CN107522169A - A kind of normal temperature prepares pure organic homogeneous precipitation method of nano-oxide - Google Patents
A kind of normal temperature prepares pure organic homogeneous precipitation method of nano-oxide Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/36—Methods for preparing oxides or hydroxides in general by precipitation reactions in aqueous solutions
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- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The present invention relates to pure organic homogeneous precipitation method that a kind of normal temperature prepares nano-oxide.This method is reaction in-situ, prepared nano-oxide has the characteristics that small preparation method simple, normal temperature synthesis, particle diameter, structure, pattern and chemical composition are controllable, cost is low, can be mass, and the nano-oxide can further synthesize titanium oxide, silica, zirconium oxide, aluminum oxide, zinc oxide etc. at normal temperatures has high-efficiency activated oxide.It is characterized in that comprise the following steps：Will be using alcohol solution as solvent, amine solution is that the metal salt such as buffer, titanium, zinc, silicon, aluminium, zirconium is source metal, and organic acid is as precipitating reagent.Metal salt and amine solution are dissolved in alcohol and solution A are made, solution B will be made in organic acid soln alcohol, A, B solution are mixed, make to be uniformly distributed in the organic acid and alcohol reaction generation hydrone in system, hydrolysis generation high-activity nano oxidation material directly occurs with the metal salt being uniformly distributed in solution using the hydrone.
Description
Technical field
The present invention relates to pure organic homogeneous precipitation method that a kind of normal temperature prepares nano-oxide, and in particular to a kind of with organic
The method of homogeneous precipitation method preparation structure, pattern and the controllable nano-oxide of chemical composition under normal temperature condition, this method are
Reaction in-situ, prepared nano-oxide can further synthesize titanium oxide, silica, zirconium oxide, oxygen in a mild condition
Changing aluminium, zinc oxide etc. has high-efficiency activated oxide.
Background technology
Nanometer oxide material is widely used in making catalyst, fine ceramics, composite, magnetic material, phosphor
Material, moisture-sensitive sensor and infrared absorbing material etc., as conventional material is presented in terms of magnetic, light, electric sensitive material in nano zine oxide
The not available specific function of material so that the zinc oxide of high-quality has a extensive future；Nano aluminium oxide is as important pottery
Ceramic material, there is very high application value；High-purity Nano-class SnO2It can be used to make air-sensitive and dew cell；Nano-titanium oxide
Due to the extensive use in terms of fine ceramics, semiconductor, catalysis material, also increasingly cause the concern of people.In recent years
Through developing a variety of methods for preparing metal oxide nano-material, conventional method includes sol-gel process, the precipitation method, hydro-thermal
Synthetic method, Hydrolyze method, gas-phase decomposition method, microemulsion method etc..Wherein sol-gel process grows up in the recent period, can replace height
Warm solid phase synthesis prepares the new method of ceramics, glass and many solid materials.As synthesizing nothing under low temperature or temperate condition
The important method of machine compound or inorganic material, has occupied critical role in soft chemical synthesis, is also widely used in preparation nanometer
Particle.But the method still suffers from many problems, cost of material as used costly, generally whole sol-gel process institute
Take time longer (often needing a few days or a few weeks), a large amount of micropores present in gel easily escape in the drying process many gases and
Organic matter simultaneously produces contraction etc..The precipitation method be by chemical reaction make raw material active ingredient generate precipitation, then by filtering,
Washing, dry, thermally decompose to yield nano-particle, being a kind of most economical method for preparing metallic oxide nano powder.The party
Although method operation is fairly simple, the reaction time is long, is formed precipitation generally be present and be difficult to filter because jelly and wash, sink
The addition of shallow lake agent may cause the problems such as local concentration is too high, generation reunion or composition is not uniform enough.Hydrothermal synthesis method often only
Suitable for preparing oxide material or narrower to the insensitive material of water, application.In a word, already present method still can not at present
Show the advantages such as preparation method is simple, cost is low, energy consumption is small, product morphology is controllable, can be mass, explore at present in which kind of bar
Metal oxide nanoparticles are carried out with size cutting under part and pattern is controlled and how nano-metal-oxide changed
Journal of Sex Research is extremely urgent, it would be highly desirable to finds a kind of method and is used to realizing that prepared nano-oxide to have any surface finish, particle
Regular shape, particle diameter distribution are uniform, granularity is controllable, be not easy to reunite, to be easy to collection, heat endurance, good dispersion, yield height etc. excellent
More performance, and the material is further widely used in magnetic material, ceramic material, lubriation material, photochemical catalyst and composite wood
In material.
The content of the invention
It is an object of the invention to provide pure organic homogeneous precipitation method that a kind of normal temperature prepares nano-oxide, this method is
Reaction in-situ, prepared nano-oxide have small preparation method simple, normal temperature synthesis, particle diameter, structure, pattern and chemical group
Into it is controllable, cost is low, can be mass, long lifespan, safely and effectively, non-secondary pollution the features such as.
A kind of normal temperature of the present invention prepares pure organic homogeneous precipitation method of nano-oxide, comprises the following steps：
(1) using alcohol solution as solvent, amine solution is that the metal salt such as buffer, titanium, zinc, silicon, aluminium, zirconium is source metal,
Organic acid soln is as precipitating reagent.Metal salt and amine solution are dissolved in alcohol and solution A are made, will be made in organic acid soln alcohol
Solution B, A, B solution are mixed, make to be uniformly distributed in the organic acid and alcohol solution reaction generation hydrone in system, utilize
Directly with the metal salt being uniformly distributed in solution hydrolysis occurs for the hydrone, is stirred continuously until reaction generation white is muddy
Turbid precipitation.
(2) the synthesis ratio of mentioned reagent is：The metal salt 1ml-200ml such as titanium, zinc, silicon, aluminium, zirconium, amine solution 1%-
60%, alcoholic solution 10ml-300ml, organic metal salt 0-100%, organic acid 5ml-300ml.In addition, organic acid addition is got over
More, reaction is faster, and the time for producing precipitation is shorter.
(3) solution of above-mentioned stirring to cloudy state is placed under the conditions of certain temperature and is aged 24h, obtain accounting for solution total
The precipitation of volume 4/5ths.With organic solvent washing, centrifuged in 10000r/min supercentrifuge, remove supernatant
Liquid, so wash 3 times repeatedly.Clean sediment obtains nano-oxide after 60 DEG C of baking ovens toast 24h mortar grinders.
The particle diameter of the nano-oxide powder can realize ＜ 20nm.
The nano-oxide can further synthesize nano-titanium oxide, silica, zirconium oxide, aluminum oxide, oxygen at normal temperatures
Changing zinc etc. has high-efficiency activated oxide.
Receiving with high efficiency photocatalysis performance can be further made under normal temperature condition processing in the nano-oxide powder
Rice TiO2, the nano-TiO2Crystal formation is anatase phase titanium dioxide nanometer powder, has superior degraded hazardous contaminant
Performance.
The present invention principle be：
Easily reunite at high temperature for nano-oxide, active the problems such as reducing, the present invention uses pure organic homogeneous deposition
Nano-oxide prepared by method be able to can synthesize under normal temperature condition, and preparation condition gently ensure that low energy consumption, and realizes and receive
Rice oxide diameter sizes size, structure, pattern and chemical composition it is controllable, this method effectively prevent high temperature to nano oxidized physical property
The influence of energy, solve thes problems, such as that nano-oxide is also easy to produce reunion under the high temperature conditions, uses the nano-oxide institute
The nano-titanium oxide prepared, silica, zirconium oxide, aluminum oxide, zinc oxide etc. are with a wide range of applications.
The present invention concrete application method be：
(1) the methods of nano-oxide that the present invention prepares can not only pass through normal temperature dipping further generates nano oxygen
Changing titanium, silica, zirconium oxide, aluminum oxide, zinc oxide etc. has the nano material of high activity, while can also have applied to water body
In the degraded of malicious noxious pollutant.Furthermore it is also possible to nano-oxide is applied to by epoxy using online step situ aggregation method
In the modification of resin, it is with a wide range of applications.
(2) nano-oxide prepared by the present invention, what the methods of nano-oxide is passed through into normal temperature dipping prepared
Structure, pattern and chemical composition are controllable, have the catalysis materials such as the nano titanium oxide of high efficiency photocatalysis activity, silica can
With in the degraded applied to hazardous contaminants such as organic dye waste water, formaldehyde.Furthermore it is also possible to it will be received using different process
The photochemical catalyst that rice oxide prepares synthesis is scattered in veneer plate surface；Using different dispersion technologies by photocatalyst applications in
Acrylic acid aqueous woodcare paint etc..
(3) by further furtheing investigate, the nano-oxide can be combined with a variety of environment-friendly materials, and preparing has
The multifunctional material of the characteristics such as acid and alkali-resistance, heat-resisting, cold-resistant, antisepsis and sterilization, high-efficiency self-cleaning and effective decomposing harmful substances, more
Applied in indoor rustproof lacquer, glass, ceramics, means of transportation.
The present invention compared with prior art its be particularly advantageous in that：
(1) traditional method for preparing oxide usually requires hot conditions, exists and is unfavorable for the control of reaction condition, prepares
Cost is high, the low drawback of the nano-oxide of generation activity, and the present invention can not only be effectively reduced system using normal temperature preparation method
Standby cost, energy consumption is saved, can more prevent growth and reunion of the nano-oxide in preparation process, can so as to prepare pattern
Control, the nano-oxide of lower price high efficiency.It is by what the further reaction of the nano-oxide of this method synthesis was prepared simultaneously
Nano-photocatalyst material with special appearance, it is characterized in that the catalyst has visible light catalysis activity and catalytic activity is much
Higher than similar products at home and abroad.
(2) present invention uses non-aqueous system, the hydrolysis generation of titanium hydrochlorate is received using the water that alcoholysis reaction generates is controlled
Rice oxide precipitation, and can have been prepared by normal temperature dipping or low-temperature heat morphology controllable ultra-fine monodisperse titanium dioxide,
The nano materials such as silica.This method not only avoid because titanate acutely hydrolyzes or hydrolyzed uneven caused product shape
The problem of looks and unmanageable structure, and significantly reduce cost while technique is simplified.Using pure organic homogeneous
(001) face with greater activity under visible light of sedimentation synthesis accounts for leading special construction nano material, makes photocatalysis
Performance has obvious increase under visible light, and effectively increases the quantum efficiency of photochemical catalyst.
(3) present invention use independent research pure organic homogeneous precipitation method, this method have equipment is simple, cost is cheap,
The features such as yield is high, non-environmental-pollution；The nano-photocatalyst produced has efficient, antifouling, self-cleaning, anti-corrosion, resistance to bacterium, use
The advantages that long lifespan and asepsis environment-protecting, it can be widely applied to the fields such as environmental protection, traffic, building, medical treatment.
(4) nano-TiO prepared by the present invention2Degraded of the photochemical catalyst to organic dye waste water such as methylene blue waste water, tool
There is significantly effect, degradation capability is significantly larger than Germany's production P25 nanometer powders, and PARA FORMALDEHYDE PRILLS(91,95) also has good degradation effect.
Brief description of the drawings
Fig. 1 is the SEM spectrograms (200nm) of the nano-oxide particles obtained by organic homogeneous precipitation method；
Fig. 2 is the SEM spectrograms (500nm) of the flower-like nanometer oxide obtained by organic homogeneous precipitation method；
Fig. 3 is the SEM spectrograms (100nm) of the flower-like nanometer oxide obtained by organic homogeneous precipitation method.
Embodiment
The present invention will be described in more detail by embodiment, but protection scope of the present invention is not limited to
These embodiments.
Embodiment 1
(1) 10.98ml titanium tetrachlorides, 0.149g triethanolamines are dissolved in 15ml absolute ethyl alcohols and solution A is made, by 20ml
Formic acid solution, which is dissolved in 15ml alcohol, is made solution B, and A, B solution are mixed, and is stirred continuously until reaction produces white opacity precipitation.
After being aged 24h at room temperature, after washing, centrifuged in 1000r/min supercentrifuge, remove supernatant, so wash repeatedly
Wash 3 times.Clean sediment obtains nano-oxide after 45 DEG C of baking ovens toast 24h mortar grinders.(2) by above-mentioned nanometer
Oxide is placed in Muffle furnace, temperature programming obtains nano titanium dioxide powder to 250 DEG C of calcining 6h.
Embodiment 2
(1) 10.98ml titanium tetrachlorides, 0.0745g triethanolamines are dissolved in 30ml absolute ethyl alcohols and solution A is made, by 20ml
Formic acid solution, which is dissolved in 30ml alcohol, is made solution B, and A, B solution are mixed, and is stirred continuously until reaction produces white opacity precipitation.
After being aged 24h at room temperature, after washing, centrifuged in 1000r/min supercentrifuge, remove supernatant, so wash repeatedly
Wash 3 times.Clean sediment obtains nano-oxide after 45 DEG C of baking ovens toast 24h mortar grinders.(2) by above-mentioned nanometer
Oxide, which is placed in 0.018mol/L metaphosphoric acid solution to be sufficiently stirred, makes its reaction complete, is soaked 5 days after ultrasonic 30min, from
The heart, it is washed with deionized 3 times, gained powder is phosphor adulterated highly efficient titania nanometer light after 45 DEG C of baking oven baking 24h
Catalyst.
Embodiment 3
(1) 21.96ml titanium tetrachlorides, 0.061g monoethanolamines are dissolved in 15ml absolute ethyl alcohols and solution A is made, by 15ml
Formic acid solution, which is dissolved in 15ml alcohol, is made solution B, and A, B solution are mixed, and is stirred continuously until reaction produces white opacity precipitation.
After being aged 24h at room temperature, after washing, centrifuged in 1000r/min supercentrifuge, remove supernatant, so wash repeatedly
Wash 3 times.Clean sediment obtains nano-oxide after 45 DEG C of baking ovens toast 24h mortar grinders.(2) by above-mentioned nanometer
Oxide, which is placed in 0.02mol/L sodium hydroxide solution to be sufficiently stirred, makes its reaction complete, is soaked 5 days after ultrasonic 30min, from
The heart, it is washed with deionized 3 times, gained powder is new and effective titanium dioxide nano photocatalysis after 45 DEG C of baking oven baking 24h
Agent.
Embodiment 4
(1) 21.96ml titanium tetrachlorides, 0.149g triethanolamines are dissolved in 15ml absolute ethyl alcohols and solution A is made, by 20ml
Formic acid solution, which is dissolved in 15ml alcohol, is made solution B, and A, B solution are mixed, and is stirred continuously until reaction produces white opacity precipitation.
After being aged 24h at room temperature, after washing, centrifuged in 1000r/min supercentrifuge, remove supernatant, so wash repeatedly
Wash 3 times.Clean sediment obtains nano-oxide after 45 DEG C of baking ovens toast 24h mortar grinders.(2) by above-mentioned nanometer
Oxide is placed in Muffle furnace, temperature programming to 350 DEG C of calcining 6h, that is, obtains the nano titanium dioxide powder of doping iron.
Embodiment 5
(1) 16.47ml titanium tetrachlorides, 0.061g monoethanolamines are dissolved in 15ml absolute ethyl alcohols and solution A is made, by 15ml
Formic acid solution, which is dissolved in 30ml alcohol, is made solution B, and A, B solution are mixed, and is stirred continuously until reaction produces white opacity precipitation.
After being aged 24h at room temperature, after washing, centrifuged in 1000r/min supercentrifuge, remove supernatant, so wash repeatedly
Wash 3 times.Clean sediment obtains nano-oxide after 45 DEG C of baking ovens toast 24h mortar grinders.(2) by above-mentioned nanometer
Oxide, which is placed in 1mol/L metaphosphoric acid solution to be sufficiently stirred, makes its reaction complete, soaks 7 days, centrifugation, uses after ultrasonic 30min
Deionized water is washed 3 times, and gained powder is phosphor adulterated highly efficient titania nano-photo catalytic after 45 DEG C of baking oven baking 24h
Agent.
Embodiment 6
(1) 21.96ml titanium tetrachlorides, 0.122g monoethanolamines are dissolved in 30ml absolute ethyl alcohols and solution A is made, by 15ml
Formic acid solution, which is dissolved in 15ml alcohol, is made solution B, and A, B solution are mixed, and is stirred continuously until reaction produces white opacity precipitation.
After being aged 24h at room temperature, after washing, centrifuged in 1000r/min supercentrifuge, remove supernatant, so wash repeatedly
Wash 3 times.Clean sediment obtains nano-oxide after 45 DEG C of baking ovens toast 24h mortar grinders.(2) by above-mentioned nanometer
Copper presoma is placed in Muffle furnace, temperature programming to 450 DEG C of calcining 6h, that is, obtains the nano titanium dioxide powder of copper doped.
Embodiment 7
(1) 21.96ml titanium tetrachlorides, 0.061g monoethanolamines are dissolved in 15ml absolute ethyl alcohols and solution A is made, by 15ml
Formic acid solution, which is dissolved in 30ml alcohol, is made solution B, and A, B solution are mixed, and is stirred continuously until reaction produces white opacity precipitation.
After being aged 24h at room temperature, after washing, centrifuged in 1000r/min supercentrifuge, remove supernatant, so wash repeatedly
Wash 3 times.Clean sediment obtains nano-oxide after 45 DEG C of baking ovens toast 24h mortar grinders.(2) by above-mentioned nanometer
Oxide, which is placed in 0.04mol/L sodium hydroxide solution to be sufficiently stirred, makes its reaction complete, is soaked 7 days after ultrasonic 30min, from
The heart, it is washed with deionized 3 times, gained powder is new and effective titanium dioxide nano photocatalysis after 45 DEG C of baking oven baking 24h
Agent.
Embodiment 8
(1) 21.96ml titanium tetrachlorides, 0.149g triethanolamines are dissolved in 15ml absolute ethyl alcohols and solution A is made, by 10ml
Formic acid solution, which is dissolved in 15ml alcohol, is made solution B, and A, B solution are mixed, and is stirred continuously until reaction produces white opacity precipitation.
After being aged 24h at room temperature, after washing, centrifuged in 1000r/min supercentrifuge, remove supernatant, so wash repeatedly
Wash 3 times.Clean sediment obtains nano-oxide after 45 DEG C of baking ovens toast 24h mortar grinders.(2) by above-mentioned nanometer
Copper presoma is placed in Muffle furnace, temperature programming to 550 DEG C of calcining 6h, that is, obtains the nano titanium dioxide powder of copper doped.
Embodiment 9
(1) 21.96ml titanium tetrachlorides, 0.298g triethanolamines are dissolved in 30ml absolute ethyl alcohols and solution A is made, by 10ml
Formic acid solution, which is dissolved in 15ml alcohol, is made solution B, and A, B solution are mixed, and is stirred continuously until reaction produces white opacity precipitation.
After being aged 24h at room temperature, after washing, centrifuged in 1000r/min supercentrifuge, remove supernatant, so wash repeatedly
Wash 3 times.Clean sediment obtains nano-oxide after 45 DEG C of baking ovens toast 24h mortar grinders.(2) by above-mentioned nanometer
Cobalt precursor is placed in Muffle furnace, temperature programming to 650 DEG C of calcining 6h, that is, obtains the nano titanium dioxide powder of cation doping.
Embodiment 10
(1) 21.96ml titanium tetrachlorides, 0.298g triethanolamines are dissolved in 30ml absolute ethyl alcohols and solution A is made, by 10ml
Formic acid solution, which is dissolved in 15ml alcohol, is made solution B, and A, B solution are mixed, and is stirred continuously until reaction produces white opacity precipitation.
After being aged 24h at room temperature, after washing, centrifuged in 1000r/min supercentrifuge, remove supernatant, so wash repeatedly
Wash 3 times.Clean sediment obtains nano-oxide after 45 DEG C of baking ovens toast 24h mortar grinders.(2) by above-mentioned nanometer
Oxide, which is placed in 0.05mol/L metaphosphoric acid solution to be sufficiently stirred, makes its reaction complete, is soaked 7 days after ultrasonic 30min, from
The heart, it is washed with deionized 3 times, gained powder is phosphor adulterated highly efficient titania nanometer light after 45 DEG C of baking oven baking 24h
Catalyst.
Claims (5)
1. a kind of normal temperature prepares pure organic homogeneous precipitation method of nano-oxide, it is characterised in that：The reaction is reaction in-situ, should
Nano-oxide prepared by method has small preparation method simple, normal temperature synthesis, particle diameter, structure, pattern and chemical composition can
Control, cost is low, can be mass, long lifespan, safely and effectively, non-secondary pollution the features such as, while the nano-oxide can be
Further synthesis titanium oxide, silica, zirconium oxide, aluminum oxide, zinc oxide etc. have high-efficiency activated oxide under temperate condition.
2. a kind of normal temperature according to claim 1 prepares pure organic homogeneous precipitation method of nano-oxide, it is characterised in that
The preparation method of nano-oxide：
(1) prepare nano-oxide according to add different source metal (titanium, silicon, zirconium, aluminium, zinc etc.) obtain it is different nano oxidized
Thing, the nano-oxide of gained different metal doping are respectively provided with the ability of efficient degradation hazardous contaminant.
(2) synthesis of nano-oxide is divided into two parts：Part I is stirring, and using alcohol solution as solvent, amine solution is
The metal salt such as buffer, titanium, zinc, silicon, aluminium, zirconium is source metal, and metal salt and amine solution are dissolved in by organic acid as precipitating reagent
Solution A is made in alcohol, solution B will be made in acetic acid solution alcohol, A, B solution are mixed, make to be uniformly distributed in system
Acetic acid and alcohol reaction generation hydrone, it is anti-directly to occur hydrolysis using the hydrone with the metal salt being uniformly distributed in solution
Should, be stirred continuously until reaction produce white opacity precipitation, normal temperature (15 DEG C -30 DEG C or so), stirring 1-12h solution turned cloudies with
A large amount of precipitations are produced afterwards, and static rear supernatant is clear shape, and whole whipping process is sealed with sealed membrane, is completely cut off in air
Vapor, the reaction are exothermic reaction；Part II is ageing and washing, and the solution of above-mentioned stirring to cloudy state is placed in into one
24h is aged under the conditions of constant temperature degree, obtains accounting for the precipitation of overall solution volume half, then with organic solvent washing,
1000r/min supercentrifuge centrifuges, and removes supernatant, so washs 3 times repeatedly, and clean sediment is in 45 DEG C of bakings
Nano-oxide is obtained after case baking 24h mortar grinders.
(3) the synthesis ratio for preparing nano-oxide is：The metal salt 1ml-200ml such as titanium, zinc, silicon, aluminium, zirconium, amine solution
1%-60%, alcoholic solution 10ml-300ml, organic metal salt 0-100%, organic acid 5ml-300ml, organic acid in course of reaction
Addition is more, and reaction is faster, and the time for producing precipitation is shorter.
3. the preparation method of nano-oxide according to claim 2, the addition and synthesis ratio of its reactant being related to
Example can synchronously expand multiple, and reaction mechanism is constant, realizes the production in enormous quantities of nano-oxide.
4. the particle diameter of nano-oxide powder according to claim 2 can realize ＜ 20nm.
5. nano-oxide according to claim 2 can further synthesize nano-titanium oxide, silica, oxidation at normal temperatures
Zirconium, aluminum oxide, zinc oxide etc. have high-efficiency activated oxide.
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| CN108465475A (en) * | 2018-04-04 | 2018-08-31 | 东莞市石鼓污水处理有限公司 | A kind of preparation method of WO3-ZrO2 photocatalysis sewages processing composite membrane |
| CN108976715A (en) * | 2018-07-27 | 2018-12-11 | 青岛理工大学 | Nano oxide modified epoxy resin and preparation method thereof |
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