CN109338454A - The preparation method of the siliceous titanium dioxide crystal whisker of rutile-type - Google Patents
The preparation method of the siliceous titanium dioxide crystal whisker of rutile-type Download PDFInfo
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- CN109338454A CN109338454A CN201811121437.5A CN201811121437A CN109338454A CN 109338454 A CN109338454 A CN 109338454A CN 201811121437 A CN201811121437 A CN 201811121437A CN 109338454 A CN109338454 A CN 109338454A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
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Abstract
The invention belongs to the technical fields of siliceous titanium dioxide crystal whisker preparation, are related to a kind of preparation method of siliceous titanium dioxide crystal whisker of rutile-type.The present invention includes the following steps, titanium oxide-tin oxide/activation attapulgite composite material is made in attapulgite and pink salt and metatitanic acid after acid activation, add the phosphate of sodium, the sinter that mixture is made is calcined, using dispersing, be filtered, washed, be dried to obtain the siliceous titanium dioxide crystal whisker of rutile-type.The present invention is during synthesis of titanium dioxide whisker, it joined activation attapulgite, its club shaped structure plays the role of shape inducer, its active oxidation silicon components acts as the effect of cosolvent, to reduce synthesis temperature, and the present invention is added with the phosphate and tin oxide of sodium, plays the role of collaboration to the formation of rutile titanium dioxide and promotes.
Description
Technical field
The invention belongs to the technical fields of siliceous titanium dioxide crystal whisker preparation, are related to a kind of siliceous titanium dioxide of rutile-type
The preparation method of whisker.
Background technique
Titanium dioxide crystal whisker is a kind of composite material reinforcing fiber for possessing excellent properties, using its excellent draw ratio,
The properties such as good mechanical property, electrical insulating property, low heat conductivity are widely used in conductive material, reinforcing material, electrical isolation material
The base of the substances such as material, heat-insulating material, filler, catalyst carrier.
Currently, the method for synthesis of titanium dioxide whisker mainly includes sintering process, hydro-thermal method, fusion method etc..Chinese patent
200710037251.7 refer to that titanium source material, raw material containing potassium and cosolvent mixing will be contained, and are sintered, will be sintered at 600-1300 DEG C
Object obtains the variable conversion sizing object of titanium dioxide crystal whisker after dispersing naturally, then after pickling takes off K+ ion；Finally washing,
It is dry, it is sintered under 600-1300 DEG C of high temperature, obtaining length is 50-100 μm, 5-10 μm of diameter of titanium dioxide crystal whisker.But it should
Preparation process is relatively lengthy and jumbled, needs by high-temperature burning process twice, and preparation cost is higher, seriously limits its high-volume
Production.
Chinese patent 96117084.0 propose using amorphous titania powder, potassium hydroxide and deionized water as raw material,
Hydro-thermal 2-16h under conditions of 100-220 DEG C, preparing length is 15-30 μm, 1-3 μm of diameter of titanium dioxide crystal whisker.But it should
It is simple process, easily operated, but its preparation process needs high temperature and pressure, and its yield is lower, is unfavorable for industrialized production.
Summary of the invention
Regarding the issue above, the present invention provides a kind of preparation side of the siliceous titanium dioxide crystal whisker of rutile-type
Method.
In order to achieve the above objectives, present invention employs following technical proposals:
A kind of preparation method of the siliceous titanium dioxide crystal whisker of rutile-type, comprising the following steps:
Step 1: being added pink salt in oxytropism activator solution, after completely dissolution, sequentially adds attapulgite and inclined titanium
Acid stirs 0.5-3h controlled at 25-60 DEG C, adjusts pH value to 6.0-7.0 with alkaline solution, filtering, washing filter cake until
Cleaning solution conductivity after washing dry, pulverize less than 300 μ S/cm, and it is compound to obtain titanium oxide-tin oxide/activation attapulgite
Material；
Step 2: the phosphorus of sodium is added in titanium oxide-tin oxide/activation attapulgite composite material obtained into step 1
Hydrochlorate is uniformly mixed, is placed under air atmosphere, in 850-1200 DEG C of temperature lower calcination 2-5h, cooled to room temperature is obtained
The sinter of mixture；
Step 3: being placed in water dispersion for the sinter of mixture obtained in step 2, filters, and washs, dry, obtains
The siliceous titanium dioxide crystal whisker of rutile-type.
Acidic activator solution in the preparation method of the above-mentioned siliceous titanium dioxide crystal whisker of rutile-type, in step 1
For the hydrochloric acid solution of 1-5mol/L, alkaline solution is ammonium hydroxide.
In the preparation method of the above-mentioned siliceous titanium dioxide crystal whisker of rutile-type, pink salt in step 1 be stannic chloride,
Stannous chloride or nitric acid tin.
In the preparation method of the above-mentioned siliceous titanium dioxide crystal whisker of rutile-type, metatitanic acid and attapulgite in step 1
Mass ratio be 1.0-2.5:1, the quality summation of metatitanic acid and attapulgite is 0.2-0.5:1 with the mass ratio of hydrochloric acid solution.
In the preparation method of the above-mentioned siliceous titanium dioxide crystal whisker of rutile-type, in step 1 the addition quality of pink salt with
Stannic oxide meter, the mass ratio with metatitanic acid are 0.005-0.03:1.
In the preparation method of the above-mentioned siliceous titanium dioxide crystal whisker of rutile-type, the phosphate of sodium is phosphoric acid in step 2
Sodium dihydrogen, disodium hydrogen phosphate, sodium pyrophosphate or calgon.
In the preparation method of the above-mentioned siliceous titanium dioxide crystal whisker of rutile-type, the phosphate of sodium and oxidation in step 2
Titanium-tin oxide/activation attapulgite composite material mass ratio is 0.03-0.07:1.
In the preparation method of the above-mentioned siliceous titanium dioxide crystal whisker of rutile-type, at the end of being washed in step 3, washing
Cleaning solution afterwards is substantially in neutrality.
Compared with prior art, the present invention has the advantages that
1, the present invention joined activation attapulgite, club shaped structure plays during synthesis of titanium dioxide whisker
The effect of shape inducer, active oxidation silicon components act as the effect of cosolvent, to reduce synthesis temperature.
2, the present invention is added with the phosphate and tin oxide of sodium, plays collaboration to the formation of rutile titanium dioxide and promotees
Into effect.
3, the present invention utilizes hydrochloric acid activation attapulgite, while solving solidifying metatitanic acid, so that it is recessed to prepare titanium oxide/activation
Convex stick stone composite material, on the one hand improves the utilization rate of hydrochloric acid, reduces the generation of spent acid, on the other hand due to silica and
The isoelectric point of titanium oxide is different, and the solidifying nano-titanium oxide formed of metatitanic acid solution can form preferable packet on activation attapulgite surface
Coating.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of the siliceous titanium dioxide crystal whisker of rutile-type obtained in embodiment 3；
Specific embodiment
Reagent as used in the following examples can be commercially available unless otherwise specified from routine biochemistry reagent shop.
Embodiment 1
The present embodiment provides a kind of preparation methods of the siliceous titanium dioxide crystal whisker of rutile-type, specifically, including it is following
Step:
Step 1: 0.63g stannous chloride being added into the hydrochloric acid solution of 280g 1mol/L, after completely dissolution, then successively adds
Enter 40g attapulgite and 100g metatitanic acid, controlled at 25 DEG C, stir 0.5h, with ammonia spirit adjusting pH value to 6.0, mistake
Filter cake is washed in filter, and washing measures the cleaning solution conductivity after washing when completing be 287 μ S/cm, dry, pulverize, is aoxidized
Titanium-tin oxide/activation attapulgite composite material；
Step 2: 4.2g phosphorus is added in titanium oxide-tin oxide/activation attapulgite composite material obtained into step 1
Acid dihydride sodium is uniformly mixed, is placed under air atmosphere, in 850 DEG C of temperature lower calcination 2h, cooled to room temperature is mixed
Close the sinter of material；
Step 3: being placed in water dispersion for the sinter of mixture obtained in step 2, filters, and washing, washing is completed
When to measure the cleaning solution pH value after washing be 6.58, it is dry, obtain the siliceous titanium dioxide crystal whisker of rutile-type.
Embodiment 2
The present embodiment provides a kind of preparation methods of the siliceous titanium dioxide crystal whisker of rutile-type, specifically, including it is following
Step:
Step 1: 3.77g stannous chloride is added into the hydrochloric acid solution of 1000g 5mol/L, after completely dissolution, then successively
100g attapulgite and 100g metatitanic acid is added, controlled at 60 DEG C, stirs 3h, with ammonia spirit adjusting pH value to 7.0, mistake
Filter cake is washed in filter, and washing measures the cleaning solution conductivity after washing when completing be 300 μ S/cm, dry, pulverize, is aoxidized
Titanium-tin oxide/activation attapulgite composite material；
Step 2: 14.3g is added in titanium oxide-tin oxide/activation attapulgite composite material obtained into step 1
Sodium dihydrogen phosphate is uniformly mixed, is placed under air atmosphere, in 1200 DEG C of temperature lower calcination 5h, cooled to room temperature is obtained
The sinter of mixture；
Step 3: being placed in water dispersion for the sinter of mixture obtained in step 2, filters, and washing, washing is completed
When to measure the cleaning solution pH value after washing be 6.62, it is dry, obtain the siliceous titanium dioxide crystal whisker of rutile-type.
Embodiment 3
The present embodiment provides a kind of preparation methods of the siliceous titanium dioxide crystal whisker of rutile-type, specifically, including it is following
Step:
Step 1: 2.20g stannous chloride being added into the hydrochloric acid solution of 640g 3mol/L, after completely dissolution, then successively adds
Enter 70g attapulgite and 100g metatitanic acid, controlled at 40 DEG C, stir 1.5h, with ammonia spirit adjusting pH value to 6.5, mistake
Filter cake is washed in filter, and washing measures the cleaning solution conductivity after washing when completing be 293 μ S/cm, dry, pulverize, is aoxidized
Titanium-tin oxide/activation attapulgite composite material；
Step 2: 8.5g phosphorus is added in titanium oxide-tin oxide/activation attapulgite composite material obtained into step 1
Acid dihydride sodium is uniformly mixed, is placed under air atmosphere, in 1000 DEG C of temperature lower calcination 3.5h, cooled to room temperature is obtained
The sinter of mixture；
Step 3: being placed in water dispersion for the sinter of mixture obtained in step 2, filters, and washing, washing is completed
When to measure the cleaning solution pH value after washing be 6.60, it is dry, obtain the siliceous titanium dioxide crystal whisker of rutile-type, resulting rutile
The transmission electron microscope picture of the siliceous titanium dioxide crystal whisker of type is as shown in Figure 1, wherein transmission electron microscope picture is given birth to by Thermo Fischer Scient Inc.
The 20 type transmission electron microscope of Tecnai G2 of production measures.
Embodiment 4
The present embodiment provides a kind of preparation methods of the siliceous titanium dioxide crystal whisker of rutile-type, specifically, including it is following
Step:
Step 1: 3.02g stannic chloride is added into the hydrochloric acid solution of 640g 3mol/L and sequentially adds after completely dissolution
70g attapulgite and 100g metatitanic acid stir 1.5h controlled at 40 DEG C, with ammonia spirit adjusting pH value to 6.5, filter,
Filter cake is washed, washing measures the cleaning solution conductivity after washing when completing be 290 μ S/cm, dry, pulverize, obtains titanium oxide-oxygen
Change tin/activation attapulgite composite material；
Step 2: 8.5g phosphorus is added in titanium oxide-tin oxide/activation attapulgite composite material obtained into step 1
Sour disodium hydrogen is uniformly mixed, is placed under air atmosphere, in 1000 DEG C of temperature lower calcination 3.5h, cooled to room temperature is obtained
The sinter of mixture；
Step 3: being placed in water dispersion for the sinter of mixture obtained in step 2, filters, and washing, washing is completed
When to measure the cleaning solution pH value after washing be 6.54, it is dry, obtain the siliceous titanium dioxide crystal whisker of rutile-type.
Embodiment 5
The present embodiment provides a kind of preparation methods of the siliceous titanium dioxide crystal whisker of rutile-type, specifically, including it is following
Step:
Step 1: 4.26g nitric acid tin is added into the hydrochloric acid solution of 640g 3mol/L and sequentially adds after completely dissolution
70g attapulgite and 100g metatitanic acid stir 1.5h controlled at 40 DEG C, with ammonia spirit adjusting pH value to 6.5, filter,
Filter cake is washed, washing measures the cleaning solution conductivity after washing when completing be 295 μ S/cm, dry, pulverize, obtains titanium oxide-oxygen
Change tin/activation attapulgite composite material；
Step 2: it is burnt that 8.5g is added in titanium oxide-tin oxide/activation attapulgite composite material obtained into step 1
Sodium phosphate is uniformly mixed, is placed under air atmosphere, in 1000 DEG C of temperature lower calcination 3.5h, cooled to room temperature is mixed
Close the sinter of material；
Step 3: being placed in water dispersion for the sinter of mixture obtained in step 2, filters, and washing, washing is completed
When to measure the cleaning solution pH value after washing be 6.64, it is dry, obtain the siliceous titanium dioxide crystal whisker of rutile-type.
Embodiment 6
The present embodiment provides a kind of preparation methods of the siliceous titanium dioxide crystal whisker of rutile-type, specifically, including it is following
Step:
Step 1: 4.26g nitric acid tin is added into the hydrochloric acid solution of 640g 3mol/L and sequentially adds after completely dissolution
70g attapulgite and 100g metatitanic acid stir 1.5h controlled at 40 DEG C, with ammonia spirit adjusting pH value to 6.5, filter,
Filter cake is washed, washing measures the cleaning solution conductivity after washing when completing be 292 μ S/cm, dry, pulverize, obtains titanium oxide-oxygen
Change tin/activation attapulgite composite material；
Step 2: 8.5g six is added in titanium oxide-tin oxide/activation attapulgite composite material obtained into step 1
Sodium metaphosphate is uniformly mixed, is placed under air atmosphere, in 1000 DEG C of temperature lower calcination 3.5h, cooled to room temperature is obtained
The sinter of mixture；
Step 3: being placed in water dispersion for the sinter of mixture obtained in step 2, filters, and washing, washing is completed
When to measure the cleaning solution pH value after washing be 6.67, it is dry, obtain the siliceous titanium dioxide crystal whisker of rutile-type.
Specific embodiment described herein is only an example for the spirit of the invention.The neck of technology belonging to the present invention
The technical staff in domain can make various modifications or additions to the described embodiments or replace by a similar method
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (8)
1. a kind of preparation method of the siliceous titanium dioxide crystal whisker of rutile-type, which comprises the following steps:
Step 1: being added pink salt in oxytropism activator solution, after completely dissolution, sequentially adds attapulgite and metatitanic acid,
Controlled at 25-60 DEG C, 0.5-3h is stirred, adjusts pH value to 6.0-7.0 with alkaline solution, filtering, washing filter cake is until wash
Cleaning solution conductivity after washing dry, pulverize less than 300 μ S/cm, obtain titanium oxide-tin oxide/activation attapulgite composite wood
Material；
Step 2: the phosphoric acid of sodium is added in titanium oxide-tin oxide/activation attapulgite composite material obtained into step 1
Salt is uniformly mixed, is placed under air atmosphere, in 850-1200 DEG C of temperature lower calcination 2-5h, cooled to room temperature is mixed
Close the sinter of material；
Step 3: being placed in water dispersion for the sinter of mixture obtained in step 2, filters, and washs, dry, obtains golden red
The siliceous titanium dioxide crystal whisker of stone-type.
2. the preparation method of the siliceous titanium dioxide crystal whisker of rutile-type as described in claim 1, it is characterised in that: in step 1
Acidic activator solution be 1-5mol/L hydrochloric acid solution, alkaline solution is ammonium hydroxide.
3. the preparation method of the siliceous titanium dioxide crystal whisker of rutile-type as described in claim 1, it is characterised in that: in step 1
Pink salt be stannic chloride, stannous chloride or nitric acid tin.
4. the preparation method of the siliceous titanium dioxide crystal whisker of rutile-type as described in claim 1, it is characterised in that: in step 1
The mass ratio of metatitanic acid and attapulgite is 1.0-2.5:1, the quality summation of metatitanic acid and attapulgite, the matter with hydrochloric acid solution
Amount is than being 0.2-0.5:1.
5. the preparation method of the siliceous titanium dioxide crystal whisker of rutile-type as described in claim 1, it is characterised in that: in step 1
For the addition quality of pink salt in terms of stannic oxide, the mass ratio with metatitanic acid is 0.005-0.03:1.
6. the preparation method of the siliceous titanium dioxide crystal whisker of rutile-type as described in claim 1, it is characterised in that: in step 2
The phosphate of sodium is sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium pyrophosphate or calgon.
7. the preparation method of the siliceous titanium dioxide crystal whisker of rutile-type as described in claim 1, it is characterised in that: in step 2
The phosphate and titanium oxide-tin oxide/activation attapulgite composite material mass ratio of sodium are 0.03-0.07:1.
8. the preparation method of the siliceous titanium dioxide crystal whisker of rutile-type as described in claim 1, it is characterised in that: in step 3
At the end of washing, the cleaning solution after washing is substantially in neutrality.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110882713A (en) * | 2019-11-22 | 2020-03-17 | 常州纳欧新材料科技有限公司 | Conductive attapulgite/titanium oxide/carbon nitride quantum dot composite material, preparation method thereof and application thereof in photocatalytic desulfurization |
| CN115873306A (en) * | 2022-12-14 | 2023-03-31 | 江苏纳欧新材料有限公司 | Preparation method of conductive material with high length-diameter ratio and high whiteness |
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| CN102580713A (en) * | 2012-01-18 | 2012-07-18 | 常州大学 | Method for preparing titanium dioxide/silicate mineral nano composites |
| JP2015182938A (en) * | 2014-03-25 | 2015-10-22 | 多木化学株式会社 | Rutile-type titanium oxide sol and method for producing the same |
| CN106698504A (en) * | 2016-11-24 | 2017-05-24 | 攀枝花市钛都化工有限公司 | Salt treatment method for rutile titanium dioxide and treated titanium dioxide initial product |
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2018
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| CN102580713A (en) * | 2012-01-18 | 2012-07-18 | 常州大学 | Method for preparing titanium dioxide/silicate mineral nano composites |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110882713A (en) * | 2019-11-22 | 2020-03-17 | 常州纳欧新材料科技有限公司 | Conductive attapulgite/titanium oxide/carbon nitride quantum dot composite material, preparation method thereof and application thereof in photocatalytic desulfurization |
| CN110882713B (en) * | 2019-11-22 | 2022-04-26 | 常州纳欧新材料科技有限公司 | Conductive attapulgite/titanium oxide/carbon nitride quantum dot composite material, preparation method thereof and application thereof in photocatalytic desulfurization |
| CN115873306A (en) * | 2022-12-14 | 2023-03-31 | 江苏纳欧新材料有限公司 | Preparation method of conductive material with high length-diameter ratio and high whiteness |
| CN115873306B (en) * | 2022-12-14 | 2024-02-06 | 江苏纳欧新材料有限公司 | Preparation method of high-length-diameter-ratio and high-whiteness conductive material |
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