CN103977713B - A kind of ceramic support hybridization silicon oxide film preparation technique - Google Patents
A kind of ceramic support hybridization silicon oxide film preparation technique Download PDFInfo
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- CN103977713B CN103977713B CN201410166327.6A CN201410166327A CN103977713B CN 103977713 B CN103977713 B CN 103977713B CN 201410166327 A CN201410166327 A CN 201410166327A CN 103977713 B CN103977713 B CN 103977713B
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Abstract
The invention discloses a kind of ceramic support hybridization silicon oxide film preparation skill, belong to technical field of membrane separation, prepare film pipe, and purge described film pipe with nitrogen, with the dust of clean described film tube-surface; Described film pipe is put into calcining furnace to fire to remove the organic matter on described film pipe; Use coating equipment by carrier material on described film pipe; After coating is good, described film pipe is placed in described calcining furnace and calcines; Use diamond to be polished at the two ends of described film pipe, described film pipe by the length about 10 millimeters polished, and applies one deck glass; Coating equipment is used to be coated with one deck carrier material more first-class to described film pipe.Compared with prior art, hybridization silicon oxide film of the present invention is by SiO
2middle part Si-O-Si key Si-CmHn-Si replaces, have with molecular screen membrane on equal separating property basis, add resistant to hydrolysis performance, acid resistance and resistance to elevated temperatures, and then extend the membrane material life-span, fill up the blank that infiltrating and vaporizing membrane product both domestic and external adopts the coating of earthenware inwall.
Description
Technical field
The invention belongs to technical field of membrane separation, particularly relate to a kind of ceramic support hybridization silicon oxide film preparation technique.
Background technology
Along with rapid industrial development, various organic solvent is used widely, and comprises the chemical solvents such as alcohols, ester class, ketone, ethers, aromatic compound and is applied to the fields such as the energy, medicine, biology, play an important role in national economy.At present both at home and abroad research also the infiltration evaporation membrane material of dehydration of organic solvent technology of industrial applications can mainly contain two kinds: organic polymer membrane material and organic zeolite membrane material.For characteristics such as most organic solvent slant acidity and infiltration evaporation treatment temperature height, these two kinds of membrane materials all have drawback, organic pervaporation membrane heatproof, resistance to erosion, acid and alkali-resistance and swelling resistance scarce capacity, only there is the life-span of some months, add the processing cost of infiltration evaporation because the life-span is short, the substitute is inoranic membrane gradually.Organic zeolite membrane take NaA as representative, though can obtain good separating property index, its long-term hydrothermal stability is bad.In addition, because self Si-O-Si key of molecular sieve is unstable, acid resistance and resistant to hydrolysis poor performance, therefore can not be used in the lower dehydration of organic solvent of pH value, and the membrane material life-span is shorter.
In addition in prior art, earthenware is used to be mostly that outer wall applies as supporter coat film material, although paint-on technique difficulty is low, outer wall coat film pipe, easily damages when installation operates; When use operates pipe outer walk fluid, vacuumize in pipe, in pipe, space is little, and vacuumize efficiency low and cause film service efficiency low, the infiltrating and vaporizing membrane product of the present invention's exploitation is by Material coating on earthenware inwall, can avoid above problem.
Summary of the invention
The present invention is directed to deficiency of the prior art, provide a kind of ceramic support hybridization silicon oxide film preparation technique, fill up the blank that infiltrating and vaporizing membrane product both domestic and external adopts the coating of earthenware inwall.
In order to solve the problems of the technologies described above, the present invention is solved by following technical proposals: a kind of ceramic support hybridization silicon oxide film preparation technique, concrete steps are as follows: step S1: prepare film pipe, and purge described film pipe with nitrogen, with the dust of clean described film tube-surface; Step S2: described film pipe is put into calcining furnace and fire to remove the organic matter on described film pipe; Step S3: use coating equipment and adopt earthenware inwall coating method by carrier material on described film pipe, to obtain the internal layer of ceramic support hybridization silicon oxide film; Step S4: after coating is good, described film pipe is placed in calcining furnace and calcines; Step S5: use diamond to be polished at the two ends of described film pipe, described film pipe by the length about 10 millimeters polished, and applies one deck glass in the region be polished, to be lived by sealing joint; Step S6: use coating equipment to be coated with on one deck carrier material to described film pipe again, to obtain the intermediate layer of ceramic support hybridization silicon oxide film; Step S7: the described film pipe of step S6 is placed on drying box inner drying, and temperature keeps 40 DEG C, relative humidity 60%; Step S8: after to be dried, is placed into described film pipe in described calcining furnace and continues calcining; Step S9: use coating equipment by hybridization silicon oxide Material coating on described film pipe, to obtain the skin of ceramic support hybridization silicon oxide film; Step S10: be placed in calcining furnace by the described film pipe in step S9, after placing at least 12 hours, uses 300 DEG C-400 DEG C sintered membrane pipes, is made ceramic support hybridization silicon oxide film under room temperature condition.
Ceramic support hybridization silicon oxide infiltrating and vaporizing membrane is using earthenware as supporter, with λ-Al
2o
3, titanium dioxide, the material such as zirconia or silica be carrier, be the micropore dense film of 20 ~ 2000nm at 0.3 ~ 0.6nm, thickness at formation one deck average pore size integrated distribution of carrier surface by modified hybridization silicon oxide Material coating, therefore from structure and aperture point, this film is made up of trilaminate material altogether, ground floor ceramic supporting body is macroporous granules material, second layer carrier material is as mesoporous particles material, third layer hybridization silicon oxide is as microporous particulate material, progressive, and then the infiltrating and vaporizing membrane that formation rule is level and smooth.
As preferably, the firing temperature in the calcining furnace in above-mentioned steps S2 is 500 DEG C-600 DEG C, in air atmosphere heat treatment 2h, intensification cooldown rate be 0.5 DEG C/min.
As preferably, the firing temperature in the calcining furnace in above-mentioned steps S4 is 1000 DEG C-1200 DEG C, in air atmosphere heat treatment 2h, intensification rate of temperature fall be 0.5 DEG C/min.
As preferably, the firing temperature in the calcining furnace in above-mentioned steps S8 is 500 DEG C-600 DEG C, in air atmosphere heat treatment 2h, intensification cooldown rate be 0.5 DEG C/min.
Beneficial effect of the present invention: the hybridization silicon oxide membrane material of the present invention's exploitation is by SiO
2middle Si-O-Si key, part Si-CmHn-Si replaces, have with molecular screen membrane on equal separating property basis, add resistant to hydrolysis performance, acid resistance and resistance to elevated temperatures, and then extend the membrane material life-span, and the ceramic support hybridization silicon oxide infiltrating and vaporizing membrane manufactured by technique scheme has following superior function: 1) hydrothermal can work for a long time under 120 DEG C ~ 150 DEG C thermal and hydric environments, the highlyest bear 170 ~ 190 DEG C; 2) resistance to acids and bases is applicable to the organic solvent of PH=3 ~ 8; 3) solvent resistance is applicable to various solvent and the mixed solvents thereof such as common alcohol, ether, ketone, ester, benzene, phenol, oxolane, acetonitrile.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in further detail.
Embodiment 1: a kind of ceramic support hybridization silicon oxide film preparation technique, comprise coating, dry and calcination process, concrete steps are as follows: step S1: prepare film pipe, and purge described film pipe with nitrogen, with the dust of clean described film tube-surface; Step S2: described film pipe is put into calcining furnace and fire to remove the organic matter on described film pipe; Step S3: use coating equipment and adopt earthenware inwall coating method by carrier material on described film pipe, to obtain the internal layer of ceramic support hybridization silicon oxide film; Step S4: after coating is good, described film pipe is placed in calcining furnace and calcines; Step S5: use diamond to be polished at the two ends of described film pipe, described film pipe by the length about 10 millimeters polished, and applies one deck glass in the region be polished, to be lived by sealing joint; Step S6: use coating equipment to be coated with on one deck carrier material to described film pipe again, to obtain the intermediate layer of ceramic support hybridization silicon oxide film; Step S7: the described film pipe of step S6 is placed on drying box inner drying, and temperature keeps 40 DEG C, relative humidity 60%; Step S8: after to be dried, is placed into described film pipe in described calcining furnace and continues calcining; Step S9: use coating equipment by hybridization silicon oxide Material coating on described film pipe, to obtain the skin of ceramic support hybridization silicon oxide film; Step S10: be placed in calcining furnace by the described film pipe in step S9, after placing at least 12 hours, uses 300 DEG C of sintered membrane pipes, is made ceramic support hybridization silicon oxide film under room temperature condition.
Ceramic support hybridization silicon oxide infiltrating and vaporizing membrane is using earthenware as supporter, with λ-Al
2o
3, titanium dioxide, the material such as zirconia or silica be carrier, be the micropore dense film of 20 ~ 2000nm at 0.3 ~ 0.6nm, thickness at formation one deck average pore size integrated distribution of carrier surface by modified hybridization silicon oxide Material coating, therefore from structure and aperture point, this film is made up of trilaminate material altogether, ground floor ceramic supporting body is macroporous granules material, second layer carrier material is as mesoporous particles material, third layer hybridization silicon oxide is as microporous particulate material, progressive, and then the infiltrating and vaporizing membrane that formation rule is level and smooth.
In technique scheme, the firing temperature in the calcining furnace in above-mentioned steps S2 is 600 DEG C, in air atmosphere heat treatment 2h, intensification cooldown rate be 0.5 DEG C/min.
In technique scheme, the firing temperature in the calcining furnace in above-mentioned steps S4 is 1200 DEG C, in air atmosphere heat treatment 2h, intensification rate of temperature fall be 0.5 DEG C/min.
In technique scheme, the firing temperature in the calcining furnace in above-mentioned steps S8 is 600 DEG C, in air atmosphere heat treatment 2h, intensification cooldown rate be 0.5 DEG C/min.
Embodiment 2: described carrier material is titanium dioxide, firing temperature in described step S2 and S8 in calcining furnace is 500 DEG C, firing temperature in described step S4 in calcining furnace is 1100 DEG C, and the firing temperature in described step S10 is 400 DEG C, and all the other technical schemes are same embodiment 1.
Embodiment 3: described carrier material is zirconia, firing temperature in described step S2 and S8 in calcining furnace is 550 DEG C, firing temperature in described step S4 in calcining furnace is 1050 DEG C, and the firing temperature in described step S10 is 350 DEG C, and all the other technical schemes are same embodiment 1.
Embodiment 4: described carrier material is silica, firing temperature in described step S2 and S8 in calcining furnace is 600 DEG C, firing temperature in described step S4 in calcining furnace is 1000 DEG C, and the firing temperature in described step S10 is 300 DEG C, and all the other technical schemes are same embodiment 1.
That more than enumerates is only specific embodiments of the invention, obviously, the invention is not restricted to above embodiment.All distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate, all should belong to protection scope of the present invention.
Claims (4)
1. a ceramic support hybridization silicon oxide film preparation technique, it is characterized in that, concrete steps are as follows: step S1: prepare film pipe, and purge described film pipe with nitrogen, with the dust of clean described film tube-surface; Step S2: described film pipe is put into calcining furnace and fire to remove the organic matter on described film pipe; Step S3: use coating equipment and adopt earthenware inwall coating method by carrier material on described film pipe, to obtain the internal layer of ceramic support hybridization silicon oxide film; Step S4: after coating is good, described film pipe is placed in calcining furnace and calcines; Step S5: use diamond to be polished at the two ends of described film pipe, described film pipe by the length 10 millimeters polished, and applies one deck glass in the region be polished, to be lived by sealing joint; Step S6: use coating equipment to be coated with on one deck carrier material to described film pipe again, to obtain the intermediate layer of ceramic support hybridization silicon oxide film; Step S7: the described film pipe of step S6 is placed on drying box inner drying, and temperature keeps 40 DEG C, relative humidity 60%; Step S8: after to be dried, is placed into described film pipe in described calcining furnace and continues calcining; Step S9: use coating equipment by hybridization silicon oxide Material coating on described film pipe, to obtain the skin of ceramic support hybridization silicon oxide film; Step S10: be placed in calcining furnace by the described film pipe in step S9, after placing at least 12 hours, uses 300 DEG C-400 DEG C sintered membrane pipes, is made ceramic support hybridization silicon oxide film under room temperature condition.
2. a kind of ceramic support hybridization silicon oxide film preparation technique according to claim 1, is characterized in that: described carrier material is λ-Al
2o
3, titanium dioxide, zirconia or silica.
3. a kind of ceramic support hybridization silicon oxide film preparation technique according to claim 1, is characterized in that: the firing temperature in the calcining furnace in described step S2 and described step S8 is 500 DEG C-600 DEG C.
4. a kind of ceramic support hybridization silicon oxide film preparation technique according to claim 1, is characterized in that: the firing temperature in the calcining furnace in described step S4 is 1000 DEG C-1200 DEG C.
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| CN103977713B true CN103977713B (en) | 2015-10-28 |
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| CN105777206B (en) * | 2016-01-28 | 2018-05-01 | 常州大学 | A kind of method for preparing ultra-thin organosilicon membrane |
| CN110787660A (en) * | 2019-10-29 | 2020-02-14 | 南京工业大学 | Method for recycling organic-inorganic composite membrane ceramic support |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997010045A1 (en) * | 1995-09-12 | 1997-03-20 | Instituut Voor Agrotechnologisch Onderzoek (Ato-Dlo) | Tubular membrane, method for manufacturing same, and membrane separation process |
| CN1310138A (en) * | 2001-04-09 | 2001-08-29 | 南京化工大学 | Ceramic film tube bioreaction and separation system |
| CN101664646A (en) * | 2009-09-27 | 2010-03-10 | 南京工业大学 | Preparation method of ceramic ultrafiltration membrane and automatic coating device |
| CN101708400A (en) * | 2009-12-01 | 2010-05-19 | 韶关市贝瑞过滤科技有限公司 | Method for preparing seamless sintering metal powder filtering membrane tube |
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2014
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997010045A1 (en) * | 1995-09-12 | 1997-03-20 | Instituut Voor Agrotechnologisch Onderzoek (Ato-Dlo) | Tubular membrane, method for manufacturing same, and membrane separation process |
| CN1310138A (en) * | 2001-04-09 | 2001-08-29 | 南京化工大学 | Ceramic film tube bioreaction and separation system |
| CN101664646A (en) * | 2009-09-27 | 2010-03-10 | 南京工业大学 | Preparation method of ceramic ultrafiltration membrane and automatic coating device |
| CN101708400A (en) * | 2009-12-01 | 2010-05-19 | 韶关市贝瑞过滤科技有限公司 | Method for preparing seamless sintering metal powder filtering membrane tube |
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