CN105504886A - Preparation method of modified hollow TiO2 microspheres - Google Patents
Preparation method of modified hollow TiO2 microspheres Download PDFInfo
- Publication number
- CN105504886A CN105504886A CN201510905106.0A CN201510905106A CN105504886A CN 105504886 A CN105504886 A CN 105504886A CN 201510905106 A CN201510905106 A CN 201510905106A CN 105504886 A CN105504886 A CN 105504886A
- Authority
- CN
- China
- Prior art keywords
- hollow
- tio2
- mps
- microballoon
- dehydrated alcohol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3669—Treatment with low-molecular organic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a preparation method of modified hollow TiO2 microspheres. The preparation method comprises the following steps of putting dried PS (Poly Styrene)/TiO2 composite powder in a muffle furnace, drying for one hour, and enabling absolute ethyl alcohol to be totally evaporated; rising the temperature, and calcining for two hours, thus finally obtaining hollow TiO2 microspheres; adding the calcined hollow TiO2 microspheres in the absolute ethyl alcohol, and carrying out ultrasonic treatment for one hour; then adding MPS (Modified Poly Styrene), ammonium hydroxide and deionized water; putting the hollow TiO2 microspheres in an oil bath pan to carry out a reaction under room temperature, then washing by using the absolute ethyl alcohol, and carrying out centrifugal separation, thus obtaining MPS-TiO2. The preparation method disclosed by the invention has the advantages that the preparation method is simple, the cost is low, the particle size of the prepared MPS-TiO2 is larger, and better heat insulation and sound insulation effects are obtained.
Description
Technical field
The present invention relates to a kind of composite coating, particularly relate to the hollow TiO2 method for preparing microsphere of a kind of modification.
Background technology
Ti02 has excellent physics and chemistry character, is commonly used for the filler of fine materials.It has high refractive index, high dielectric property and high-melting-point.Just because of its advantage, be all applied, as light at a lot of material
Electricity material, photocatalyst material and semiconductor material etc.Because Ti02 has excellent optical property, it is excellent white pigment.Usually, the specific refractory power of pigment is most important physical properties, because this physical property determines reducing power and the opacifying power of pigment.Due to when using Ti02 as color stuffing, the utilization of its optical property and pigment performance is all confined to the top layer of particle, and the effect that will reach, its particle size must reach certain value, otherwise the reflectivity of visible region is not high, be not fully utilized causing the kernel portion of occupying significant proportion.Relative to other white pigment, the value of Ti02 is much expensive again, therefore can prepare the material of core/shell type, so just can utilize cheap raw material substitution kernel, by its Surface coating one deck Ti02.So not only play Ti02 pigment performance, and the consumption of Ti02 can have been saved well, thus reduce preparation cost.The method preparing Ti02 particle mainly comprises Physical and chemical method, and wherein Physical comprises: vapour deposition process, high-energy ball milling method, plasma method, ermal physics method, evaporation. coacervation and Amorphous Crystallization method; Chemical method comprises: metal alkoxide hydrolysis method, colloidal sol. gel method, liquid-phase precipitation method, hydrothermal method, colloidal sol extraction process, microemulsion method, gas phase hydrolysis method and vapour phase oxidation process.Colloidal sol coacervation, because preparation method is simple, cost is low, therefore generally uses in an experiment.
Summary of the invention
It is simple, with low cost that technical problem to be solved by this invention is to provide a kind of method, and the particle diameter of preparation is comparatively large, has the hollow TiO2 method for preparing microsphere of modification that is heat insulation and soundproof effect preferably.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: the hollow TiO2 method for preparing microsphere of a kind of modification, comprises the steps:
Dried PS/Ti02 composite powder is placed in retort furnace, dry one hour, dehydrated alcohol is evaporated completely;
Temperature is raised, calcines two hours, finally obtain hollow Ti02 microballoon;
Hollow Ti02 microballoon after calcining is added in dehydrated alcohol, ultrasonic 1h;
Add MPS, ammoniacal liquor and deionized water;
Place in oil bath pan and react under room temperature, afterwards with absolute ethanol washing and centrifugation, prepare MPS-Ti02.
On the basis of technique scheme, the present invention can also do following improvement
Further, described by dried PS/Ti02 composite powder placement retort furnace, dry one hour, make dehydrated alcohol evaporate being implemented as follows of step completely:
Placed in retort furnace by dried PS/Ti02 composite powder, 80-120 DEG C of inner drying one hour, makes dehydrated alcohol evaporate completely.
Further, described by temperature rising, calcine two hours, finally obtain being implemented as follows of hollow Ti02 microballoon step:
Temperature is risen to 500-550 DEG C, calcines two hours, finally obtain hollow Ti02 microballoon.
Further, described by calcining after hollow Ti02 microballoon add in dehydrated alcohol, being implemented as follows of ultrasonic 1h step:
O.05-0.08g the hollow Ti02 microballoon after calcining is added in 50-100mL dehydrated alcohol, ultrasonic 1-2h.
Further, being implemented as follows of MPS, ammoniacal liquor and deionized water step is added described in:
Add O.03-0.035gMPS, 0.04-0.06g ammoniacal liquor and 0.06-0.055g deionized water.
Further, react under room temperature in described placement oil bath pan, afterwards with absolute ethanol washing and centrifugation, prepare being implemented as follows of MPS-Ti02 step:
Place in oil bath pan and react 48-60h under room temperature, afterwards with absolute ethanol washing and centrifugation, prepare MPS-Ti02.
The invention has the beneficial effects as follows: method is simple, with low cost, the particle diameter of preparation is comparatively large, has heat insulation and soundproof effect preferably.
Embodiment
Be described principle of the present invention and feature below in conjunction with example, example, only for explaining the present invention, is not intended to limit scope of the present invention.
The hollow TiO2 method for preparing microsphere of a kind of modification, comprises the steps:
Dried PS/Ti02 composite powder is placed in retort furnace, dry one hour, dehydrated alcohol is evaporated completely;
Temperature is raised, calcines two hours, finally obtain hollow Ti02 microballoon;
Hollow Ti02 microballoon after calcining is added in dehydrated alcohol, ultrasonic 1h;
Add MPS, ammoniacal liquor and deionized water;
Place in oil bath pan and react under room temperature, afterwards with absolute ethanol washing and centrifugation, prepare MPS-Ti02.
Embodiment 1:
Placed in retort furnace by dried PS/Ti02 composite powder, 80 DEG C of inner dryings one hour, make dehydrated alcohol evaporate completely; Temperature is risen to 500 DEG C, calcine two hours, finally obtain hollow Ti02 microballoon; O.05g the hollow Ti02 microballoon after calcining is added in 50mL dehydrated alcohol, ultrasonic 1h;
Add O.03gMPS, 0.04g ammoniacal liquor and 0.06g deionized water; Place in oil bath pan and react 48h under room temperature, afterwards with absolute ethanol washing and centrifugation, prepare MPS-Ti02.
Embodiment 2:
Placed in retort furnace by dried PS/Ti02 composite powder, 90 DEG C of inner dryings one hour, make dehydrated alcohol evaporate completely; Temperature is risen to 520 DEG C, calcine two hours, finally obtain hollow Ti02 microballoon; O.06g the hollow Ti02 microballoon after calcining is added in 60mL dehydrated alcohol, ultrasonic 1.5h; Add O.033gMPS, 0.05g ammoniacal liquor and 0.07g deionized water; Place in oil bath pan and react 50h under room temperature, afterwards with absolute ethanol washing and centrifugation, prepare MPS-Ti02.
Embodiment 3:
Placed in retort furnace by dried PS/Ti02 composite powder, 120 DEG C of inner dryings one hour, make dehydrated alcohol evaporate completely; Temperature is risen to 550 DEG C, calcine two hours, finally obtain hollow Ti02 microballoon; O.055g the hollow Ti02 microballoon after calcining is added in 80mL dehydrated alcohol, ultrasonic 2h; Add O.035gMPS, 0.05g ammoniacal liquor and 0.08g deionized water; Place in oil bath pan and react 60h under room temperature, afterwards with absolute ethanol washing and centrifugation, prepare MPS-Ti02.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. the hollow TiO2 method for preparing microsphere of modification, is characterized in that, comprise the steps:
Dried PS/Ti02 composite powder is placed in retort furnace, dry one hour, dehydrated alcohol is evaporated completely;
Temperature is raised, calcines two hours, finally obtain hollow Ti02 microballoon;
Hollow Ti02 microballoon after calcining is added in dehydrated alcohol, ultrasonic 1h;
Add MPS, ammoniacal liquor and deionized water;
Place in oil bath pan and react under room temperature, afterwards with absolute ethanol washing and centrifugation, prepare MPS-Ti02.
2. the hollow TiO2 method for preparing microsphere of a kind of modification according to claim 1, is characterized in that, describedly places in retort furnace by dried PS/Ti02 composite powder, dry one hour, makes dehydrated alcohol evaporate being implemented as follows of step completely:
Placed in retort furnace by dried PS/Ti02 composite powder, 80-120 DEG C of inner drying one hour, makes dehydrated alcohol evaporate completely.
3. the hollow TiO2 method for preparing microsphere of a kind of modification according to claim 1, is characterized in that, describedly temperature is raised, and calcines two hours, finally obtains being implemented as follows of hollow Ti02 microballoon step:
Temperature is risen to 500-550 DEG C, calcines two hours, finally obtain hollow Ti02 microballoon.
4. the hollow TiO2 method for preparing microsphere of a kind of modification according to claim 1, is characterized in that, describedly adds in dehydrated alcohol by the hollow Ti02 microballoon after calcining, being implemented as follows of ultrasonic 1h step:
O.05-0.08g the hollow Ti02 microballoon after calcining is added in 50-100mL dehydrated alcohol, ultrasonic 1-2h.
5. the hollow TiO2 method for preparing microsphere of a kind of modification according to claim 1, is characterized in that, described in add being implemented as follows of MPS, ammoniacal liquor and deionized water step:
Add O.03-0.035gMPS, 0.04-0.06g ammoniacal liquor and 0.06-0.055g deionized water.
6. the hollow TiO2 method for preparing microsphere of a kind of modification according to claim 1, is characterized in that, react in described placement oil bath pan under room temperature, afterwards with absolute ethanol washing and centrifugation, prepares being implemented as follows of MPS-Ti02 step:
Place in oil bath pan and react 48-60h under room temperature, afterwards with absolute ethanol washing and centrifugation, prepare MPS-Ti02.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510905106.0A CN105504886A (en) | 2015-12-10 | 2015-12-10 | Preparation method of modified hollow TiO2 microspheres |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510905106.0A CN105504886A (en) | 2015-12-10 | 2015-12-10 | Preparation method of modified hollow TiO2 microspheres |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105504886A true CN105504886A (en) | 2016-04-20 |
Family
ID=55713205
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510905106.0A Pending CN105504886A (en) | 2015-12-10 | 2015-12-10 | Preparation method of modified hollow TiO2 microspheres |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105504886A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109207066A (en) * | 2018-08-08 | 2019-01-15 | 佛山科学技术学院 | A kind of aquosity heat insulating heat preserving paint and preparation method thereof |
| CN109534685A (en) * | 2018-11-23 | 2019-03-29 | 陕西科技大学 | A kind of schemochrome film of underwater oleophobic and its preparation method and application |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1631906A (en) * | 2003-12-23 | 2005-06-29 | 中国科学院理化技术研究所 | Process for preparing monodispersity shell/core composite granular emulsion by using nano silicon dioxide microsphere coated by polystyrene |
| CN1772363A (en) * | 2004-11-11 | 2006-05-17 | 中国科学院化学研究所 | Template process of preparing hollow ball and composite hollow ball |
| CN101559951A (en) * | 2009-05-15 | 2009-10-21 | 江苏大学 | Method for preparing nanoscale silica hollow microspheres |
| CN104477921A (en) * | 2014-11-04 | 2015-04-01 | 齐鲁工业大学 | Pomegranate-shaped multicore-shell SiO2-TiO2 composite material and preparation method thereof |
| CN104525067A (en) * | 2014-12-11 | 2015-04-22 | 同济大学 | Functional composite microsphere with pomegranate-shaped structure and preparation method of functional composite microsphere |
-
2015
- 2015-12-10 CN CN201510905106.0A patent/CN105504886A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1631906A (en) * | 2003-12-23 | 2005-06-29 | 中国科学院理化技术研究所 | Process for preparing monodispersity shell/core composite granular emulsion by using nano silicon dioxide microsphere coated by polystyrene |
| CN1772363A (en) * | 2004-11-11 | 2006-05-17 | 中国科学院化学研究所 | Template process of preparing hollow ball and composite hollow ball |
| CN101559951A (en) * | 2009-05-15 | 2009-10-21 | 江苏大学 | Method for preparing nanoscale silica hollow microspheres |
| CN104477921A (en) * | 2014-11-04 | 2015-04-01 | 齐鲁工业大学 | Pomegranate-shaped multicore-shell SiO2-TiO2 composite material and preparation method thereof |
| CN104525067A (en) * | 2014-12-11 | 2015-04-22 | 同济大学 | Functional composite microsphere with pomegranate-shaped structure and preparation method of functional composite microsphere |
Non-Patent Citations (2)
| Title |
|---|
| 安永: "中空氧化钛粒子的表面改性及其电泳显示液的制备", 《天津大学硕士学位论文》 * |
| 王彩艳: "中空电泳粒子的制备及电泳性能研究", 《天津大学硕士学位论文》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109207066A (en) * | 2018-08-08 | 2019-01-15 | 佛山科学技术学院 | A kind of aquosity heat insulating heat preserving paint and preparation method thereof |
| CN109534685A (en) * | 2018-11-23 | 2019-03-29 | 陕西科技大学 | A kind of schemochrome film of underwater oleophobic and its preparation method and application |
| CN109534685B (en) * | 2018-11-23 | 2021-08-27 | 陕西科技大学 | Underwater oleophobic structural color film and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102206445B (en) | Heat insulating coating surface glue and heat insulating coating | |
| CN107140606B (en) | A kind of preparation method of oxide hollow microsphere | |
| CN102286243A (en) | Method for preparing solar selective heat absorbing paint by using spinel type pigment as light absorbent | |
| CN101786900B (en) | Preparation method of quaternary xerogel | |
| CN103949193A (en) | Universal method for preparation of inorganic hollow microspheres | |
| CN105504886A (en) | Preparation method of modified hollow TiO2 microspheres | |
| CN103736502B (en) | A kind of composite semiconductor light-catalyst and application thereof | |
| CN105642262A (en) | Two-dimensional-layered titanium-dioxide nanometer photocatalytic material and preparing method | |
| CN103897667A (en) | Solar heat storage material taking kaolin as supporting basal body and preparation method of solar heat storage material | |
| CN105129857A (en) | Flower-shaped tungsten oxide nanometer material and preparing method thereof | |
| CN104785180A (en) | Method for preparing hollow microsphere taking silicon dioxide as inner shell layer and titanium dioxide as outer shell layer | |
| CN103977780A (en) | Method for preparing mesoporous carbon loaded TiO2 (titanium dioxide) photocatalysis material in two-step hydrothermal method | |
| CN104084096A (en) | Method for preparing TiO2@SiO2 core-shell particles with solar heat reflection function | |
| CN102249275B (en) | Method for preparing photoelectric-grade high-purity alumina with high sintering activity | |
| CN105462452A (en) | Anti-ultraviolet and anti-aging powder coating added with nano titanium dioxide | |
| CN104179066B (en) | A kind of production method for decorative laminate Rutile type titanium dioxide | |
| CN111018528A (en) | Low-emissivity ceramic material under 3-5 mu m wave band and preparation method thereof | |
| CN106629753A (en) | Preparation method of SiO2 aerogel and doped TiO2 composite | |
| CN107746074B (en) | A kind of titanium dioxide of core-shell structure mesoporous material and preparation method thereof with cavity | |
| CN104556193B (en) | Hot assisting sol-the gel method of a kind of employing prepares Sm2o3/ SnO2the method of nano-complex | |
| CN101348255A (en) | Method for preparing hydrophobic silica aerogel from rice husk ash based aquagel | |
| CN104071821B (en) | A kind of homogeneous phase hydrothermal method that adopts prepares Sm (OH) 3the method of/ZnO laminated film | |
| CN104051163B (en) | The preparation method of compound dielectric film aluminum electrode foil | |
| CN103871749B (en) | A kind of dye-sensitized solar cell anode film light scattering layer and preparation method thereof | |
| CN106147472A (en) | A kind of heat insulating coatings and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160420 |