CN110498444A - A kind of low temperature process preparation nano material - Google Patents
A kind of low temperature process preparation nano material Download PDFInfo
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- CN110498444A CN110498444A CN201910659931.5A CN201910659931A CN110498444A CN 110498444 A CN110498444 A CN 110498444A CN 201910659931 A CN201910659931 A CN 201910659931A CN 110498444 A CN110498444 A CN 110498444A
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The invention belongs to field of nanometer material technology, and in particular to a kind of low temperature process preparation nano material includes the following steps: step 1, tetrabutyl titanate is added to absolute ethanol and is stirred evenly, by ethyl cellulose and methyl ethyl ketone peroxide ultrasonic disperse 1-2h, obtains titanium alcohol liquid；Step 2, titanium alcohol liquid is put into vacuum distillation in vacuum distillation reaction kettle and forms siccative, fragmentation obtains particle；Step 3, oleic acid is added and is stirred evenly into dehydrated alcohol, obtained oleic acid alcohol liquid, be then coated uniformly on particle surface, constant temperature drying obtains plating particles；Step 4, gellan gum is added to the water, stirs evenly to form sizing material, low temperature ultrasonic is then added into sizing material in plating particles be dispersed to and be completely dispersed, cooling solidification obtains solid block, obtains dispersible granule after fragmentation；Step 5, dispersible granule tiling is put into constant temperature illumination reaction 2-4h in illumination reaction kettle, then successively soaking and stirring reaction in distilled water and dehydrated alcohol, drying obtains hydrophobic nano titanium dioxide after filtering.
Description
Technical field
The invention belongs to field of nanometer material technology, and in particular to a kind of low temperature process preparation nano material.
Background technique
Nano-titanium dioxide is square in magnetism, catalytic, conductance, hardness and fusing point etc. because of its bulk effect and surface benefit
Face has many excellent performances than other materials.In recent years, nano-titanium dioxide is added in other materials to improve it
The research of the performance of its material becomes more and more active.But since the partial size of nano-titanium dioxide is small, specific surface energy and large specific surface area,
It is easy to reunite in a dispersion medium；In addition, nano-titanium dioxide has great surface energy, it is easy to absorb the vapor in air
And hydration occurs, so that its surface be made to generate hydroxyl.Therefore nano-titanium dioxide exists with biggish agglomerate particle form,
Even also reduce the original performance of subsequent organic polymer material such as intensity, compactness and glossiness etc..
Summary of the invention
For the problems of the prior art, the present invention provides a kind of low temperature process preparation nano material, solves nano material
Agglomeration traits, using cryogenic particlesization with ultraviolet heating reaction combine, formed cavity reaction system, dredged after washed
Water nano-titanium dioxide.
To realize the above technical purpose, the technical scheme is that
A kind of low temperature process preparation nano material, includes the following steps:
Step 1, tetrabutyl titanate is added to absolute ethanol and is stirred evenly, ethyl cellulose and methyl ethyl ketone peroxide are surpassed
Sound disperses 1-2h, obtains titanium alcohol liquid；
Step 2, titanium alcohol liquid is put into vacuum distillation in vacuum distillation reaction kettle and forms siccative, fragmentation obtains particle；
Step 3, oleic acid is added and is stirred evenly into dehydrated alcohol, obtained oleic acid alcohol liquid, be then coated uniformly on particle
Surface, constant temperature drying obtain plating particles；
Step 4, gellan gum is added to the water, stirs evenly to form sizing material, then plating particles are added into sizing material low
For warm ultrasonic disperse to being completely dispersed, cooling solidification obtains solid block, obtains dispersible granule after fragmentation；
Step 5, dispersible granule tiling is put into constant temperature illumination reaction 2-4h in illumination reaction kettle, then successively distilled water and nothing
Soaking and stirring is reacted in water-ethanol, and drying obtains hydrophobic nano titanium dioxide after filtering.
Concentration of the tetrabutyl titanate in dehydrated alcohol is 50-100g/L in the step 1, and the ethyl cellulose adds
Enter the 150-200% that amount is tetrabutyl titanate quality, the additional amount of methyl ethyl ketone peroxide is the 10- of tetrabutyl titanate quality
15%, the temperature of the ultrasonic disperse is 30-50 DEG C, supersonic frequency 30-50kHz.
The temperature of vacuum distillation in the step 2 is 65-75 DEG C, and pressure is the 70-80% of atmospheric pressure, and the fragmentation is adopted
With constant temperature ball-milling method, temperature is not higher than 50 DEG C.
The mass ratio of oleic acid and dehydrated alcohol in the step 3 is 1:3-6, and the mixing speed stirred evenly is 800-
1000r/min, the coated weight uniformly coated are 4-10mL/cm2, the temperature of constant temperature drying is 80-90 DEG C.
The mass ratio of gellan gum and distilled water in the step 4 is 1:2-4, and the additional amount of gellan gum is tetrabutyl titanate
The 500-1000% of quality, the mixing speed stirred evenly are 2000-3000r/min, and the temperature of low temperature ultrasonic is 10-20 DEG C,
Supersonic frequency is 50-80kHz, and the cured temperature that cools down is -5~-2 DEG C, and the partial size of dispersible granule is 0.1-0.5mm.
The temperature of constant temperature illumination reaction in the step 5 is 130-150 DEG C, and illumination uses ultraviolet light, and intensity of illumination is
5-10mW/cm2, the temperature dried after filtering is 80-100 DEG C.
Tetrabutyl titanate is dissolved in dehydrated alcohol by step 1, and is stirred evenly, while ethyl cellulose is as dispersion
Agent is added into dehydrated alcohol, can be coated on tetrabutyl titanate surface and form stable cladding system, wherein by metatitanic acid cladding,
Methyl ethyl ketone peroxide can be dissolved in dehydrated alcohol, achieve the effect that dissolution dispersion.
Step 2 is removed dehydrated alcohol in the way of vacuum distillation, and temperature at this time can not cause peroxidating first and second
Ketone is decomposed reaction, so, methyl ethyl ketone peroxide is uniformly distributed in entire dissolution system, mistake during removing dehydrated alcohol
Methyl Ethyl Ketone Oxidation is evenly dispersed in ethyl cellulose, forms good dispersion, and form particle during fragmentation.
Step 3 is evenly dispersed into dehydrated alcohol by oleic acid, is then coated on ethyl cellulose surface, since ethyl alcohol is to second
Base fiber is known as dissolubility, forms osmotic system, oleic acid is brought into ethyl cellulose, and will be anhydrous during constant temperature drying
Ethyl alcohol removal, oleic acid rest in ethyl cellulose.
Step 4 stirs evenly the slurry to be formed using gellan gum in water, while in water not using ethyl cellulose
Dissolution characteristics, it can be ensured that plating particles are evenly distributed in the hydrolytic sol of gellan gum with grain structure, form uniform point
It dissipates, and fragmentation is in dispersible granule after low-temperature setting, is achieved the effect that evenly dispersed.
Dispersible granule tiling is put into illumination reaction kettle and carries out illumination reaction by step 5, and the transparency based on gellan gum can
By ultraviolet light thoroughly to ethyl cellulose surface, form the degradation of ethyl cellulose, at the same methyl ethyl ketone peroxide at a temperature of formed
Oxidative decomposition, it is ensured that tetrabutyl titanate is converted into nano-titanium dioxide, while pressure and temperature state at this time, being capable of shape
At reacting for oleic acid and titanium dioxide, achieve the effect that hydrophobization；Above-mentioned reaction is anyway in ethyl cellulose package metatitanic acid
In dispersible granule, and using gellan gum as surface structure, stable transparent covered effect is formed；Using distilled water and dehydrated alcohol
Washing, gellan gum can be recycled and reused, while dehydrated alcohol can be washed into excessive oleic acid, be dredged after drying
Water type nano-titanium dioxide.
From the above, it can be seen that the present invention has following advantages:
1. the present invention solves the agglomeration traits of nano material, combined using cryogenic particlesization with ultraviolet heating reaction,
Cavity reaction system is formed, obtains hydrophobic nano-titanium dioxide after washed.
2. the present invention can not destroy fragmentation in the case where molecular structure using the repeatability of gellan gum, while physics is molten
The mode of solution can be realized the reuse of gellan gum.
Specific embodiment
The present invention will be described in detail in conjunction with the embodiments, but does not do any restriction to claim of the invention.
Embodiment 1
A kind of low temperature process preparation nano material, includes the following steps:
Step 1, tetrabutyl titanate is added to absolute ethanol and is stirred evenly, ethyl cellulose and methyl ethyl ketone peroxide are surpassed
Sound disperses 1h, obtains titanium alcohol liquid；
Step 2, titanium alcohol liquid is put into vacuum distillation in vacuum distillation reaction kettle and forms siccative, fragmentation obtains particle；
Step 3, oleic acid is added and is stirred evenly into dehydrated alcohol, obtained oleic acid alcohol liquid, be then coated uniformly on particle
Surface, constant temperature drying obtain plating particles；
Step 4, gellan gum is added to the water, stirs evenly to form sizing material, then plating particles are added into sizing material low
For warm ultrasonic disperse to being completely dispersed, cooling solidification obtains solid block, obtains dispersible granule after fragmentation；
Step 5, dispersible granule tiling is put into constant temperature illumination reaction 2h in illumination reaction kettle, then successively distilled water and anhydrous
Soaking and stirring is reacted in ethyl alcohol, and drying obtains hydrophobic nano titanium dioxide after filtering.
Concentration of the tetrabutyl titanate in dehydrated alcohol is 50g/L, the additional amount of the ethyl cellulose in the step 1
It is the 150% of tetrabutyl titanate quality, the additional amount of methyl ethyl ketone peroxide is the 10% of tetrabutyl titanate quality, the ultrasound point
Scattered temperature is 30 DEG C, supersonic frequency 30kHz.
The temperature of vacuum distillation in the step 2 is 65 DEG C, and pressure is the 70% of atmospheric pressure, and the fragmentation uses constant temperature
Ball-milling method, temperature are 50 DEG C.
The mass ratio of oleic acid and dehydrated alcohol in the step 3 is 1:3, and the mixing speed stirred evenly is 800r/
Min, the coated weight uniformly coated are 4mL/cm2, the temperature of constant temperature drying is 80 DEG C.
The mass ratio of gellan gum and distilled water in the step 4 is 1:2, and the additional amount of gellan gum is tetrabutyl titanate matter
The 500% of amount, the mixing speed stirred evenly are 2000r/min, and the temperature of low temperature ultrasonic is 10 DEG C, supersonic frequency 50-
80kHz, the cured temperature that cools down are -5 DEG C, and the partial size of dispersible granule is 0.1mm.
The temperature of constant temperature illumination reaction in the step 5 is 130 DEG C, and illumination uses ultraviolet light, intensity of illumination 5mW/
cm2, the temperature dried after filtering is 80 DEG C.
Embodiment 2
A kind of low temperature process preparation nano material, includes the following steps:
Step 1, tetrabutyl titanate is added to absolute ethanol and is stirred evenly, ethyl cellulose and methyl ethyl ketone peroxide are surpassed
Sound disperses 2h, obtains titanium alcohol liquid；
Step 2, titanium alcohol liquid is put into vacuum distillation in vacuum distillation reaction kettle and forms siccative, fragmentation obtains particle；
Step 3, oleic acid is added and is stirred evenly into dehydrated alcohol, obtained oleic acid alcohol liquid, be then coated uniformly on particle
Surface, constant temperature drying obtain plating particles；
Step 4, gellan gum is added to the water, stirs evenly to form sizing material, then plating particles are added into sizing material low
For warm ultrasonic disperse to being completely dispersed, cooling solidification obtains solid block, obtains dispersible granule after fragmentation；
Step 5, dispersible granule tiling is put into constant temperature illumination reaction 4h in illumination reaction kettle, then successively distilled water and anhydrous
Soaking and stirring is reacted in ethyl alcohol, and drying obtains hydrophobic nano titanium dioxide after filtering.
Concentration of the tetrabutyl titanate in dehydrated alcohol is 100g/L, the addition of the ethyl cellulose in the step 1
Amount is the 200% of tetrabutyl titanate quality, and the additional amount of methyl ethyl ketone peroxide is the 15% of tetrabutyl titanate quality, the ultrasound
The temperature of dispersion is 50 DEG C, supersonic frequency 50kHz.
The temperature of vacuum distillation in the step 2 is 75 DEG C, and pressure is the 80% of atmospheric pressure, and the fragmentation uses constant temperature
Ball-milling method, temperature are 40 DEG C.
The mass ratio of oleic acid and dehydrated alcohol in the step 3 is 1:, the mixing speed stirred evenly is 1000r/
Min, the coated weight uniformly coated are 10mL/cm2, the temperature of constant temperature drying is 90 DEG C.
The mass ratio of gellan gum and distilled water in the step 4 is 1:4, and the additional amount of gellan gum is tetrabutyl titanate matter
The 1000% of amount, the mixing speed stirred evenly are 3000r/min, and the temperature of low temperature ultrasonic is 20 DEG C, and supersonic frequency is
80kHz, the cured temperature that cools down are -2 DEG C, and the partial size of dispersible granule is 0.5mm.
The temperature of constant temperature illumination reaction in the step 5 is 150 DEG C, and illumination uses ultraviolet light, intensity of illumination 10mW/
cm2, the temperature dried after filtering is 100 DEG C.
Embodiment 3
A kind of low temperature process preparation nano material, includes the following steps:
Step 1, tetrabutyl titanate is added to absolute ethanol and is stirred evenly, ethyl cellulose and methyl ethyl ketone peroxide are surpassed
Sound disperses 2h, obtains titanium alcohol liquid；
Step 2, titanium alcohol liquid is put into vacuum distillation in vacuum distillation reaction kettle and forms siccative, fragmentation obtains particle；
Step 3, oleic acid is added and is stirred evenly into dehydrated alcohol, obtained oleic acid alcohol liquid, be then coated uniformly on particle
Surface, constant temperature drying obtain plating particles；
Step 4, gellan gum is added to the water, stirs evenly to form sizing material, then plating particles are added into sizing material low
For warm ultrasonic disperse to being completely dispersed, cooling solidification obtains solid block, obtains dispersible granule after fragmentation；
Step 5, dispersible granule tiling is put into constant temperature illumination reaction 3h in illumination reaction kettle, then successively distilled water and anhydrous
Soaking and stirring is reacted in ethyl alcohol, and drying obtains hydrophobic nano titanium dioxide after filtering.
Concentration of the tetrabutyl titanate in dehydrated alcohol is 80g/L, the additional amount of the ethyl cellulose in the step 1
It is the 180% of tetrabutyl titanate quality, the additional amount of methyl ethyl ketone peroxide is the 13% of tetrabutyl titanate quality, the ultrasound point
Scattered temperature is 40 DEG C, supersonic frequency 40kHz.
The temperature of vacuum distillation in the step 2 is 70 DEG C, and pressure is the 75% of atmospheric pressure, and the fragmentation uses constant temperature
Ball-milling method, temperature are 30 DEG C.
The mass ratio of oleic acid and dehydrated alcohol in the step 3 is 1:5, and the mixing speed stirred evenly is 900r/
Min, the coated weight uniformly coated are 8mL/cm2, the temperature of constant temperature drying is 85 DEG C.
The mass ratio of gellan gum and distilled water in the step 4 is 1:3, and the additional amount of gellan gum is tetrabutyl titanate matter
The 800% of amount, the mixing speed stirred evenly are 2500r/min, and the temperature of low temperature ultrasonic is 15 DEG C, supersonic frequency 70kHz,
The cured temperature that cools down is -4 DEG C, and the partial size of dispersible granule is 0.3mm.
The temperature of constant temperature illumination reaction in the step 5 is 140 DEG C, and illumination uses ultraviolet light, intensity of illumination 8mW/
cm2, the temperature dried after filtering is 90 DEG C.
Performance detection
Comparative example uses commercially available import hydrophobic titanium dioxide.
In conclusion the invention has the following advantages that
1. the present invention solves the agglomeration traits of nano material, combined using cryogenic particlesization with ultraviolet heating reaction,
Cavity reaction system is formed, obtains hydrophobic nano-titanium dioxide after washed.
2. the present invention can not destroy fragmentation in the case where molecular structure using the repeatability of gellan gum, while physics is molten
The mode of solution can be realized the reuse of gellan gum.
It is understood that being merely to illustrate the present invention above with respect to specific descriptions of the invention and being not limited to this
Technical solution described in inventive embodiments.Those skilled in the art should understand that still can be carried out to the present invention
Modification or equivalent replacement, to reach identical technical effect；As long as meet use needs, all protection scope of the present invention it
It is interior.
Claims (6)
1. a kind of low temperature process prepares nano material, characterized by the following steps:
Step 1, tetrabutyl titanate is added to absolute ethanol and is stirred evenly, by ethyl cellulose and methyl ethyl ketone peroxide ultrasound point
1-2h is dissipated, titanium alcohol liquid is obtained；
Step 2, titanium alcohol liquid is put into vacuum distillation in vacuum distillation reaction kettle and forms siccative, fragmentation obtains particle；
Step 3, oleic acid is added and is stirred evenly into dehydrated alcohol, obtained oleic acid alcohol liquid, be then coated uniformly on particle surface,
Constant temperature drying obtains plating particles；
Step 4, gellan gum is added to the water, stirs evenly to form sizing material, low temperature is then added into sizing material in plating particles and is surpassed
Sound, which is dispersed to, to be completely dispersed, and cooling solidification obtains solid block, obtains dispersible granule after fragmentation；
Step 5, dispersible granule tiling is put into constant temperature illumination reaction 2-4h in illumination reaction kettle, then successively distilled water and anhydrous second
Soaking and stirring is reacted in alcohol, and drying obtains hydrophobic nano titanium dioxide after filtering.
2. low temperature process according to claim 1 prepares nano material, it is characterised in that: tetrabutyl titanate in the step 1
Concentration in dehydrated alcohol is 50-100g/L, and the additional amount of the ethyl cellulose is the 150- of tetrabutyl titanate quality
200%, the additional amount of methyl ethyl ketone peroxide is the 10-15% of tetrabutyl titanate quality, and the temperature of the ultrasonic disperse is 30-50
DEG C, supersonic frequency 30-50kHz.
3. low temperature process according to claim 1 prepares nano material, it is characterised in that: the vacuum distillation in the step 2
Temperature be 65-75 DEG C, pressure be atmospheric pressure 70-80%, the fragmentation use constant temperature ball-milling method, temperature be not higher than 50 DEG C.
4. low temperature process according to claim 1 prepares nano material, it is characterised in that: oleic acid and nothing in the step 3
The mass ratio of water-ethanol is 1:3-6, and the mixing speed stirred evenly is 800-1000r/min, and the coated weight uniformly coated is 4-
10mL/cm2, the temperature of constant temperature drying is 80-90 DEG C.
5. low temperature process according to claim 1 prepares nano material, it is characterised in that: gellan gum in the step 4 with
The mass ratio of distilled water is 1:2-4, and the additional amount of gellan gum is the 500-1000% of tetrabutyl titanate quality, and what is stirred evenly stirs
Mixing speed is 2000-3000r/min, and the temperature of low temperature ultrasonic is 10-20 DEG C, supersonic frequency 50-80kHz, is cooled down cured
Temperature is -5~-2 DEG C, and the partial size of dispersible granule is 0.1-0.5mm.
6. low temperature process according to claim 1 prepares nano material, it is characterised in that: the constant temperature illumination in the step 5
The temperature of reaction is 130-150 DEG C, and illumination uses ultraviolet light, intensity of illumination 5-10mW/cm2, the temperature dried after filtering is
80-100℃。
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| CN201910659931.5A CN110498444A (en) | 2019-07-22 | 2019-07-22 | A kind of low temperature process preparation nano material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112742365A (en) * | 2020-12-31 | 2021-05-04 | 吴亚良 | Preparation method of hollow porous photocatalyst carrier |
| CN112871158A (en) * | 2021-02-20 | 2021-06-01 | 浙江工业大学上虞研究院有限公司 | Preparation method of titanium dioxide-palladium composite catalyst |
| CN116622277A (en) * | 2023-06-06 | 2023-08-22 | 安徽纽亚达科技有限责任公司 | Preparation method of antirust material of nano oxide coated mica iron oxide |
-
2019
- 2019-07-22 CN CN201910659931.5A patent/CN110498444A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112742365A (en) * | 2020-12-31 | 2021-05-04 | 吴亚良 | Preparation method of hollow porous photocatalyst carrier |
| CN112871158A (en) * | 2021-02-20 | 2021-06-01 | 浙江工业大学上虞研究院有限公司 | Preparation method of titanium dioxide-palladium composite catalyst |
| CN116622277A (en) * | 2023-06-06 | 2023-08-22 | 安徽纽亚达科技有限责任公司 | Preparation method of antirust material of nano oxide coated mica iron oxide |
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