Mesoporous nanopowder titanium dioxide bionic synthesis method
Abstract
The holes nanometre TiO2 powder the superoleophobic synthesis method, belonging to the nanometre technical field. Fermenting in the water solution and surfactant, the emulsified form A emulsion; A wherein the inorganic A solution is added by dropping to emulsion In the brain, pH=7-9, in THE emulsion; , Wherein the washing the alcohol, wherein the thermal treatment; the temperature 300-600℃ in the furnace, and surfactant template; the insulation 1-2h, namely of the hole type nanometre TiO2 powder, of rutile-type nanometre TiO2 powder is 600-700℃ insulation 1-2h. The invention inexpensive use of a surfactant, the biological the nanometre vesicle multi-layer structure and mineralization process of depositing, wherein the hole nanometre TiO2 micro powder in the temperate condition, and as spherical, the particle diameter distribution range is narrow; the dispersing and is good, activity is high, the preparation process is simple, wherein it is low; without pollution.
Term
No projected expiry on record.
- Priority and filed
- Granted
- Today
6 claims: 6 independent, 0 dependent
- 11 Of nanometre Tio2 powder the superoleophobic synthesis method, characterised is a, steps as follows (1) fermenting at normal temperature and pressure of the aqueous solution and surfactant, wherein the surfactant and ball of mother solution, adding the auxiliary and 0-0.002. , at a, the room temperature emulsified is 20-60 minutes, wherein the upper micelle concentration OF emulsion;The biological surfactant is glycolipid, the is phospholipid, fatty acid, is one of protein prime system surfactant or the combination thereof, adding at the upper wherein the micelle 1-10 times;(2) Under the action of magnetic stirring, wherein the comprises inorganic A solution, according to each of 2 to 10 at rate of the solution is added to the emulsion is A liquid, wherein The " is capable of absorbing the biological surfactant cell surface and fully group, the content of The control of 50 to 120g/L, at normal temperature and magnetic force for 0.5 to 1 hours, a wherein the;(3) Under room temperature the ammonia water according to one of dropping speed instillments per minute to any OF solution, regulating p^7-9, to that are stirred 2-3h, wherein the cell structure is mineralization of the surfactant to precipitate, preparing emulsion;C(4) Emulsion IS standing l-2h, wherein the washing of 2 times, for 2 times, wherein the Ntf+ and Cl- and Hao,(5) Is the water and ratio of the 60-80'C the drying 2-3h, wherein the drying and settling of the thermal treatment, a less than the furnace 10 ' speed warming of C/min to 300-60 (CENTIGRADE, and surfactant template;the insulation l-2h, namely of the hole type nanometre Tio2 powder, of rutile-type nanometre Tio2 powder is 600-70 (degrees centigrade and insulating 1-2h. 1.介孔纳米粉体TiO2的仿生合成方法,其特征在于,步骤如下: (1)将生物表面活性剂于常温常压下在水溶液中发酵,形成生物表面活性剂的球丝酵母水溶液,加入糖助剂0-0.1g/L,搅拌,室温乳化20-60分钟,形成临界胶束浓度的乳化液A;所述的生物表面活性剂是糖脂系、磷脂系、脂肪酸系、蛋白质系表面活性剂之一或组合,加入量为其临界胶束浓度的1-10倍; (2)在磁力搅拌的作用下,将含有Ti4+的无机溶液,按每分钟2-10滴的滴加速度加到上述乳化液液体A中,让Ti4+能够充分吸附到生物表面活性剂细胞表面的阴离子群上,TiO2含量控制在50~120g/L,常温下磁力搅拌0.5~1小时后,得溶液B; (3)室温下将氨水按每分钟1-5滴的速度滴加到上述B溶液中,调节pH=7-9,继续搅拌2-3h,让生物表面活性剂的细胞结构充分矿化沉淀,得到乳浊液C; (4)将乳浊液C静置1-2h,然后将沉淀物水洗2次,醇洗2次,分别除去NH4+和Cl-以及H2O; (5)将水洗和醇洗后的沉淀物在60-80℃干燥2-3h,再将干燥后的沉淀物进行热处理,在煅烧炉中以小于10℃/min的速度升温到300-600℃,除去生物表面活性剂模板,保温1-2h后,即得到介孔锐钛矿TiO2纳米粉体,在600-700℃保温1-2h后得到介孔金红石TiO2纳米粉体。
- 2If the nanometre Tio2 powder the superoleophobic synthesis method according to claim wherein the is a characterised, wherein the Ti and raw material selected from the titanium sulphate, chloric the acid solution, the nitric acid titanium, citric acid, titanium white hydroxide or titanium dioxide one or the combination. 2. 如权利要求l所述的介孔纳米粉体Ti02的仿生合成方法,其特征在于,所述的含Ti" 的原料选自硫酸钛、氯酸钛、硝酸钛、柠檬酸钛、氢氧化钛或氧化钛之一或组合。
- 3Wherein the hole nanometre Tio2 powder the superoleophobic synthesis method according to any one of the is a characterised, wherein the glycolipid is of the compound or a rhamnose fertilizer, the alga glycolipid or scholartree glycolipid, the scholartree glycolipid is a sphere of yeast or yeast is wherein the glucose and is as the dike hydrocarbon or the long chain fatty acid and is. 3. 如权利要求l所述的介孔纳米粉体Ti02的仿生合成方法,其特征在于,所述糖脂系生 物表面活性剂为鼠李糖脂、海藻糖脂或槐糖脂,其中槐糖脂是球丝酵母或假丝酵母在葡萄糖 和正构垸烃或长链脂肪酸中培养时产生的。
- 4Wherein the hole nanometre Tio2 powder the superoleophobic synthesis method according to any one of the is a characterised, wherein the phospholipid is of the compound or the lecithin or a composite bacteria fermentation culturing of phospholipid. 4. 如权利要求l所述的介孔纳米粉体Ti02的仿生合成方法,其特征在于,所述磷脂系生 物表面活性剂为卵磷脂或由硫磺细菌发酵培养的磷脂。
- 5Wherein the hole nanometre Tio2 powder the superoleophobic synthesis method according to any one of the is a characterised, wherein the fatty acid is the surfactant to cover the mycolic acid or the penicillium brevicompactum in the gallic acid. 5. 如权利要求l所述的介孔纳米粉体Ti02的仿生合成方法,其特征在于,所述脂肪酸系 生物表面活性剂为覆盖霉菌酸或青霉孢子酸。
- 6Wherein the hole nanometre Tio2 powder the superoleophobic synthesis method according to any one of the is a characterised, wherein the protein is the surfactant or and adhesive proteolysis product and arginine the condensation compound is not. 6. 如权利要求l所述的介孔纳米粉体Ti02的仿生合成方法,其特征在于,所述蛋白质 系生物表面活性剂为明胶或用胶原蛋白质水解产物与精氨酸反应的縮合物。
Independent claims6
4 paragraphs, as filed
The thermoplastic biological synthesis method of the powder nanometre titanium dioxide
technical field
The invention relates to the low-cost preparing the nanometre Tio2 powder the superoleophobic synthesis method, belonging to the nanometre technical field. Background of nano-level hole is Ratio of the non-toxic, chemical thermostability and aerobic, high performance water and special photo-catalysis performance and an performance, and widely used for high-concentration the operation of from industrial waste water process of the photocatalyst, wherein in solar battery material and catalyst material, and can also be used for high performance the ceramic. The research of the nanometre Tio2 of the superoleophobic method for preparing; the grain distributed on one radius narrowly, absence of the reunited, the intermediate particle size of anatase of 8-20nm, BET comprises as high as 280m7g, activity is high, of which the particle size of 70 degrees with of the range 25-100nm oxide particles, regardless of of anatase or rutile, wherein the particle has the structure hole, wherein the middle size of 3-15nm, is represented by the transmission electron microscope following evaluating 3 and 4 in. A pore structure 丌 02 activity of high, wherein the nanometre and packaging, a wherein the wavelength range reaction, and solar factor is performed, having high yield quantum, so the visible light and infrared light in solar spectrum of the effective the catalyst is activated. The technique for preparing method of the sol gel method, a precipitation and Water Method, the template method and so on, wherein the particle The reunited of ABR+OBR preparation method of serious, activity is low; the preparing technique is complex, and it is high, the use effect is added that wherein the hard wherein application thereof. Improved how to prepare the low-cost preparing the nanometre Tio2 powder is field the novel topic. The problem of the invention content to solve the existing technology, comprising the invention claims a hole nanometre Tio2 powder the superoleophobic synthesis method, for preparing the nanometre Tio2 micro powder by low cost system. The invention uses a biological surfactant is a template, and a Ti raw materials, the mineralization biological film under mild conditions, wherein the superoleophobic nanometre assembly, wherein the inorganic organic compound material, finally removing organic template, the prepared in preparing a hole 1102 nanometres micro powder. The invention claims a thermoplastic biological synthesis method of the nanometre Tio2 powder, the steps as follows: (1) Fermenting at normal temperature and pressure of the aqueous solution and surfactant, wherein the surfactant and ball the yeast solution, adding sugar O-O agent. , at a, the room temperature emulsified is 20-60 minutes. On the upper micelle concentration OF emulsion. The biological the surfactant is carried out the self-assembly template method, wherein the VH the circular or elliptic structure cell, wherein the upper micelle concentration OF emulsion. A circular or combination of cell structure into emulsion further researching in-situ the heating. (2) Under the action of magnetic stirring, wherein the Ti and inorganic solution, according to each of 2 to 10 at rate of the solution is added to the emulsion is A liquid, wherein The " is capable of absorbing the bioactive agent cell surface and diatom, wherein The control is 50 to 120g/L (Tio2 the content of contains inorganic salt solution conversion of TT+ is), at normal temperature and magnetic force and a 0.5-l hours, a dispersing solution B. An inorganic salt cationic The of the microscope the absorption the presence of cell wall; the researching in-situ - into 2 in. (3) Under room temperature the ammonia water according to one of dropping speed instillments per minute to any OF solution, regulating P^7-9, to that are stirred 2-3h, wherein the cell structure is mineralization of the surfactant to precipitate, obtaining THE emulsion. (4) Emulsion IS standing 1-2h, wherein the washing of 2 times, for 2 times, and NH4+ and Cr and (3-6).
(5) Is the water and ratio of of 60-8 (degrees centigrade for 2-3h, wherein the drying and settling of the thermal treatment, a less than the furnace to (speed warming of TC/min to 300-60 (CENTIGRADE, and surfactant template; the insulation l-2h, namely of the hole type nanometre Tio2 powder (IN-SITU the spectrum as shown in Figure 5), of rutile-type nanometre Tio2 powder is 600-7 (XTC insulation 1-2h (IN-SITU the spectrum as shown in Figure 6). The is comprising The raw materials of the titanium sulphate, chloric the titanium acid, nitric acid, citric acid, titanium neodymium hydroxide or titanium dioxide one or the combination. The biological surfactant is the is glycolipid, which comprises comprises the is ammonia, phospholipid, is fatty acid, is one of protein prime system surfactant or the combination thereof, the adding amount of the upper micelle concentration 1-10 times. The glycolipid is the surfactant is generally the rhamnose fertilizer, the alga glycolipid, the scholartree glycolipid and so on, the scholartree glycolipid of the ball the yeast or yeast is wherein the glucose is as of the organic or the long chain fatty acid for producing; The n-acyl comprises the ammonia is the surfactant is chamber is bacillus - subtilis and culture of the product; The phospholipid is the surfactant is generally lecithin or a composite bacteria fermentation culture phospholipid and so on,The fatty acid is the surfactant to cover the mycolic acid or the penicillium brevicompactum in the gallate chamber and so on,Protein prime biological system surfactant or chamber and adhesive proteolysis product and arginine the condensation compound is gelatine and so on. The invention, wherein and technology of removing the surfactant template, the collapse of the structure formed, wherein the concentration of higher, and ball wall is thicker, vice versa. The control < lCTC/rain and thermal treatment heating speed of the template. , And the biological containing compound and is used, and hole of the size of the pore structure is formed with a important improved. Compared to the existing technology, the invention method for and use inexpensive a biological surfactant, the biological the nanometre vesicle multi-layer structure and mineralization process of depositing, wherein the hole nanometre Tio2 micro powder in the temperate condition, and as spherical, the particle diameter distribution range is narrow; the dispersing and is good, activity is high, the preparation process is simple, wherein it is low; without pollution. The anatase The middle particle size of 8-20nm, wherein the middle size of 3-15nm, reaches as high as 280raVg specific surface area 3-0.1 (), the photo-catalysis degrading high-concentration difficult to for waste water by using oxygen consumption is reduced to 80. A, the weight percentage of decolouring 99% reached. Hole type 650 in. C may form a layer of hole oxide, 700°: (The crystallinity of rutile-type is 99.95%; the particle size of 25-100nm, reaches as high as 112ra7g specific surface area () 3-0.1. The low-cost about the process of 50%. The layer of hole TiC 2) can be used for nanometre material component and high concentration is difficulty to degrade the industrial waste the photocatalyst, a solar cell, an electronic, ceramic composite material, the ultraviolet shielding material and so on. The herein described instructional diagram is 1 to implement as two glycolipid is a circular or the combination of the yeast cells with the surfactant scholartree glycolipid emulsion for researching in-situ (400) is. With 2 to implement as two inorganic salt and A ion absorption of the scholartree glycolipid and yeast cell wall for researching in-situ (400) is. The isolated is 3 to implement as 2 to 500 ' end C, anatase the electron microscope following step (270,000) is. The isolated is 4 to implement as 2 to 70 DEGREES the oil, or the electron microscope following (16-2 million) is. The isolated is 5 to implement as 2 to 50 DEGREES the calcined, an X-ray diffraction spectrogram of anatase, wherein the molar ratio of the is strength, the abscissa of the angle is. The 郞 of from 2 to 70 DEGREES the oil, or degrees centigrade In the diffracts honey, wherein the molar ratio of the is strength, the abscissa of the angle is. Detailed description of illustrated embodiments substantially as catalyst. 150ml 6. 7g/L (upper micelle concentration of the glycolipid is a biological scholartree surfactant glycolipid and yeast aqueous solution sweetens 0.5g to stir and emulsify for 20 minutes under room temperature, obtaining A emulsion, and ml, 0.4mol/L Ti (phenyl GROUP of solution, wherein each of 10 dropping speed of instillments to The emulsion, of the magnetic force stirring to 30 min, The ph to the water is fully the biological cell vesicle nanometre structure. A is 5 of the added by dropping the mol/l ammonia water is added slowly, 1-7, ^=7 to that the magnetic force to stir 2h, wherein the cell division structure mineralization deposition, standing and 2h, wherein the centrifugal separation, the water, the alcohol comprises twice, and S0/- and NtV and Hao. The final 80 of oven. The optimal C, 2h of 5. C/min heating speed, wherein the compound 400: A 70 (rC thermal treatment, 2h hole type hole and rutile of are. The Tio2 type particle size of 10-25nm, wherein the middle size of 3-llnm, BET comprises as high as 220m7g. The grain size of rutile-type is 52-120nm, BET comprises as high as 62m7g. Substantially as 2. 6 ml. 7g/L (upper micelle concentration of the glycolipid is a biological scholartree surfactant glycolipid and yeast aqueous solution sweetens 0.5g under room temperature, stirring emulsified 20 min after The emulsion. the 50ral 0.5mol/LTiCl4 solution, the dropping speed of each 16-2 is reduced to The emulsion, of the magnetic force to stirring for 30 minutes, a Hydrogen to the water is fully the biological cell vesicle nanometre structure. A is 5 of the added by dropping the mol/l ammonia water is added slowly, 1-7, PH-7 to that the magnetic force to stir 2h, wherein the cell structure is mineralization deposition, standing and 2h, wherein the centrifugal separation, the water, the alcohol comprises twice, and C1- and NH/and (3-6). The desilting in an oven 8 degrees drying 1200, wherein a 5 ' C/min heating speed, wherein the 500. CENTIGRADE and 700 ' THE thermal treatment, 2h includes a hole type hole and rutile. The anatase The middle particle size of 8-20nra, wherein the middle size of 3-15nm, BET comprises as high as 280m7g, the intermediate particle size of rutile-type of 25-100nm, BET comprises as high as 112ra7g. The pharmaceutical composition according to claim 3. such administering to the truthfully, 0-50% of different is the thermal treatment heating speed of the (TC/min, the thermal treatment temperature is 450 ' CENTIGRADE and form. The Tio2 type particle size of 12-31nm, wherein the middle size of 5-13nm, BET comprises as high as 180m2/g. The grain size of rutile-type is 62-110nm, BET comprises as high as 56m7g. The pharmaceutical composition according to claim 4. executes as 2 to truthfully, 0-50% of different is the thermal treatment heating speed of the (TC/min, the thermal treatment temperature is 45 degrees CENTIGRADE and 75 degrees. The anatase The middle particle size of 8-25nm, wherein the middle size of 4-10nm, BET comprises as high as 250mVg, rutile particle size of 29-110nm, BET comprises as high as 102m7g. The pharmaceutical composition according to claim 5. executes as 2 to truthfully, 0-50% of different is a biological or a phospholipid is a biological lecithin surfactant, wherein concentration of 0.0014g/L, and not sweeten. The anatase The middle particle size of 18-70nm, wherein the middle size of 3-10nm, the intermediate particle size of rutile-type of 85-180nm . The pharmaceutical composition according to claim 6. such administering to the truthfully, 0-50% of different is the surfactant is penicillium brevicompactum in the gallic acid. The pharmaceutical composition according to claim 7. such administering to the truthfully, 0-50% of different is the surfactant is not.
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| Document | Relation | Office | Cited during |
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| CN1192992A | Cites | China | Search report |
| CN1248550A | Cites | China | Search report |
| CN1316383A | Cites | China | Search report |
| CN1636879A | Cites | China | Search report |
| JP2004131366A | Cites | Japan | Search report |
2 members in 1 office
Priority claims2
| Document | Office | Kind | Date |
|---|---|---|---|
| 200510044588 | China | A | |
| CN2005144588 | – | – | – |
Members2
| Document | Office | Kind | |
|---|---|---|---|
| CN1762828A | China | A | |
| CN100368301CThis record | China | C |
Numbers
- Publication
- 100368301
- Publication, DOCDB
- 100368301
- Publication, EPODOC
- CN100368301C
- Application
- 100445881
- Application, DOCDB
- 200510044588
- Application, EPODOC
- CN200510044588
Titles2
- English
- Mesoporous nanopowder titanium dioxide bionic synthesis method
- Chinese
- 介孔纳米粉体二氧化钛的仿生合成方法
Classification
- IPC, 1
- C01G23 047