CN108751252A - A kind of titanium dioxide process of size tunable - Google Patents
A kind of titanium dioxide process of size tunable Download PDFInfo
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- CN108751252A CN108751252A CN201810575124.0A CN201810575124A CN108751252A CN 108751252 A CN108751252 A CN 108751252A CN 201810575124 A CN201810575124 A CN 201810575124A CN 108751252 A CN108751252 A CN 108751252A
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- titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention discloses a kind of titanium dioxide process of size tunable, include the following steps：Step 1, ethyl cellulose is added into absolute ethyl alcohol, is stirred to being completely dissolved, obtain dispersion alcohol liquid；Step 2, tetrabutyl titanate is slowly added dropwise into dispersion alcohol liquid, stirs evenly rear stand at low temperature, obtains titanium alcohol liquid；Step 3, ultrasonic disperse is added into titanium alcohol liquid in methylcellulose and forms precipitated liquid；Step 4, low temperature is slowly added dropwise into precipitated liquid in distilled water to stir evenly, until being added dropwise to complete, then low temperature ultrasonic reacts 2-4h, heats ultrasonic reaction 2-4h, and constant temperature obtains suspended sol solutions；Step 5, gel is obtained using absolute ethyl alcohol constant temp after suspended sol solutions being filtered；Gradually 6, circulator bath ultrasonic reaction 2-5h, cold filtration is added into ultrasonic reaction kettle in gel and obtains nano-titanium dioxide.The present invention, as coating agent, tetrabutyl titanate is wrapped up, achievees the purpose that indirect control nano-titanium dioxide grain size using ethyl cellulose.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of titanium dioxide process of size tunable.
Background technology
Currently as the TiO of one of semiconductor light-catalyst2Catalysis material is a kind of Novel ring of current most study
Border friendly materials, the property of photochemical catalyst are the key factors in Photocatalytic Oxidation.TiO2Crystal form, grain size and grain
The factors such as diameter, surface state have larger impact to its photocatalysis performance.The big nano-particle of surface area due to its skin effect and
Bulk effect determines that it has good catalytic activity and selectivity.Nano-TiO2Since its quantum size effect makes it lead
Band and valence-band level become discrete energy levels, and energy gap broadens, and conduction band current potential becomes more negative, and the corrigendum that valence band current potential becomes, this meaning
It with stronger oxidation and reducing power；Again because the grain size of nano-particle is small, photo-generated carrier more holds than coarse granule
Easily surface is moved to from inside particles, hence it is evident that reduce electronics and the recombination probability in hole, be also beneficial to improve photocatalysis performance.
Therefore, the small TiO of large specific surface area, grain size is prepared2Have become the focus of photocatalysis field research.
As the improvement of people's living standards, environmentally conscious materials are more paid close attention to by people, titanium dioxide optical catalyst tool
Have that oxidation activity is high, catalytic performance is strong, activity stabilized, moisture resistance is good and the sterilizing ability excellent properties such as by force, in wastewater degradation, disappears
Removing and harmful gas, sterilization and purification air etc. are widely used.However the preparation side of existing titanium dioxide powder
Method, such as traditional solid phase reaction and sintering process and modern chemical vapour deposition technique, physical vaporous deposition, chemical vapor infiltration
Method, sol-gel processing etc., current preparation method complex steps, yield is unstable, and the particle diameter distribution prepared
Extensively, it is difficult to meet customer requirement.
Invention content
For the problems of the prior art, the present invention provides a kind of titanium dioxide process of size tunable, solves
The problem of existing nano-titanium dioxide size controlling difficulty is wrapped up tetrabutyl titanate using ethyl cellulose as coating agent,
Achieve the purpose that indirect control nano-titanium dioxide grain size.
To realize the above technical purpose, the technical scheme is that：
A kind of titanium dioxide process of size tunable, includes the following steps：
Step 1, ethyl cellulose is added into absolute ethyl alcohol, is stirred to being completely dissolved, obtain dispersion alcohol liquid；
Step 2, tetrabutyl titanate is slowly added dropwise into dispersion alcohol liquid, stirs evenly rear stand at low temperature, obtains titanium alcohol liquid；
Step 3, ultrasonic disperse is added into titanium alcohol liquid in methylcellulose and forms precipitated liquid；
Step 4, low temperature is slowly added dropwise into precipitated liquid in distilled water to stir evenly, until being added dropwise to complete, then low temperature is super
Phonoresponse 2-4h, heats ultrasonic reaction 2-4h, and constant temperature obtains suspended sol solutions；
Step 5, gel is obtained using absolute ethyl alcohol constant temp after suspended sol solutions being filtered；
Gradually 6, circulator bath ultrasonic reaction 2-5h is added into ultrasonic reaction kettle in gel, cold filtration obtains nanometer two
Titanium oxide.
A concentration of 50-100g/L of the ethyl cellulose in absolute ethyl alcohol in the step 1, the stirring speed of the stirring
Degree is 800-1400r/min.
The addition of tetrabutyl titanate in the step 2 is the 130-170% of ethyl cellulose quality, the stirring
Mixing speed is 500-800r/min, and the temperature of stand at low temperature is 1-7 DEG C, time of repose 1-3h.
The addition of methylcellulose in the step 3 is the 60-80% of ethyl cellulose quality.
The temperature of ultrasonic disperse in the step 3 is 50-60 DEG C, supersonic frequency 20-25kHz.
The addition of distilled water in the step 4 is the 90-130% of absolute ethyl alcohol quality, the dropwise addition speed being slowly added dropwise
Degree is 1-3mL/min, and the temperature of the low temperature stirring is 0-5 DEG C, mixing speed 1000-2000r/min.
The temperature of low temperature ultrasonic reaction in the step 4 is 5-10 DEG C, supersonic frequency 20-30kHz, and the heating is super
The temperature of phonoresponse is 60-70 DEG C, supersonic frequency 50-80kHz, and the temperature of the constant temperature is 70-75 DEG C.
The temperature of absolute ethyl alcohol constant temp in the step 5 is 60-70 DEG C.
Absolute ethyl alcohol is added again after the completion of ethyl alcohol washing in the step 5, then stirring distillation obtains gel, described
The temperature of stirring distillation is 75-85 DEG C, mixing speed 1000-2000r/min.
The supersonic frequency of circulator bath ultrasonic reaction in the step 6 is 50-70kHz, the temperature range of circulator bath
It is 20-50 DEG C, cycle period 10-20min.
Ethyl cellulose is dissolved in absolute ethyl alcohol by step 1, and forms quickly dissolving under agitation, is divided
Dissipate alcohol liquid.
Tetrabutyl titanate is dissolved in dispersion alcohol liquid by step 2, can be evenly dispersed to ethanol solution by tetrabutyl titanate
In；Ethyl cellulose disperses tetrabutyl titanate as dispersant, while being also used as coating agent, by tetrabutyl titanate material packet
It wraps up in, forms package dispersity.
Methylcellulose is added into titanium alcohol liquid step 3, can form suspension particles, is deposited on ethyl alcohol bottom, then
Under ultrasound condition, the tetrabutyl titanate of package status is made a breach, lost ethyl cellulose is acted on to methylcellulose
Surface, while capable of forming dispersion, methylcellulose forms suspended state, is evenly distributed in absolute ethyl alcohol.
Distilled water is added into precipitated liquid step 4, the exposed surface of tetrabutyl titanate can be utilized to be contacted with distilled water instead
It answers, reaches hydrolysis effect；Nano-titanium dioxide is formed after tetrabutyl titanate hydrolysis, and reaches outstanding under ethyl cellulose effect
Turbid dispersion effect, while distilled water can dissolve methylcellulose, and act on to nano-titanium dioxide surface, it is formed suspended
Liquid status；Low temperature ultrasonic reaction process can ensure that nano-titanium dioxide is dispersed in distilled water and ethanol system, cryogenic conditions
It can ensure that methylcellulose is dissolved in water, and not form colloidal sol, keep dissolved state；It heats in ultrasonic procedure, with temperature
The raising of degree, methylcellulose is slowly formed colloidal sol, and is gradually converted into gel, and nano-titanium dioxide is solidificated in gel,
With the effect of ultrasound, gel is constantly broken, continuous solidifyingization, after reaction the coagulant liquid under constant temperature.
Step 5 is filtered the absolute ethyl alcohol containing ethyl cellulose by way of filtering, is obtained cladding titanium dioxide and is received
The gel of rice corpuscles, and under the constant temp of absolute ethyl alcohol, remaining ethyl cellulose is cleaned, and constant temperature item
Methyl cellulose gel can be kept under part.
Step 6 can constantly be converted methylcellulose in gel by circulator bath ultrasonic reaction with dissolving, and
In the case where nano-titanium dioxide is exposed, ultrasonic clutch can form passivation, prevent from reuniting, while ultrasonic clutch can carry enough
Energy converts nano-titanium dioxide to anatase titanium dioxide；Methylcellulose is dissolved in water in the cooling condition, forms nano-silica
Change titanium suspension, nano-titanium dioxide is obtained by filtration.
From the above, it can be seen that the present invention has following advantages：
1. the present invention solves the problems, such as that existing nano-titanium dioxide size controlling is difficult, using ethyl cellulose as packet
Agent is wrapped up in, tetrabutyl titanate is wrapped up, achievees the purpose that indirect control nano-titanium dioxide grain size.
2. the present invention is ensured by the dispersibility of methylcellulose and ethyl cellulose in nano-titanium dioxide hydrolytic process
Dispersion effect, can ensure the package effect on nano-titanium dioxide surface.
3. the present invention makes full use of dissolubility variation of the different dispersants in different solvents, reach the effect of stable conversion
Fruit obtains the double control to form grain size.
4. the waste liquid that the present invention obtains contains a large amount of dispersants, recycling can be formed and made full use of.
Specific implementation mode
The specific embodiment that the present invention will be described in detail in conjunction with the embodiments, but the claim of the present invention is not done any
It limits.
Embodiment 1
A kind of titanium dioxide process of size tunable, includes the following steps：
Step 1, ethyl cellulose is added into absolute ethyl alcohol, is stirred to being completely dissolved, obtain dispersion alcohol liquid；
Step 2, tetrabutyl titanate is slowly added dropwise into dispersion alcohol liquid, stirs evenly rear stand at low temperature, obtains titanium alcohol liquid；
Step 3, ultrasonic disperse is added into titanium alcohol liquid in methylcellulose and forms precipitated liquid；
Step 4, low temperature is slowly added dropwise into precipitated liquid in distilled water to stir evenly, until being added dropwise to complete, then low temperature is super
Phonoresponse 2h, heats ultrasonic reaction 2h, and constant temperature obtains suspended sol solutions；
Step 5, gel is obtained using absolute ethyl alcohol constant temp after suspended sol solutions being filtered；
Gradually 6, circulator bath ultrasonic reaction 2h, cold filtration is added into ultrasonic reaction kettle in gel and obtains nano-silica
Change titanium.
A concentration of 50g/L of the ethyl cellulose in absolute ethyl alcohol in the step 1, the mixing speed of the stirring are
800r/min。
The addition of tetrabutyl titanate in the step 2 is the 130% of ethyl cellulose quality, the stirring of the stirring
Speed is 500r/min, and the temperature of stand at low temperature is 1 DEG C, time of repose 1h.
The addition of methylcellulose in the step 3 is the 60% of ethyl cellulose quality.
The temperature of ultrasonic disperse in the step 3 is 50 DEG C, supersonic frequency 20kHz.
The addition of distilled water in the step 4 is the 90% of absolute ethyl alcohol quality, and the rate of addition being slowly added dropwise is
The temperature of 1mL/min, the low temperature stirring are 0 DEG C, mixing speed 1000r/min.
The temperature of low temperature ultrasonic reaction in the step 4 is 5 DEG C, supersonic frequency 20kHz, the heating ultrasonic reaction
Temperature be 60 DEG C, supersonic frequency 50kHz, the temperature of the constant temperature is 70 DEG C.
The temperature of absolute ethyl alcohol constant temp in the step 5 is 60 DEG C.
Absolute ethyl alcohol is added again after the completion of ethyl alcohol washing in the step 5, then stirring distillation obtains gel, described
The temperature of stirring distillation is 75 DEG C, mixing speed 1000r/min.
The supersonic frequency of circulator bath ultrasonic reaction in the step 6 is 50kHz, and the temperature range of circulator bath is
20-50 DEG C, cycle period 10min.
Embodiment 2
A kind of titanium dioxide process of size tunable, includes the following steps：
Step 1, ethyl cellulose is added into absolute ethyl alcohol, is stirred to being completely dissolved, obtain dispersion alcohol liquid；
Step 2, tetrabutyl titanate is slowly added dropwise into dispersion alcohol liquid, stirs evenly rear stand at low temperature, obtains titanium alcohol liquid；
Step 3, ultrasonic disperse is added into titanium alcohol liquid in methylcellulose and forms precipitated liquid；
Step 4, low temperature is slowly added dropwise into precipitated liquid in distilled water to stir evenly, until being added dropwise to complete, then low temperature is super
Phonoresponse 4h, heats ultrasonic reaction 4h, and constant temperature obtains suspended sol solutions；
Step 5, gel is obtained using absolute ethyl alcohol constant temp after suspended sol solutions being filtered；
Gradually 6, circulator bath ultrasonic reaction 5h, cold filtration is added into ultrasonic reaction kettle in gel and obtains nano-silica
Change titanium.
A concentration of 100g/L of the ethyl cellulose in absolute ethyl alcohol in the step 1, the mixing speed of the stirring
For 1400r/min.
The addition of tetrabutyl titanate in the step 2 is the 170% of ethyl cellulose quality, the stirring of the stirring
Speed is 800r/min, and the temperature of stand at low temperature is 7 DEG C, time of repose 3h.
The addition of methylcellulose in the step 3 is the 80% of ethyl cellulose quality.
The temperature of ultrasonic disperse in the step 3 is 60 DEG C, supersonic frequency 25kHz.
The addition of distilled water in the step 4 is the 130% of absolute ethyl alcohol quality, and the rate of addition being slowly added dropwise is
The temperature of 3mL/min, the low temperature stirring are 5 DEG C, mixing speed 2000r/min.
The temperature of low temperature ultrasonic reaction in the step 4 is 10 DEG C, supersonic frequency 30kHz, and the heating ultrasound is anti-
The temperature answered is 70 DEG C, supersonic frequency 80kHz, and the temperature of the constant temperature is 75 DEG C.
The temperature of absolute ethyl alcohol constant temp in the step 5 is 70 DEG C.
Absolute ethyl alcohol is added again after the completion of ethyl alcohol washing in the step 5, then stirring distillation obtains gel, described
The temperature of stirring distillation is 85 DEG C, mixing speed 2000r/min.
The supersonic frequency of circulator bath ultrasonic reaction in the step 6 is 70kHz, and the temperature range of circulator bath is
20-50 DEG C, cycle period 20min.
Embodiment 3
A kind of titanium dioxide process of size tunable, includes the following steps：
Step 1, ethyl cellulose is added into absolute ethyl alcohol, is stirred to being completely dissolved, obtain dispersion alcohol liquid；
Step 2, tetrabutyl titanate is slowly added dropwise into dispersion alcohol liquid, stirs evenly rear stand at low temperature, obtains titanium alcohol liquid；
Step 3, ultrasonic disperse is added into titanium alcohol liquid in methylcellulose and forms precipitated liquid；
Step 4, low temperature is slowly added dropwise into precipitated liquid in distilled water to stir evenly, until being added dropwise to complete, then low temperature is super
Phonoresponse 3h, heats ultrasonic reaction 3h, and constant temperature obtains suspended sol solutions；
Step 5, gel is obtained using absolute ethyl alcohol constant temp after suspended sol solutions being filtered；
Gradually 6, circulator bath ultrasonic reaction 4h, cold filtration is added into ultrasonic reaction kettle in gel and obtains nano-silica
Change titanium.
A concentration of 80g/L of the ethyl cellulose in absolute ethyl alcohol in the step 1, the mixing speed of the stirring are
1200r/min。
The addition of tetrabutyl titanate in the step 2 is the 150% of ethyl cellulose quality, the stirring of the stirring
Speed is 600r/min, and the temperature of stand at low temperature is 4 DEG C, time of repose 2h.
The addition of methylcellulose in the step 3 is the 70% of ethyl cellulose quality.
The temperature of ultrasonic disperse in the step 3 is 55 DEG C, supersonic frequency 23kHz.
The addition of distilled water in the step 4 is the 120% of absolute ethyl alcohol quality, and the rate of addition being slowly added dropwise is
The temperature of 2mL/min, the low temperature stirring are 2 DEG C, mixing speed 1500r/min.
The temperature of low temperature ultrasonic reaction in the step 4 is 8 DEG C, supersonic frequency 25kHz, the heating ultrasonic reaction
Temperature be 65 DEG C, supersonic frequency 70kHz, the temperature of the constant temperature is 73 DEG C.
The temperature of absolute ethyl alcohol constant temp in the step 5 is 65 DEG C.
Absolute ethyl alcohol is added again after the completion of ethyl alcohol washing in the step 5, then stirring distillation obtains gel, described
The temperature of stirring distillation is 80 DEG C, mixing speed 1500r/min.
The supersonic frequency of circulator bath ultrasonic reaction in the step 6 is 60kHz, and the temperature range of circulator bath is
20-50 DEG C, cycle period 15min.
Performance detection
In conclusion the present invention has the following advantages：
1. the present invention solves the problems, such as that existing nano-titanium dioxide size controlling is difficult, using ethyl cellulose as packet
Agent is wrapped up in, tetrabutyl titanate is wrapped up, achievees the purpose that indirect control nano-titanium dioxide grain size.
2. the present invention is ensured by the dispersibility of methylcellulose and ethyl cellulose in nano-titanium dioxide hydrolytic process
Dispersion effect, can ensure the package effect on nano-titanium dioxide surface.
3. the present invention makes full use of dissolubility variation of the different dispersants in different solvents, reach the effect of stable conversion
Fruit obtains the double control to form grain size.
4. the waste liquid that the present invention obtains contains a large amount of dispersants, recycling can be formed and made full use of.
It is understood that above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to this
Technical solution described in inventive embodiments.It will be understood by those of ordinary skill in the art that still can be carried out to the present invention
Modification or equivalent replacement, to reach identical technique effect；As long as meet use needs, all protection scope of the present invention it
It is interior.
Claims (10)
1. a kind of titanium dioxide process of size tunable, it is characterised in that：Include the following steps：
Step 1, ethyl cellulose is added into absolute ethyl alcohol, is stirred to being completely dissolved, obtain dispersion alcohol liquid；
Step 2, tetrabutyl titanate is slowly added dropwise into dispersion alcohol liquid, stirs evenly rear stand at low temperature, obtains titanium alcohol liquid；
Step 3, ultrasonic disperse is added into titanium alcohol liquid in methylcellulose and forms precipitated liquid；
Step 4, low temperature is slowly added dropwise into precipitated liquid in distilled water to stir evenly, until being added dropwise to complete, then low temperature ultrasonic is anti-
2-4h is answered, ultrasonic reaction 2-4h is heated, constant temperature obtains suspended sol solutions；
Step 5, gel is obtained using absolute ethyl alcohol constant temp after suspended sol solutions being filtered；
Gradually 6, circulator bath ultrasonic reaction 2-5h, cold filtration is added into ultrasonic reaction kettle in gel and obtains nanometer titanium dioxide
Titanium.
2. a kind of titanium dioxide process of size controlling according to claim 1, it is characterised in that：The step 1
In a concentration of 50-100g/L of the ethyl cellulose in absolute ethyl alcohol, the mixing speed of the stirring is 800-1400r/
min。
3. a kind of titanium dioxide process of size controlling according to claim 1, it is characterised in that：The step 2
In tetrabutyl titanate addition be ethyl cellulose quality 130-170%, the mixing speed of the stirring is 500-
The temperature of 800r/min, stand at low temperature are 1-7 DEG C, time of repose 1-3h.
4. a kind of titanium dioxide process of size controlling according to claim 1, it is characterised in that：The step 3
In methylcellulose addition be ethyl cellulose quality 60-80%.
5. a kind of titanium dioxide process of size controlling according to claim 1, it is characterised in that：The step 3
In ultrasonic disperse temperature be 50-60 DEG C, supersonic frequency 20-25kHz.
6. a kind of titanium dioxide process of size controlling according to claim 1, it is characterised in that：The step 4
In distilled water addition be absolute ethyl alcohol quality 90-130%, the rate of addition being slowly added dropwise be 1-3mL/min, it is described
The temperature of low temperature stirring is 0-5 DEG C, mixing speed 1000-2000r/min.
7. a kind of titanium dioxide process of size controlling according to claim 1, it is characterised in that：The step 4
In the temperature of low temperature ultrasonic reaction be 5-10 DEG C, supersonic frequency 20-30kHz, the temperature of the heating ultrasonic reaction is 60-
70 DEG C, supersonic frequency 50-80kHz, the temperature of the constant temperature is 70-75 DEG C.
8. a kind of titanium dioxide process of size controlling according to claim 1, it is characterised in that：The step 5
In absolute ethyl alcohol constant temp temperature be 60-70 DEG C.
9. a kind of titanium dioxide process of size controlling according to claim 1, it is characterised in that：The step 5
In ethyl alcohol washing after the completion of absolute ethyl alcohol is added again, then stirring distillation obtains gel, and the temperature of the stirring distillation is
75-85 DEG C, mixing speed 1000-2000r/min.
10. a kind of titanium dioxide process of size controlling according to claim 1, it is characterised in that：The step 6
In the supersonic frequency of circulator bath ultrasonic reaction be 50-70kHz, the temperature range of circulator bath is 20-50 DEG C, cycle period
For 10-20min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109205664A (en) * | 2018-11-08 | 2019-01-15 | 绍兴文理学院 | A kind of method that electrostatic spinning prepares nano-titanium dioxide |
| CN111299591A (en) * | 2020-04-15 | 2020-06-19 | 无锡乐普金属科技有限公司 | Preparation method of tungsten-copper alloy plate |
| CN111410756A (en) * | 2020-04-22 | 2020-07-14 | 无锡嘉弘塑料科技有限公司 | Preparation method of weather-resistant polyvinyl chloride granules |
| CN114477279A (en) * | 2022-01-19 | 2022-05-13 | 陕西瑞科新材料股份有限公司 | Green preparation method of nano titanium dioxide |
| CN115490455A (en) * | 2022-10-09 | 2022-12-20 | 临沂海螺新材料科技有限公司 | Low-doping-amount enhanced cement grinding aid and preparation method thereof |
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| CN1097400A (en) * | 1994-04-28 | 1995-01-18 | 雷亚林 | The manufacture method of super fine powder of titanium dioxide |
| CN105936514A (en) * | 2016-06-12 | 2016-09-14 | 长兴中昊化工有限公司 | Making process of rutile type titanium dioxide nano-powder |
| CN106976907A (en) * | 2017-04-27 | 2017-07-25 | 吴亚良 | A kind of nano titanium oxide preparation method of size tunable |
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| CN1097400A (en) * | 1994-04-28 | 1995-01-18 | 雷亚林 | The manufacture method of super fine powder of titanium dioxide |
| CN105936514A (en) * | 2016-06-12 | 2016-09-14 | 长兴中昊化工有限公司 | Making process of rutile type titanium dioxide nano-powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109205664A (en) * | 2018-11-08 | 2019-01-15 | 绍兴文理学院 | A kind of method that electrostatic spinning prepares nano-titanium dioxide |
| CN111299591A (en) * | 2020-04-15 | 2020-06-19 | 无锡乐普金属科技有限公司 | Preparation method of tungsten-copper alloy plate |
| CN111410756A (en) * | 2020-04-22 | 2020-07-14 | 无锡嘉弘塑料科技有限公司 | Preparation method of weather-resistant polyvinyl chloride granules |
| CN114477279A (en) * | 2022-01-19 | 2022-05-13 | 陕西瑞科新材料股份有限公司 | Green preparation method of nano titanium dioxide |
| CN115490455A (en) * | 2022-10-09 | 2022-12-20 | 临沂海螺新材料科技有限公司 | Low-doping-amount enhanced cement grinding aid and preparation method thereof |
| CN115490455B (en) * | 2022-10-09 | 2023-08-18 | 临沂海螺新材料科技有限公司 | Low-doping-amount enhanced cement grinding aid and preparation method thereof |
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| CN108751252B (en) | 2020-05-19 |
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