CN107858755A - Using titaniferous waste material as sodium hexatitanate whisker of raw material and preparation method thereof - Google Patents
Using titaniferous waste material as sodium hexatitanate whisker of raw material and preparation method thereof Download PDFInfo
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- CN107858755A CN107858755A CN201711145652.4A CN201711145652A CN107858755A CN 107858755 A CN107858755 A CN 107858755A CN 201711145652 A CN201711145652 A CN 201711145652A CN 107858755 A CN107858755 A CN 107858755A
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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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- 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
- C30B29/22—Complex oxides
- C30B29/32—Titanates; Germanates; Molybdates; Tungstates
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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of using titaniferous waste material as sodium hexatitanate whisker of raw material and preparation method thereof.Its technical scheme is：Titaniferous waste material is heat-treated 2 ~ 4 hours under the conditions of 1000 ~ 1300 DEG C, grinding to granularity is less than 0.045mm, obtains grinding material A.50 ~ 70wt% grinding material A, 10 ~ 20wt% titanium dioxide and 10 ~ 30wt% thermosetting resin are mixed, it is compressing, it is heat-treated 1 ~ 3 hour, crushes, grinding to granularity is less than 0.088mm, obtains grinding material B in 1200 ~ 1400 DEG C and neutral atmosphere.40 ~ 60wt% grinding material B, 10 ~ 30wt% natrium carbonicum calcinatum and 10 ~ 30wt% sodium acetate trihydrate are mixed, grinding, it is heat-treated 1 ~ 3 hour under the conditions of 400 ~ 600 DEG C, it is heat-treated 1 ~ 3 hour under the conditions of 800 ~ 1000 DEG C, grinding to granularity is less than 0.088mm, and the sodium hexatitanate whisker using titaniferous waste material as raw material is made.Production cost of the present invention is low and technique is simple, the crystallinity height and size uniform of made product.
Description
Technical field
The invention belongs to sodium hexatitanate whisker technical field.More particularly to a kind of sodium hexatitanate using titaniferous waste material as raw material
Whisker and preparation method thereof.
Background technology
There is sodium hexatitanate whisker high intensity, low-heat to lead and the characteristic such as environmental protection, in friction, biology, catalysis, heat-insulated and compound
The fields such as material are with a wide range of applications.Current preparation method mainly has hydro-thermal method, sintering process, flux growth metrhod, melting
Method etc., though each having the advantages of different, all come with some shortcomings：Hydro-thermal method needs HTHP, condition harshness；Sintering process
Whisker separation difficulty is prepared, size is difficult to control；Though the whisker draw ratio of flux growth metrhod preparation is big, size is controllable, by fluxing
The impurity that agent introduces is mingled with the product, it is difficult to remove the performance for totally, influenceing whisker；Fusion method is needed raw material high temperature melting
Melt, and by subsequent material by twice or multiple high temp calcination processing, obtained whisker in crystallization process easy conglomeration with
Blocking, energy consumption is big and production cost is too high.
In recent years, with the fast development of the industries such as chemical industry, biology, the purposes of titanium and its compound is more and more wider, is producing
Caused titaniferous waste material is also more and more during product production and use, how efficiently to utilize titaniferous waste material, turns into one very
Important and urgent research work.Currently, it is more for the recoverying and utilizing method of titaniferous waste material development, such as pass through congruent melting, chemistry
The technique recovery Pds such as leaching, crystallization and calcining, though known progress is achieved, the existing most complex process of technical method,
And after extracting titanium, it can still produce secondary slugs.
The content of the invention
It is contemplated that overcome the deficiencies in the prior art, it is therefore an objective to provide that a kind of production cost is low and technique simply with containing
Titanium waste material is the preparation method of the sodium hexatitanate whisker of raw material；The sodium hexatitanate using titaniferous waste material as raw material prepared with this method
The crystallinity height and size uniform of whisker.
To achieve the above object, the step of the technical solution adopted by the present invention is be：
The first step, titaniferous waste material is heat-treated 2 ~ 4 hours under the conditions of 1000 ~ 1300 DEG C, then grinding to granularity is less than
0.045mm, obtain grinding material A.
Second step, grinding material A, 10 ~ 20wt% titanium dioxide and the 10 ~ 30wt% thermosetting resin by 50 ~ 70wt%
It is well mixed, it is compressing under the conditions of 50 ~ 100MPa, 1 ~ 3 is heat-treated under the conditions of 1200 ~ 1400 DEG C and in neutral atmosphere
Hour, crush, grinding to granularity is less than 0.088mm, obtains grinding material B.
3rd step, the grinding material B, 10 ~ 30wt% natrium carbonicum calcinatum and 10 ~ 30wt% three water second by 40 ~ 60wt%
Sour sodium is well mixed, and is ground 0.5 ~ 1 hour；Then it is heat-treated 1 ~ 3 hour under the conditions of 400 ~ 600 DEG C, then at 800 ~ 1000 DEG C
Under the conditions of be heat-treated 1 ~ 3 hour, grinding to granularity is less than 0.088mm, and sodium hexatitanate whisker using titaniferous waste material as raw material is made.
The titaniferous waste material：Ti contents are more than 52wt%, and Al, Ni, V, Co, Cr, Ca and Si content summation are less than
0.9wt%；The granularity of titaniferous waste material is less than 0.088mm.
The granularity of the titanium dioxide is less than 0.088mm；TiO in the titanium dioxide2Content be more than 99wt%.
The neutral atmosphere is nitrogen atmosphere or is argon gas atmosphere.
The granularity of the natrium carbonicum calcinatum is less than 0.088mm；Na in the natrium carbonicum calcinatum2CO3Content be more than 99wt%.
Due to there is following good effect compared with prior art using above-mentioned technical proposal, the present invention：
(1) the present invention accompanies on the Research foundations such as temperature evolution to the composition of titaniferous waste material, structure and its thing, by the system of product
Standby process substep controls：Feedstock property regulation, formation interphase and whisker grow.By the granularity of considered critical raw material and
The technical parameter of the preparation process such as the granularity of intermediate product, treatment temperature, processing time, atmosphere, it is the shape of sodium hexatitanate whisker
Necessary requirement is provided into growing up, makes prepared crystallinity height and chi using titaniferous waste material as the sodium hexatitanate whisker of raw material
It is very little uniform.
(2) the present invention is using titaniferous waste material as primary raw material, then is equipped with the works such as titanium dioxide, thermosetting resin and natrium carbonicum calcinatum
The common raw material of industry, preparation process substep is controlled, energy consumption and loss of material caused by both having reduced high-temperature process, and to whisker
Different growth phases have carried out accurate adjustment, realize the Balance route of properties of product, preparation process energy consumption and Material Cost.Cause
This, not only used raw material sources are extensive, and simple production process and production cost are low.
The present invention prepare using titaniferous waste material as raw material sodium hexatitanate whisker after testing：A diameter of 0.5 ~ 2 μm；Length is
3~20μm；Whisker size is uniform, and crystallinity is high.
Therefore, production cost of the present invention is low and technique is simple, prepared brilliant using titaniferous waste material as the sodium hexatitanate of raw material
The crystallinity height and size uniform of palpus.
Embodiment
With reference to embodiment, the present invention will be further described, not to the limitation of its protection domain.
It is first that the raw material Unify legislation of present embodiment is as follows to avoid repeating, repeated no more in each embodiment：
The titaniferous waste material：Ti contents are more than 52wt%, and Al, Ni, V, Co, Cr, Ca and Si content summation are less than 0.9wt%；Contain
The granularity of titanium waste material is less than 0.088mm.
The granularity of the titanium dioxide is less than 0.088mm；TiO in the titanium dioxide2Content be more than 99wt%.
The granularity of the natrium carbonicum calcinatum is less than 0.088mm；Na in the natrium carbonicum calcinatum2CO3Content be more than 99wt%.
Embodiment 1
It is a kind of using titaniferous waste material as sodium hexatitanate whisker of raw material and preparation method thereof.Described in the present embodiment the step of preparation method
It is：
The first step, titaniferous waste material is heat-treated 2 ~ 4 hours under the conditions of 1000 ~ 1300 DEG C, then grinding to granularity is less than
0.045mm, obtain grinding material A.
Second step, grinding material A, 10 ~ 20wt% titanium dioxide and the 20 ~ 30wt% thermosetting resin by 50 ~ 60wt%
It is well mixed, it is compressing under the conditions of 50 ~ 100MPa, 1 ~ 3 is heat-treated under the conditions of 1200 ~ 1400 DEG C and in neutral atmosphere
Hour, crush, grinding to granularity is less than 0.088mm, obtains grinding material B.
3rd step, the grinding material B, 20 ~ 30wt% natrium carbonicum calcinatum and 20 ~ 30wt% three water second by 40 ~ 50wt%
Sour sodium is well mixed, and is ground 0.5 ~ 1 hour；Then it is heat-treated 1 ~ 3 hour under the conditions of 400 ~ 600 DEG C, then at 800 ~ 1000 DEG C
Under the conditions of be heat-treated 1 ~ 3 hour, grinding to granularity is less than 0.088mm, and sodium hexatitanate whisker using titaniferous waste material as raw material is made.
The neutral atmosphere is nitrogen atmosphere.
It is manufactured in the present embodiment using titaniferous waste material as raw material sodium hexatitanate whisker after testing：A diameter of 0.5 ~ 1.5 μm；It is long
Spend for 3 ~ 20 μm；Whisker size is uniform, and crystallinity is high.
Embodiment 2
It is a kind of using titaniferous waste material as sodium hexatitanate whisker of raw material and preparation method thereof.Described in the present embodiment the step of preparation method
It is：
The first step, titaniferous waste material is heat-treated 2 ~ 4 hours under the conditions of 1000 ~ 1300 DEG C, then grinding to granularity is less than
0.045mm, obtain grinding material A.
Second step, grinding material A, 10 ~ 20wt% titanium dioxide and the 10 ~ 20wt% thermosetting resin by 60 ~ 70wt%
It is well mixed, it is compressing under the conditions of 50 ~ 100MPa, 1 ~ 3 is heat-treated under the conditions of 1200 ~ 1400 DEG C and in neutral atmosphere
Hour, crush, grinding to granularity is less than 0.088mm, obtains grinding material B.
3rd step, the grinding material B, 10 ~ 20wt% natrium carbonicum calcinatum and 20 ~ 30wt% three water second by 50 ~ 60wt%
Sour sodium is well mixed, and is ground 0.5 ~ 1 hour；Then it is heat-treated 1 ~ 3 hour under the conditions of 400 ~ 600 DEG C, then at 800 ~ 1000 DEG C
Under the conditions of be heat-treated 1 ~ 3 hour, grinding to granularity is less than 0.088mm, and sodium hexatitanate whisker using titaniferous waste material as raw material is made.
The neutral atmosphere is argon gas atmosphere.
It is manufactured in the present embodiment using titaniferous waste material as raw material sodium hexatitanate whisker after testing：A diameter of 0.5 ~ 1.5 μm；It is long
Spend for 5 ~ 20 μm；Whisker size is uniform, and crystallinity is high.
Embodiment 3
It is a kind of using titaniferous waste material as sodium hexatitanate whisker of raw material and preparation method thereof.Described in the present embodiment the step of preparation method
It is：
The first step, titaniferous waste material is heat-treated 2 ~ 4 hours under the conditions of 1000 ~ 1300 DEG C, then grinding to granularity is less than
0.045mm, obtain grinding material A.
Second step, grinding material A, 10 ~ 20wt% titanium dioxide and the 20 ~ 30wt% thermosetting resin by 50 ~ 60wt%
It is well mixed, it is compressing under the conditions of 50 ~ 100MPa, 1 ~ 3 is heat-treated under the conditions of 1200 ~ 1400 DEG C and in neutral atmosphere
Hour, crush, grinding to granularity is less than 0.088mm, obtains grinding material B.
3rd step, the grinding material B, 20 ~ 30wt% natrium carbonicum calcinatum and 10 ~ 20wt% three water second by 50 ~ 60wt%
Sour sodium is well mixed, and is ground 0.5 ~ 1 hour；Then it is heat-treated 1 ~ 3 hour under the conditions of 400 ~ 600 DEG C, then at 800 ~ 1000 DEG C
Under the conditions of be heat-treated 1 ~ 3 hour, grinding to granularity is less than 0.088mm, and sodium hexatitanate whisker using titaniferous waste material as raw material is made.
The neutral atmosphere is argon gas atmosphere.
It is manufactured in the present embodiment using titaniferous waste material as raw material sodium hexatitanate whisker after testing：A diameter of 0.5 ~ 1.5 μm；It is long
Spend for 8 ~ 20 μm；Whisker size is uniform, and crystallinity is high.
Embodiment 4
It is a kind of using titaniferous waste material as sodium hexatitanate whisker of raw material and preparation method thereof.Described in the present embodiment the step of preparation method
It is：
The first step, titaniferous waste material is heat-treated 2 ~ 4 hours under the conditions of 1000 ~ 1300 DEG C, then grinding to granularity is less than
0.045mm, obtain grinding material A.
Second step, grinding material A, 10 ~ 20wt% titanium dioxide and the 10 ~ 20wt% thermosetting resin by 60 ~ 70wt%
It is well mixed, it is compressing under the conditions of 50 ~ 100MPa, 1 ~ 3 is heat-treated under the conditions of 1200 ~ 1400 DEG C and in neutral atmosphere
Hour, crush, grinding to granularity is less than 0.088mm, obtains grinding material B.
3rd step, the grinding material B, 20 ~ 30wt% natrium carbonicum calcinatum and 20 ~ 30wt% three water second by 40 ~ 50wt%
Sour sodium is well mixed, and is ground 0.5 ~ 1 hour；Then it is heat-treated 1 ~ 3 hour under the conditions of 400 ~ 600 DEG C, then at 800 ~ 1000 DEG C
Under the conditions of be heat-treated 1 ~ 3 hour, grinding to granularity is less than 0.088mm, and sodium hexatitanate whisker using titaniferous waste material as raw material is made.
The neutral atmosphere is nitrogen atmosphere.
It is manufactured in the present embodiment using titaniferous waste material as raw material sodium hexatitanate whisker after testing：A diameter of 1 ~ 2 μm；Length is
8~20μm；Whisker size is uniform, and crystallinity is high.
Present embodiment has following good effect compared with prior art：
(1) present embodiment accompanies on the Research foundations such as temperature evolution to the composition of titaniferous waste material, structure and its thing, will
The preparation process substep of product controls：Feedstock property regulation, formation interphase and whisker grow.Pass through considered critical raw material
Granularity and the preparation process such as the granularity of intermediate product, treatment temperature, processing time, atmosphere technical parameter, be sodium hexatitanate
The formation of whisker provides necessary requirement with growing up, and makes the prepared crystallization using titaniferous waste material as the sodium hexatitanate whisker of raw material
Degree height and size uniform.
(2) present embodiment is using titaniferous waste material as primary raw material, then is equipped with titanium dioxide, thermosetting resin and anhydrous carbon
The common raw material of the industry such as sour sodium, preparation process substep is controlled, energy consumption and loss of material caused by both having reduced high-temperature process,
Accurate adjustment has been carried out to whisker different growth phases again, has realized the equal of properties of product, preparation process energy consumption and Material Cost
Weighing apparatus control.Therefore, not only used raw material sources are extensive, and simple production process and production cost are low.
Present embodiment prepare using titaniferous waste material as raw material sodium hexatitanate whisker after testing：A diameter of 0.5 ~ 2 μ
m；Length is 3 ~ 20 μm；Whisker size is uniform, and crystallinity is high.
Therefore, present embodiment production cost is low and technique is simple, it is prepared using titaniferous waste material as raw material six
The crystallinity height and size uniform of sodium titanate crystal whisker.
Claims (6)
1. a kind of preparation method using titaniferous waste material as the sodium hexatitanate whisker of raw material, it is characterised in that the preparation method is：
The first step, titaniferous waste material is heat-treated 2 ~ 4 hours under the conditions of 1000 ~ 1300 DEG C, then grinding to granularity is less than
0.045mm, obtain grinding material A；
Second step, the 50 ~ 70wt% grinding material A, 10 ~ 20wt% titanium dioxide and 10 ~ 30wt% thermosetting resin are mixed
Uniformly, compressing under the conditions of 50 ~ 100MPa, heat treatment 1 ~ 3 is small under the conditions of 1200 ~ 1400 DEG C and in neutral atmosphere
When, crush, grinding to granularity is less than 0.088mm, obtains grinding material B；
3rd step, by 40 ~ 60wt% grinding material B, 10 ~ 30wt% natrium carbonicum calcinatum and the 10 ~ 30wt% sodium acetate trihydrate
It is well mixed, grind 0.5 ~ 1 hour；Then it is heat-treated 1 ~ 3 hour under the conditions of 400 ~ 600 DEG C, then at 800 ~ 1000 DEG C of conditions
Lower heat treatment 1 ~ 3 hour, grinding to granularity is less than 0.088mm, and the sodium hexatitanate whisker using titaniferous waste material as raw material is made.
2. the preparation method using titaniferous waste material as the sodium hexatitanate whisker of raw material according to claim 1, it is characterised in that institute
State titaniferous waste material：Ti contents are more than 52wt%, and Al, Ni, V, Co, Cr, Ca and Si content summation are less than 0.9wt%；Titaniferous waste material
Granularity be less than 0.088mm.
3. the preparation method using titaniferous waste material as the sodium hexatitanate whisker of raw material according to claim 1, it is characterised in that institute
The granularity for stating titanium dioxide is less than 0.088mm；TiO in the titanium dioxide2Content be more than 99wt%.
4. the preparation method using titaniferous waste material as the sodium hexatitanate whisker of raw material according to claim 1, it is characterised in that institute
Neutral atmosphere is stated to be nitrogen atmosphere or be argon gas atmosphere.
5. the preparation method using titaniferous waste material as the sodium hexatitanate whisker of raw material according to claim 1, it is characterised in that institute
The granularity for stating natrium carbonicum calcinatum is less than 0.088mm；Na in the natrium carbonicum calcinatum2CO3Content be more than 99wt%.
A kind of 6. sodium hexatitanate whisker using titaniferous waste material as raw material, it is characterised in that six titaniums using titaniferous waste material as raw material
Sour sodium whisker is the preparation side using titaniferous waste material as the sodium hexatitanate whisker of raw material according to any one of claim 1 ~ 5
The sodium hexatitanate whisker using titaniferous waste material as raw material prepared by method.
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| CN201711145652.4A CN107858755A (en) | 2017-11-17 | 2017-11-17 | Using titaniferous waste material as sodium hexatitanate whisker of raw material and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101363136A (en) * | 2007-08-10 | 2009-02-11 | 上海晶须复合材料制造有限公司 | Synthesis method of sodium hexatitanate whisker |
| CN103342571A (en) * | 2013-07-10 | 2013-10-09 | 武汉理工大学 | Preparation method of potassium hexatitanate whisker heat insulation and heat preservation material |
| CN103693938A (en) * | 2013-12-23 | 2014-04-02 | 中国建筑材料科学研究总院 | Nano silicon oxide heat-insulating material with radiation shield layer and preparation method thereof |
| CN104947176A (en) * | 2015-06-23 | 2015-09-30 | 武汉科技大学 | Hollow structure potassium magnesium titanate whisker material and method for preparing the same |
-
2017
- 2017-11-17 CN CN201711145652.4A patent/CN107858755A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101363136A (en) * | 2007-08-10 | 2009-02-11 | 上海晶须复合材料制造有限公司 | Synthesis method of sodium hexatitanate whisker |
| CN103342571A (en) * | 2013-07-10 | 2013-10-09 | 武汉理工大学 | Preparation method of potassium hexatitanate whisker heat insulation and heat preservation material |
| CN103693938A (en) * | 2013-12-23 | 2014-04-02 | 中国建筑材料科学研究总院 | Nano silicon oxide heat-insulating material with radiation shield layer and preparation method thereof |
| CN104947176A (en) * | 2015-06-23 | 2015-09-30 | 武汉科技大学 | Hollow structure potassium magnesium titanate whisker material and method for preparing the same |
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Application publication date: 20180330 |