CN101805017A - Preparation method of rutile type titanium dioxide nano particle - Google Patents

Preparation method of rutile type titanium dioxide nano particle Download PDF

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CN101805017A
CN101805017A CN 201010146615 CN201010146615A CN101805017A CN 101805017 A CN101805017 A CN 101805017A CN 201010146615 CN201010146615 CN 201010146615 CN 201010146615 A CN201010146615 A CN 201010146615A CN 101805017 A CN101805017 A CN 101805017A
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throw out
isolated
standby
distilled water
titanium dioxide
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CN101805017B (en
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马录芳
常新红
李冠峰
康海霞
李森兰
王利亚
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Luoyang Normal University
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Abstract

The invention provides a preparation method of a rutile type titanium dioxide nano particle, and relates to the field of inorganic nonmetallic nano material preparation. The preparation method comprises the following steps: firstly preparing a titanium source dispersion solution and an alkali source dispersion solution; heating the alkali source dispersion solution to 60-95 DEG C, then admixing the alkali source solution with the titanium source dispersion solution to be subject to a reaction for 1-24 hours, carrying out centrifugal separation on the mixture after the reaction, uniformly mixing the separated precipitate with distilled water, ethanol aqueous solution and absolute ethyl alcohol sequentially, then carrying out centrifugal separation, sending to a drying box to dry so as to obtain the rutile type titanium dioxide nano particle. The invention has the advantages of low cost, no toxicity, no harm, cycle use of the raw materials, no environmental pollution, simple device and easily-mastered operating condition, and facilitates large scale production; and the size distribution range of the prepared nano particle is narrow, and the particle size can be controlled by adjusting the concentration, the reaction time and the reaction temperature of various used solutions.

Description

A kind of preparation method of rutile type titanium dioxide nano particle
Technical field
The present invention relates to the inorganic nano material preparation method, specifically a kind of preparation method of rutile type titanium dioxide nano particle.
Background technology
Titanium dioxide (TiO 2) be a kind of to the nontoxic multi-crystalline compounds of human body, three kinds of crystal habits are arranged, brookite type, anatase octahedrite and rutile-type, wherein rutile TiO 2Structure the most stable, most widely used.Nano rutile-type TiO 2Because particle is little, specific surface area is big, very strong opacifying power, tinting strength are arranged and, be widely used in fields such as anti-Sai makeup, senior paint, coating, weaving, fine ceramics to ultraviolet receptivity, very high commercial value is arranged.Simultaneously, nano rutile-type TiO 2Have functions such as surface effects, quantum size effect and macro quanta tunnel effect, thereby show fabulous resistance to chemical attack, photocatalytic activity and uvioresistant ability, also be used in aspects such as photosensor, photodissociation hydrophone spare, antifog glass, organism photodegradable aid, gas sensor, temperature sensor.
At present, the preparation method of rutile type titanium dioxide nano particle mainly contains vapor phase process and liquid phase method two big classes.Rutile type titanium dioxide nano particle purity height, good dispersity that vapor phase process is prepared, but its required equipment complexity, energy consumption is big, cost is high.Liquid phase method has that facility investment is few, technology is simple, easy to operate, low cost and other advantages.Liquid phase method be divided into again the precipitator method, hydrothermal method, microemulsion method and sol-gel method [referring to Li Xiaoxia, LiuBing Juan, Liu Guoguang.Nano-TiO 2Preparation method's commentary [J]. chemical industry and technology, 2008,29 (2), 18-20.].The precipitator method generally are with TiCl 4, Ti (SO 4) 2, titanium alkoxide etc. be that the raw material hydrolysis generates TiO 2Obtain nano-TiO after hydrate drying, 500 ℃ of roastings 2, high-temperature roasting expends the energy and easily reunites, and the cost height does not belong to low-carbon economy.Hydrothermal method is to do reaction medium with the aqueous solution in airtight high-pressure reactor, and precursor is dissolved in the hydro-thermal medium, and then the final crystal grain with certain particle size and crystal habit that forms of nucleation, growth.Hydrothermal method does not need high-temperature roasting, but this method complicated operation, to the equipment requirements height, be difficult for suitability for industrialized production.Microemulsion method is a kind of method of utilizing two kinds of mutual exclusive solvents synthetic solid phase under the effect of tensio-active agent, and the tensio-active agent that this method is introduced is difficult for reclaiming, contaminate environment, and influences product purity.Sol-gel method comprises the preparation of colloidal sol, molten gel conversion, Drying of gels and roasting, needs high-temperature roasting equally, does not belong to low-carbon economy equally, does not meet environmental protection concept.
There is the synthesis technique relative complex in above method, condition is wayward, environmental pollution is serious, high carbon emission, the shortcoming that range of application is narrow.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of rutile type titanium dioxide nano particle has that synthesis temperature is low, equipment and technology is simple, condition is easily controlled, advantage with low cost.
The present invention is the deficiency that solves the problems of the technologies described above, and the technical scheme that is adopted is: a kind of preparation method of rutile type titanium dioxide nano particle comprises the steps:
Step 1, get a kind of in titanium sulfate, titanyl sulfate or the titanium chloride, its mass fraction is 3~6 parts; Get a kind of in sulfuric acid or the hydrochloric acid soln, its mass fraction is 10~27 parts; Two kinds of raw materials choosing are mixed, and titanium source dispersion soln is made in dissolving, and is standby;
Step 2, get a kind of in sodium hydroxide or the potassium hydroxide, its mass fraction is 2.8~16 parts; Get a kind of in sodium sulfate, vitriolate of tartar, sodium-chlor or the Klorvess Liquid, its mass fraction is 20~60 parts, concentration 〉=0.1mol/L; Two kinds of raw materials choosing are mixed, and the alkali source dispersion soln is made in dissolving, and is standby;
Step 3, the alkali source dispersion soln of making is placed reactor, even heating to 60~95 ℃, after titanium source dispersion soln is joined in the alkali source dispersion soln, generate white precipitate in the reaction process, reaction times is 1~24 hour, and post reaction mixture is sent into whizzer, centrifugation, isolated centrifugate reclaims, and isolated throw out is standby;
Step 4, the isolated throw out of step 3 is added in the distilled water, the consumption of distilled water is at least 0.5 times of throw out quality, send into whizzer after mixing, centrifugation, isolated centrifugate reclaims, and isolated throw out mixes with distilled water according to aforementioned proportion again, after send into whizzer, centrifugation, isolated centrifugate reclaims, and isolated throw out is standby;
Step 5, use the aqueous ethanolic solution of being made up of the ethanol of 80% distilled water and 20% to replace distilled water, according to the method for step 4 the isolated throw out of its and step 4 is mixed also centrifugation, isolated throw out is standby;
Step 6, the isolated throw out of step 5 is mixed with dehydrated alcohol, the add-on of dehydrated alcohol is 0.8 times of throw out quality at least, sends into whizzer after mixing and separates, and isolated throw out is standby;
Step 7, the isolated throw out of step 6 is sent into vacuum drying oven, take out dry back, promptly makes rutile type titanium dioxide nano particle.
The concentration of described mineral acid dispersant solution should guarantee pH≤0.
The centrifugate that step 3 reclaims can directly be reused as raw material; The centrifugate that step 4 reclaims can be put into and reclaim use after the airing pond makes its moisture that volatilizees naturally; The centrifugates that step 5, six reclaims can reclaim ethanol and distilled water is used for producing again by simple distillation.
The invention has the beneficial effects as follows: 1, with low cost, nontoxic, raw material can be recycled, the non-environmental-pollution problem; 2, equipment used is simple, and operational condition is easy to grasp, and is convenient to scale operation; 3, nano particle diameter narrow distribution range, size can be passed through concentration, reaction times and the temperature of reaction control of the various solution of use.
Embodiment
A kind of preparation method of rutile type titanium dioxide nano particle comprises the steps:
Step 1, get a kind of as the titanium source in titanium sulfate, titanyl sulfate or the titanium chloride, its mass fraction is 3~6 parts; Get a kind of in sulfuric acid or the hydrochloric acid soln, its mass fraction is 10~27 parts, and its concentration should guarantee pH≤0 of solution, and the big more titanium dioxide nano-particle particle that finally makes of its concentration is big more; Two kinds of raw materials choosing are mixed, and titanium source dispersion soln is made in dissolving, and is standby;
Step 2, get a kind of as alkali source in sodium hydroxide or the potassium hydroxide, its mass fraction is 2.8~16 parts; Get a kind of in sodium sulfate, vitriolate of tartar, sodium-chlor or the Klorvess Liquid, its mass fraction is 20~60 parts, concentration 〉=0.1mol/L, and the big more titanium dioxide nano-particle particle that finally makes of its concentration is big more; Two kinds of raw materials choosing are mixed, and the alkali source dispersion soln is made in dissolving, and is standby;
Step 3, the alkali source dispersion soln of making is placed reactor, even heating to 60~95 ℃, after titanium source dispersion soln is joined in the alkali source dispersion soln, generate white precipitate in the reaction process, reaction times is 1~24 hour, and post reaction mixture is sent into whizzer, centrifugation, isolated centrifugate reclaims, and isolated throw out is standby;
Step 4, the isolated throw out of step 3 is added in the distilled water, the consumption of distilled water is at least 0.5 times of throw out quality, send into whizzer after mixing, centrifugation, isolated centrifugate reclaims, and isolated throw out mixes with distilled water according to aforementioned proportion again, after send into whizzer, centrifugation, isolated centrifugate reclaims, and isolated throw out is standby;
Step 5, use the aqueous ethanolic solution of being made up of the ethanol of 80% distilled water and 20% to replace distilled water, according to the method for step 4 the isolated throw out of its and step 4 is mixed also centrifugation, isolated throw out is standby;
Step 6, the isolated throw out of step 5 is mixed with dehydrated alcohol, the add-on of dehydrated alcohol is 0.8 times of throw out quality at least, sends into whizzer after mixing and separates, and isolated throw out is standby;
Step 7, the isolated throw out of step 6 is sent into vacuum drying oven, take out dry back, promptly makes rutile type titanium dioxide nano particle.
The maximum consumption of described titanium source and alkali source reaches capacity in dispersion agent with them and exceeds, and minimum amount is with product 〉=10 of the two volumetric molar concentration (mol/L) in corresponding dispersion agent -10Exceed.
Described alkali source, its consumption comprises two portions: a part is all neutralizations of acid in the mineral acid dispersant solution with the acid in the dispersion soln of titanium source; The mole number of another part, the reaction formula metering of pressing titanium source and alkali makes alkali source all be used for reaction, to save cost.
In reaction system, at selected titanium source and alkali source, select a kind of preparation titanium source dispersion soln in sulfuric acid or the hydrochloric acid soln for use, select a kind of preparation alkali source dispersion soln in sodium sulfate, vitriolate of tartar, sodium-chlor or the Klorvess Liquid for use; The negative ions of selected solution can be adsorbed in the nucleating surface of target product by electrical function, slows down nuclei growth speed; And can increase the ionic strength of reaction solution, target product can not be existed with colloid or metamict.Therefore, can make the narrow high-quality nano material of particle size distribution range.
The size of product titanium dioxide nano-particle can be passed through the concentration control in the dispersion soln of correspondence of reaction times, titanium source and alkali source.Short more, titanium source of reaction times and the concentration of alkali source in the dispersion soln of correspondence are more little, and the particle of the titanium dioxide nano-particle that makes is just more little.Otherwise long more, titanium source of reaction times and the concentration of alkali source in the dispersion soln of correspondence are big more, and the particle of the titanium dioxide nano-particle that makes is just big more.
Embodiment 1
A kind of preparation method of rutile type titanium dioxide nano particle comprises the steps:
Step 1 is got the titanium sulfate (Ti (SO of 6 mass parts 4) 2); Get H 2SO 4: H 2O=1: 4 sulphuric acid soln 27 mass parts; The titanium sulfate of being got is joined in the sulphuric acid soln, and stirring and dissolving promptly gets titanium source dispersion soln, and is standby;
Step 2 is got the sodium hydroxide (NaOH) of 11.2 mass parts; Get the sodium sulfate (Na that 60 mass parts concentration are 0.1mol/L 2SO 4) solution; In the metabisulfite solution that the sodium hydroxide of being got is joined, stirring and dissolving promptly gets the alkali source dispersion soln, and is standby;
Step 3 is transferred to the alkali source dispersion soln that makes in the reactor, in the whipping process with the method even heating to 60 of oil bath ℃, titanium source dispersion soln is joined in the middle of the alkali source dispersion soln then, generate white precipitate in the reaction process, reaction times is 24 hours, and post reaction mixture is sent into whizzer, centrifugation, isolated centrifugate reclaims, and isolated throw out is standby;
Step 4 adds the isolated throw out of step 3 in the distilled water, the consumption of distilled water is 0.5 times of throw out quality, send into whizzer after mixing, centrifugation, isolated centrifugate reclaims, and isolated throw out mixes with distilled water according to aforementioned proportion again, after send into whizzer, centrifugation, isolated centrifugate reclaims, and isolated throw out is standby;
Step 5 uses the aqueous ethanolic solution of being made up of the ethanol of 80% distilled water and 20% to replace distilled water, according to the method for step 4 the isolated throw out of its and step 4 is mixed also centrifugation, and isolated throw out is standby;
Step 6 is mixed the isolated throw out of step 5 with dehydrated alcohol, the add-on of dehydrated alcohol is 0.8 times of throw out quality, sends into whizzer after mixing and separates, and isolated throw out is standby;
Step 7 is sent the isolated throw out of step 6 into vacuum drying oven, and take out dry back, promptly makes rutile type titanium dioxide nano particle, and particle diameter is 4.21nm.
Embodiment 2
A kind of preparation method of rutile type titanium dioxide nano particle comprises the steps:
Step 1 is with 6 parts of (mass fraction, below all with) titanium sulfate (Ti (SO 4) 2) join in 27 parts of sulphuric acid solns, stirring and dissolving promptly gets titanium source dispersion soln, and is standby; H in the described sulphuric acid soln 2SO 4(dense): H 2O=1: 4.
Step 2 is with 15.7094 parts of potassium hydroxide (KOH) vitriolate of tartar (K that to join 20 parts of concentration be 1.5mol/L 2SO 4) in the solution, stirring and dissolving promptly gets the alkali source dispersion soln, and is standby;
Step 3 places reactor with the alkali source dispersion soln of making, even heating to 95 ℃, after titanium source dispersion soln is joined in the alkali source dispersion soln, generate white precipitate in the reaction process, reaction times is 24 hours, and post reaction mixture is sent into whizzer, centrifugation, isolated centrifugate reclaims, and isolated throw out is standby;
Step 4 adds the isolated throw out of step 3 in the distilled water, the consumption of distilled water is 0.8 times of throw out quality, send into whizzer after mixing, centrifugation, isolated centrifugate reclaims, and isolated throw out mixes with distilled water according to aforementioned proportion again, after send into whizzer, centrifugation, isolated centrifugate reclaims, and isolated throw out is standby;
Step 5 uses the aqueous ethanolic solution of being made up of the ethanol of 80% distilled water and 20% to replace distilled water, according to the method for step 4 the isolated throw out of its and step 4 is mixed also centrifugation, and isolated throw out is standby;
Step 6 is mixed the isolated throw out of step 5 with dehydrated alcohol, the add-on of dehydrated alcohol is 1.2 times of throw out quality, sends into whizzer after mixing and separates, and isolated throw out is standby;
Step 7 is sent the isolated throw out of step 6 into vacuum drying oven, and take out dry back, promptly makes rutile type titanium dioxide nano particle, and particle diameter is 4.9nm.
Embodiment 3
A kind of preparation method of rutile type titanium dioxide nano particle comprises the steps:
Step 1 is with 6 parts of titanium sulfate (Ti (SO 4) 2) join in 27 parts of sulphuric acid solns, stirring and dissolving promptly gets titanium source dispersion soln, and is standby; H in the described sulphuric acid soln 2SO 4(dense): H 2O=1: 4.
Step 2 is with 11.2 parts of sodium hydroxide (NaOH) sodium sulfate (Na that to join 60 parts of concentration be 1.5mol/L 2SO 4) in the solution, stirring fully dissolves it, promptly gets the alkali source dispersion soln, standby;
Step 3 is transferred to the alkali source dispersion soln that makes in the reactor, stirring down, oil bath is heated to 95 ℃, titanium source dispersion soln is joined in the middle of the alkali source dispersion soln then, the adularescent precipitation generates in the reaction process, react end in 6 hours, post reaction mixture is sent into whizzer, centrifugation, reclaim centrifugate, isolated throw out carries out next step;
Step 4 adds the isolated throw out of step 3 in the distilled water, the consumption of distilled water is 1.5 times of throw out quality, send into whizzer after mixing, centrifugation, isolated centrifugate reclaims, and isolated throw out mixes with distilled water according to aforementioned proportion again, after send into whizzer, centrifugation, isolated centrifugate reclaims, and isolated throw out is standby;
Step 5 uses the aqueous ethanolic solution of being made up of the ethanol of 80% distilled water and 20% to replace distilled water, according to the method for step 4 the isolated throw out of its and step 4 is mixed also centrifugation, and isolated throw out is standby;
Step 6 is mixed the isolated throw out of step 5 with dehydrated alcohol, the add-on of dehydrated alcohol is 1.5 times of throw out quality at least, sends into whizzer after mixing and separates, and isolated throw out is standby;
Step 7 is sent the isolated throw out of step 6 into vacuum drying oven, and take out dry back, promptly makes rutile type titanium dioxide nano particle, and particle diameter is 3.76nm.
Embodiment 4
A kind of preparation method of rutile type titanium dioxide nano particle comprises the steps:
Step 1 is with 4.7428 parts of titanium tetrachloride (TiCl 4) join in 20 parts the hydrochloric acid soln, stirring and dissolving promptly gets titanium source dispersion soln, and is standby; HCl in the described hydrochloric acid soln: H 2O=1: 1;
Step 2 is with in 14.6038 parts of potassium hydroxide (KOH) Repone K (KCl) solution that to join 20 parts of concentration be 2.0mol/L, and stirring and dissolving promptly gets the alkali source dispersion soln, and is standby;
Step 3 is transferred to the alkali source dispersion soln that makes in the reactor, stirring down, oil bath is heated to 80 ℃, titanium source dispersion soln is joined in the middle of the alkali source dispersion soln then, the adularescent precipitation generates, react after 12 hours, post reaction mixture is sent into whizzer, centrifugation, reclaim centrifugate, isolated throw out carries out next step;
Step 4 adds the isolated throw out of step 3 in the distilled water, the consumption of distilled water is 2 times of throw out quality, send into whizzer after mixing, centrifugation, isolated centrifugate reclaims, and isolated throw out mixes with distilled water according to aforementioned proportion again, after send into whizzer, centrifugation, isolated centrifugate reclaims, and isolated throw out is standby;
Step 5 uses the aqueous ethanolic solution of being made up of the ethanol of 80% distilled water and 20% to replace distilled water, according to the method for step 4 the isolated throw out of its and step 4 is mixed also centrifugation, and isolated throw out is standby;
Step 6 is mixed the isolated throw out of step 5 with dehydrated alcohol, the add-on of dehydrated alcohol is 2 times of throw out quality, sends into whizzer after mixing and separates, and isolated throw out is standby;
Step 7 is sent the isolated throw out of step 6 into vacuum drying oven, and take out dry back, promptly makes rutile type titanium dioxide nano particle, and particle diameter is 4.4nm.
Embodiment 5
A kind of preparation method of rutile type titanium dioxide nano particle comprises the steps:
Step 1 is got 3.9989 parts of titanyl sulfate (TiOSO 4) as the titanium source; Join stirring and dissolving in 10 parts of sulphuric acid solns, promptly get titanium source dispersion soln, standby, H in the described sulphuric acid soln 2SO 4(dense): H 2O=1: 4.
It is in the metabisulfite solution of 2.0mol/L that step 2 joins 20 parts of concentration with 2.8163 parts of sodium hydroxide (NaOH), and stirring and dissolving promptly gets the alkali source dispersion soln, and is standby;
Step 3 places reactor with the alkali source dispersion soln of making, even heating to 80 ℃, after titanium source dispersion soln is joined in the alkali source dispersion soln, generate white precipitate in the reaction process, reaction times is 1 hour, and post reaction mixture is sent into whizzer, centrifugation, isolated centrifugate reclaims, and isolated throw out is standby;
Step 4 adds the isolated throw out of step 3 in the distilled water, the consumption of distilled water is 0.5 times of throw out quality, send into whizzer after mixing, centrifugation, isolated centrifugate reclaims, and isolated throw out mixes with distilled water according to aforementioned proportion again, after send into whizzer, centrifugation, isolated centrifugate reclaims, and isolated throw out is standby;
Step 5 uses the aqueous ethanolic solution of being made up of the ethanol of 80% distilled water and 20% to replace distilled water, according to the method for step 4 the isolated throw out of its and step 4 is mixed also centrifugation, and isolated throw out is standby;
Step 6 is mixed the isolated throw out of step 5 with dehydrated alcohol, the add-on of dehydrated alcohol is 0.8 times of throw out quality at least, sends into whizzer after mixing and separates, and isolated throw out is standby;
Step 7 is sent the isolated throw out of step 6 into vacuum drying oven, and take out dry back, promptly makes rutile type titanium dioxide nano particle, and particle diameter is 2.3nm.
Because it is too many influence the factor in titanium dioxide nano granule footpath, embodiment can't enumerate one by one, therefore all in described time of this specification sheets, concentration range the arbitrary condition of change, all can exert an influence to the product cut size size.

Claims (2)

1. the preparation method of a rutile type titanium dioxide nano particle is characterized in that: comprise the steps:
Step 1, get a kind of in titanium sulfate, titanyl sulfate or the titanium chloride, its mass fraction is 3~6 parts; Get a kind of in sulfuric acid or the hydrochloric acid soln, its mass fraction is 10~27 parts; Two kinds of raw materials choosing are mixed, and titanium source dispersion soln is made in dissolving, and is standby;
Step 2, get a kind of in sodium hydroxide or the potassium hydroxide, its mass fraction is 2.8~16 parts; Get a kind of in sodium sulfate, vitriolate of tartar, sodium-chlor or the Klorvess Liquid, its mass fraction is 20~60 parts, concentration 〉=0.1mol/L; Two kinds of raw materials choosing are mixed, and the alkali source dispersion soln is made in dissolving, and is standby;
Step 3, the alkali source dispersion soln of making is placed reactor, even heating to 60~95 ℃, after titanium source dispersion soln is joined in the alkali source dispersion soln, generate white precipitate in the reaction process, reaction times is 1~24 hour, and post reaction mixture is sent into whizzer, centrifugation, isolated centrifugate reclaims, and isolated throw out is standby;
Step 4, the isolated throw out of step 3 is added in the distilled water, the consumption of distilled water is at least 0.5 times of throw out quality, send into whizzer after mixing, centrifugation, isolated centrifugate reclaims, and isolated throw out mixes with distilled water according to aforementioned proportion again, after send into whizzer, centrifugation, isolated centrifugate reclaims, and isolated throw out is standby;
Step 5, use the aqueous ethanolic solution of being made up of the ethanol of 80% distilled water and 20% to replace distilled water, according to the method for step 4 the isolated throw out of its and step 4 is mixed also centrifugation, isolated throw out is standby;
Step 6, the isolated throw out of step 5 is mixed with dehydrated alcohol, the add-on of dehydrated alcohol is 0.8 times of throw out quality at least, sends into whizzer after mixing and separates, and isolated throw out is standby;
Step 7, the isolated throw out of step 6 is sent into vacuum drying oven, take out dry back, promptly makes rutile type titanium dioxide nano particle.
2. the preparation method of a kind of rutile type titanium dioxide nano particle according to claim 1 is characterized in that: concentration assurance pH≤0 of described sulfuric acid or hydrochloric acid soln.
CN 201010146615 2010-04-08 2010-04-08 Preparation method of rutile type titanium dioxide nano particle Expired - Fee Related CN101805017B (en)

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CN102120612A (en) * 2011-01-27 2011-07-13 洛阳师范学院 Preparation method of anatase type titanium dioxide nanoparticles
CN110339864A (en) * 2019-07-25 2019-10-18 河南嘉利美环保材料有限公司 One kind containing TiO2The spheric granules of purification factor
CN116375024A (en) * 2023-03-20 2023-07-04 昆明理工大学 Preparation method of titanium oxide coated diamond powder

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CN110339864A (en) * 2019-07-25 2019-10-18 河南嘉利美环保材料有限公司 One kind containing TiO2The spheric granules of purification factor
CN116375024A (en) * 2023-03-20 2023-07-04 昆明理工大学 Preparation method of titanium oxide coated diamond powder

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