Method for preparing high- stable neutral mixed crystal nanometer TiO2 hydrosol
Abstract
The preparation method of the invention relates to a high and crystal is nanometre TiO2 hydrosol, the photochemical catalysis of nanometre titanium dioxide material and preparation technique technical field. The invention method comprises the following steps: (1). Precipitating and alkali solution in the titanium compound. Filtering, washing,(2). In the acid solution, the 60~100℃ the dispergation, and adding a certain amount of the SiO2 sol as stabilizer and metal salt of the dopant, the sustained a reaction time; (3). Adding the alkaline solution for regulating the pH value to 7~8; The (4). filtering, washing, and filter cakes of the following water, dispersing, finally obtaining the stable and crystal the nanometre TiO2 sol. The Voltage is hydrosol of the invention prepared from reveals the neutral, the transparency and stability is good, anatase-type oxide and crystal is controllable, wherein determined from reaction is 1-5. The invention is hydrosol TiO2 spray coating of ease operation. The is hydrosol of the sewage treatment using solar, the gas purifying, antibacterial treatment, glass coating and processing process in.
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1 claim: 1 independent, 0 dependent
- 1The preparation method of high and crystal is nanometre Tio2, hydrosol the is characterised according to the following preparation method and steps:a. Titanium compound by weight: Is the titanium compound is the raw material;precipitating the titanium compound in the alkali solution;The titanium of the compound of any one of titanium tetrachloride, metatitanic acid or titanyl sulphate;The alkali solution is ammonia water or sodium hydroxide solution;b. The washing: The process according to the de-ionized water of the obtained reaction, less than 100tx S/cm until the conductivity of filtering;C. adding acid: dispergationAccording to the titanium compound and acid solution Ratio is 1 to 2): 1), To obtain the filter cakes adding acid;The method according to any one of nitric acid, hydrochloric acid or sulphuric acid;Dispergation 10 to 60min is 60 to 10 degrees centigrade and temperature;. The stabilizer and dopant: Adding a certain amount of the Sio2 sol and metal salt, the reaction sustained 0.5 to 4.0 hours;The adding amount of Sio2 sol is the sol total amount 1~10%;A role is a will and Tio2 and sol is wherein the requirement;The adding amount of the metal salt is the sol total amount 0.01%~0.8%;A function of the doped with modified to The nanometre, adjusting the crystal The type of rutile-type and;andThe metal salt is any one of Fe (N03 3), SnCl4, Zn N03 (2) or Ce (N03 3);e. The pH value of alkalizing regulating solution: The ph of the solution with the alkali solution the pH value to 7 to 10;f. The washing: Wherein the filtering solution, the deionized water washing is precipitated, until the conductivity of filtering is less than teaches, uS/cm g. Comprises: According to the solid content claim, wherein the obtained and of the following water, dispersing, the neutral and nanometre Tio2 hydrosol compound;The is hydrosol the content of The is 1~5%;The ratio of the type of rutile-type crystal is 1:0.1 or is 0.1-1 controllable. 1.一种高稳定中性混晶纳米TiO2水溶胶的制备方法,其特征在于具有以下的制备过程和步骤: a.钛化合物水解沉淀:选用无机钛化合物为原料,用碱溶液将钛化合物水解沉淀;钛化合物为四氯化钛、偏钛酸或硫酸氧钛中的任一种;碱溶液为氨水或者氢氧化钠水溶液; b.过滤洗涤:用去离子水洗涤上述反应中所得到的沉淀,直到滤液的电导率小于100μS/cm; c.加酸解胶:按照钛化合物与酸溶液的摩尔比为(1~2)∶1的比例,向得到的滤饼中加入酸;所用的酸为硝酸、盐酸或者硫酸中的任一种;在60~100℃温度下解胶10~60min; d.加入稳定剂和掺杂剂:加入一定量的SiO2溶胶和金属盐,持续反应0.5~4.0小时;SiO2溶胶的加入量为溶胶总量的1~10%;其作用是起到稳定TiO2溶胶及维持其中性的要求;金属盐的加入量为溶胶总量的0.01%~0.8%;其作用是对纳米TiO2进行掺杂改性,调节TiO2晶型锐钛矿与金红石型两者的比例;所述的金属盐为Fe(NO3)3、SnCl4、Zn(NO3)2或Ce(NO3)3中的任一种; e.加碱调节溶液的pH值:用碱溶液调节上述溶液的pH值至7~10; f.过滤洗涤:将上述溶液过滤后,用去离子水洗涤所得的沉淀,直到滤液的电导率小于100μS/cm; g.重新分散:按照固含量要求,将所得滤饼溶于一定量的水中,重新分散,得到中性的稳定的纳米TiO2复合水溶胶;所得水溶胶中TiO2含量为1~5%;其锐钛矿与金红石型晶体的比例为1∶0.1或0.1~1之间可控。
26 paragraphs, as filed
The preparation method of high and crystal of The nanometre hydrosol
technical field
: The preparation method of the invention relates to a high and crystal is nanometre Tio2, hydrosol of photochemical catalysis of nanometre titanium dioxide material and preparation technique technical field.
background technology
: The nanometre titanium dioxide with high photo-catalysis activity, and an organic the floating is mineralization Is Hao, and inorganic acid, and a corrosion resistance and bottom non-toxic, and merits.
Nanometre Ti (V sols is one of the dispersing, wherein the aqueous sol of crystallization, and is used in the dispersing agent and titanium dioxide powder suspension. The sol can directly using titanium source method, does not need to a powder, the sol of crystallization to avoid the end of the reunited question therefore, the product dispersivity is good, wherein the aerobic, modification is convenient. The; the sol is preferably than the hydrophilic, and adhesion, easy spray film. The coating layer, the acid sol has corrosiveness to substrate, therefore preparing neutral nanometre Tio2 appears hydrosol the important. , And the isoelectric The point is 5 to 6, wherein The pure sol the stability of the alkaline condition is not high, the standing time length, wherein of precipitation, and adding the Sio2 sol, wherein the Ti-0-Si and surface Ratio, a mixture of Ti (X and z, potentials of the normal-temperature quick-solidification type nanometre Tio2 the stability.
A Tio2 the crystal seed: Rutile type titanium, and brookite. A compound of of the first two. Chamber, wherein the photo-catalysis degradation reaction, the catalytic activity of anatase titanium dioxide Tio2 and is higher than The rutile. , And the researchers discovered in recent years type treatment with the or the mixed crystal has a photo-catalysis activity, wherein the is a mixing crystal structure is capable of improving the electronic hole to the electrode, wherein the convex photo-catalysis efficiency. How use of a have the same literature report of the crystal The nanometre powder, such as follows: Net Zhenxing and adjusting (reporting the teaches audiences pharmaceutically acceptable iW /A of the synthetic structure, and photo-catalysis high performance dispersed nanometre titanium dioxide the crystal? 5J). A, the sol preparation, how to control the normal-temperature quick-solidification type nanometre Tio2 wherein the seed crystal expressed of not more is. Of reporting Yuzheng the low-temperature preparation of the crystal structure of ice Composition (sol is present to coagulation dives Aspirin Xiaoshu 7Y6yt^ and You Shuoyi sincerely/to claim handsome even the numerous sincere bearing ^^^W J7 (8 ): M and iO, and how of a given to control of the crystal seed crystal the method.
Of From is wide, light can absorb in the sunshine the ultraviolet part, a solar of factor is low. In order to a is a, which is necessary to further improves the normal-temperature quick-solidification type nanometre Tio2 the visible light according, wherein of ion-implantation 1-4, wherein the energy structure to change, preparing is capable of the titanium dioxide photo-catalytic catalytic material in the visible light activated, wherein said catalytic performance.
Use of a, the precipitating dispergation method to a nanometre titanium dioxide sol with a bottom application method. The method of using titanium alkoxide (such as follows: Purity of each, the used tetrabutyl ethyl ester, the used tetrabutyl C of ABR+OBR process in) and inorganic salt titanium (such as titanium tetrachloride, titanyl sulphate and so on) is a precursor, the nitric acid, hydrochloric acid, the tetraalkylammonium hydroxide according dike ammonium and administration of the dispergator. The titanium alkoxide to achieve the strictly controlled by reacting for preparing a, titanium alkoxide easy in the air, the organic reagent for is further and easy to give the sol introducing organic substance. , And the high cost of titanium alkoxide furthermore limited widespread the application of the method. The titanium inorganic salt to replace titanium alkoxide not can only be of the low-cost, and without the organic solvent, wherein r is a environment-friendly. D. the s.lee -51/^5 Z-A: Z/ZZ corpse re/? arati friend 7YQ? s (x/i/57'/? 7j g. THE 厶 and a precorsor. /o of /77a7 of 5b_Z-5 "" .e/? friend and c/7^ is /7 ^0 耵. The 7 ' beach W) of the titanium tetrachloride to a sol For preparing the compound, a chemical component of the acid sol, and grain Is U-SHAPED Tuyue. Roasting Tong-Xu (a2 7b/^_Z etc. 7Yft strength is /orosa/51 v/t is? acL. K/f/is zar^ws #Weriah. Endured 7 to 0 degrees centigrade W7,5^ human) of the titanyl sulphate and metatitanic acid of producing 1102 sols for preparing, and a studied sample by and gas and. Similarly, preparing catalyst is further acid sol. The preparation method of compound of CN101049962A claimed is a neutral nanometre titanium dioxide sol, and chemical H2O2 introduced to the corrosive reagent as the complexing agent is the preparation method, the sol obtained in pale - yellow, and structure is pure anatase. A Japanese claim JP2005-169160 claimed in one of the titanium tetrachloride for preparing, preparing the Sio2 is coated with The (a method of sol V, and sol has effect of ultraviolet shield, which is used for photo-catalysis by organic matter the field. A contents: A objective of the present invention provides a high and crystal with controllable nanometre Tio2 the hydrosol preparation method. The preparation method of the invention claims a high and crystal with controllable nanometre Tio2, hydrosol the is characterised according to the following preparation method and steps: a. Titanium compound by weight: Is the titanium compound is the raw material; precipitating the titanium compound in the alkali solution; The titanium compound of any one of titanium tetrachloride, metatitanic acid or titanyl sulphate; The alkali solution is ammonia water or sodium hydroxide solution; b. The washing: The process according to the de-ionized water of the obtained reaction, less than 100y S/cm until the conductivity of filtering;
c. A acid: dispergationAccording to the titanium compound and acid solution Ratio is 1 to 2): 1), To obtain the filter cakes adding acid; The method according to any one of nitric acid, hydrochloric acid or sulphuric acid; Is (DEGREES centigrade dispergation lengthways (r60min to 6, TlO
d. The stabilizer and dopant: Adding a certain amount of the Sio2 sol and metal salt, the reaction sustained 0.5 and .0 hours; The adding amount of Sio2 sol is the sol total amount to 10%; A role is a will and Tio2 and sol is wherein the requirement; The adding amount of the metal salt is the sol total amount of 0.01% to 0.8%; A function of the doped with modified to The nanometre, adjusting the crystal The type of rutile-type and; andThe metal salt is Fe (NO phenyl SnCl4, and Zn (L) 2 or any one of r1 And N03 (3). The pH value of alkalizing regulating solution: The ph of the solution with the alkali the pH value to 7 to 10;
f. The washing: Wherein the filtering solution, the deionized water washing is precipitated, until the conductivity of filtering is less than or teaches S/cm:
g.: dispersingAccording to the solid content claim, wherein the obtained and of the following water, dispersing, the neutral and nanometre Tio2 hydrosol compound; The hydrosol or 02 丌 content is 1 to 5%; The ratio of the type of rutile-type crystal is the: O. the or O. the is one controllable.
The invention method power and as FORMULA (1) invention method according Ti (V transparencies sol is good, wherein the is excellent; the crystallization degree is high, the photochemical catalysis effect of preceding claims, wherein of the flocculation or precipitated.
(2) The sol Ratio of the invention preparation method, wherein p^6 to 8, and neutral hydrosols, does not comprise an organic substance, the preparation process assistant environment-friendly. The concrete the application, is ladder-shaped is spray coating, which is selected such that the corrosion destruction to the substrate.
(3) Invention is chemical to precipitate and method for dispergation, and a lower than 10 DEGREES the condition for preparing anatase and rutile of the nanometre Tio2 sol.
(4) The invention is added that the metal salt is added to the doped to the nanometre Tio2 And. of the crystal and anatase titanium oxide is based on the controllable, wherein broadened the nanometre Tio2 as determined from.
(5) The invention, wherein the Sio2 sol can be of Ti (V sol and z potentials thereof, and The (a roles of V sol, so of the stable The neutral hydrosol.
detailed description of illustrated embodiments
: Presently concrete substantially as narration of the invention is.
Substantially as the:
The preparation method of step of the compulsive is as follows: The substantially as hydrosol The comprising and weight percents control is: 4% The Sio2, 2.5%, metal salt SnCl4, 0.5% of 93% water.
The titanium tetrachloride of the raw material, and wherein in the water solution is. Is added to a stirring and sodium hydroxide solution is titanium tetrachloride solution, and pH value of the solution is regulated to; neutralWherein the reaction is finished; the filtering, and depositing of the deionized water washing reaction to obtain, less than 100iiS/cm until the conductivity of filtering. Then adding acid dispergation, adding nitric acid solution, according to titanium tetrachloride to nitric acid Is 1.4: to the proportion of the nitric acid, and base dispergation at 95 ' C. Then adding a certain amount SiCV the sol and metal salt SnCl4, wherein that digesting the reaction 2 hours; Alkalifies and fluid in the solution the pH value to 7. Then filtering, washing, the deionized water washing is precipitated, less than 100uS/cm until the conductivity of filtering. Then dissolving the obtained and of the following water, dispersing, finally obtaining the neutral and nanometre Tio2 hydrosol compound. The hydrosol Tio2 the absolute value of the z potential's is greater than 50mV.
The degradation of method of the invention is obtained as The: hydrosolThe 10mg/L ml of methylene and active bright red X-3B or methyl orange solution, adding. 7ml of The obtained
The hydrosol, stirring under the conditions the sunshine the time is 1-3, wherein the neurodegenerative. The test result, wherein the dye solution a neurodegenerative of 2 hours rate of 95°/. The.
Nanometre Tio2 sol wherein the crystal according invention prepared for anatase titanium oxide and crystal, and reaction conditions can control the seed crystal proportion, doped with metal iron ion or tin or the zinc or the cerium sol, wherein a spectral reaction of ratio of the purity of The. The hydrosol Ratio of the invention method prepared from and neutral, the transparency is high, which is easy to preservation, wherein of the flocculation, absence corrosiveness, and photochemical catalysis effect is further.
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2 members in 1 office
Priority claims2
| Document | Office | Kind | Date |
|---|---|---|---|
| 200810040018 | China | A | |
| CN2008140018 | – | – | – |
Members2
| Document | Office | Kind | |
|---|---|---|---|
| CN101306838AThis record | China | A | |
| CN101306838B | China | B |
Numbers
- Publication
- 101306838
- Publication, DOCDB
- 101306838
- Publication, EPODOC
- CN101306838
- Application
- 100400189
- Application, DOCDB
- 200810040018
- Application, EPODOC
- CN2008140018
Titles2
- English
- Method for preparing high- stable neutral mixed crystal nanometer TiO2 hydrosol
- Chinese
- 高稳定中性混晶纳米TiO<sub>2</sub>水溶胶的制备方法
Classification
- IPC, 2
- C01G23 053
- B01J21 06