in a solvent;
2) colloidal sol step 1) obtained joins in planetary ball mill together with the pore creating material of 2-5 weight portion, fully grind under the speed conditions of 300-350r/min, disperse, mix 20-30min after discharging, carry out suction filtration and obtain mixture;
3) by step 2) mixture that obtains puts into high temperature sintering furnace, and at the temperature of 600-800 DEG C, sinter 1-2h, discharging after normal temperature cooling, then grind with planetary ball mill, then sieve, obtain porous ceramics particulate;
4) according to the needs of practical condition, the requirement of ceramic super-filtering film on thickness, shape, space structure is analyzed, utilizes computer to set up mathematical model, write performing a programme and the order of three-dimensional fast shaping;
5) porous ceramics particulate step 3) obtained joins in the hopper of powder sintered laser fast shaping machine, with computer steps for importing 4) performing a programme that writes and order, powder sintered laser fast shaping machine carries out three-dimensional fast shaping under the automatic control of computer, the ceramic super-filtering film of obtained difformity, stereochemical structure, thickness.
2. according to the preparation method of a kind of ceramic super-filtering film described in claim 1, it is characterized in that described pore creating material to be diameter be in the nano-calcium carbonate of 10-100nm, nano-calcium carbonate magnesium one or both.
3., according to the preparation method of a kind of ceramic super-filtering film described in claim 1, it is characterized in that described sieving was 2000-5000 object sieve.
4., according to the preparation method of a kind of ceramic super-filtering film described in claim 1, it is characterized in that described powder sintered laser fast shaping machine adopts selective laser sintering and moulding technology, namely adopt CO
2laser instrument is by the 3-D graphic that computer designs, under control of the computer, the principle of the printing dusty material sinter molding of the one deck be coated with on the table, the one in the main former of three-dimensional fast shaping technology, primarily of scanning system, laser control system, heating element heater, moulding cylinder, feeding system, moving component, cooling system, kinetic control system, software systems composition.
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| CN109626979B (en) * | 2019-02-15 | 2022-03-22 | 中国计量大学 | Preparation method of pore-shaped adjustable calcium silicate porous ceramic membrane |
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| WO1991012879A1 (en) * | 1990-02-21 | 1991-09-05 | Nederlandse Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek Tno | Inorganic membranes and a process for making inorganic membranes |
| CN101333115A (en) * | 2007-06-29 | 2008-12-31 | 哈尔滨工业大学 | Laminate preparation method of ceramic pieces of complex shape |
| CN102806018A (en) * | 2012-07-12 | 2012-12-05 | 三达膜环境技术股份有限公司 | Method for lower-temperature sintering to prepare acid and alkali-resistant titanium dioxide ceramic ultrafiltration membrane |
| CN103013196A (en) * | 2012-12-18 | 2013-04-03 | 上海迪道科技有限公司 | Method for manufacturing ultrathin nano-coating used for surface modification of inorganic nonmetallic material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1991012879A1 (en) * | 1990-02-21 | 1991-09-05 | Nederlandse Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek Tno | Inorganic membranes and a process for making inorganic membranes |
| CN101333115A (en) * | 2007-06-29 | 2008-12-31 | 哈尔滨工业大学 | Laminate preparation method of ceramic pieces of complex shape |
| CN102806018A (en) * | 2012-07-12 | 2012-12-05 | 三达膜环境技术股份有限公司 | Method for lower-temperature sintering to prepare acid and alkali-resistant titanium dioxide ceramic ultrafiltration membrane |
| CN103013196A (en) * | 2012-12-18 | 2013-04-03 | 上海迪道科技有限公司 | Method for manufacturing ultrathin nano-coating used for surface modification of inorganic nonmetallic material |
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Effective date of registration: 20191121 Address after: 233100 Fengyang County town, Chuzhou City, Anhui Province Patentee after: Anhui Fengyang Guofeng Ecological Technology Materials Co., Ltd. Address before: Qingyang District of Chengdu City, Sichuan province 610091 Dragon Industrial Port East Road 4 Patentee before: Chengdu Xinkeli Chemical Sci-Tech Co., Ltd. |