CN107815733A - A kind of crystal whisker of hexa potassium titanate based on titaniferous waste material and preparation method thereof - Google Patents
A kind of crystal whisker of hexa potassium titanate based on titaniferous waste material and preparation method thereof Download PDFInfo
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- CN107815733A CN107815733A CN201711147946.0A CN201711147946A CN107815733A CN 107815733 A CN107815733 A CN 107815733A CN 201711147946 A CN201711147946 A CN 201711147946A CN 107815733 A CN107815733 A CN 107815733A
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- waste material
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- titaniferous waste
- potassium titanate
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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
-
- 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
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
-
- 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
Abstract
The present invention relates to a kind of crystal whisker of hexa potassium titanate based on titaniferous waste 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 under the conditions of 1200 ~ 1400 DEG C and in reducing atmosphere.40 ~ 60wt% grinding material B, 10 ~ 30wt% Anhydrous potassium carbonate and 10 ~ 30wt% potassium acetate are mixed, ground 0.5 ~ 1 hour；First it is heat-treated respectively under the conditions of 400 ~ 600 DEG C and 800 ~ 1000 DEG C 1 ~ 3 hour, grinding to granularity is less than 0.088mm, and the crystal whisker of hexa potassium titanate based on titaniferous waste material is made.Present invention process is simple, production cost is low and is produced without secondary slugs, the crystallinity height and size uniform of made product.
Description
Technical field
The invention belongs to crystal whisker of hexa potassium titanate technical field.More particularly to a kind of crystal whisker of hexa potassium titanate based on titaniferous waste material
And preparation method thereof.
Background technology
It is steady to make it have excellent high intensity, high temperature resistant, chemistry with the chain tunnel structure of uniqueness for crystal whisker of hexa potassium titanate
The characteristic such as qualitative, insulating properties and infrared reflectivity height, thus led in heat-barrier material, reinforcing material, friction material, filtering material etc.
It is used widely in domain.Current preparation method mainly has flux growth metrhod, melting-quenching method, combustion method, hydro-thermal method and sintering process
Deng, but all come with some shortcomings.For example, though the whisker draw ratio of flux growth metrhod preparation is big and size is controllable, due to fluxing agent
The impurity of introducing is easily mingled with the product, it is difficult to remove the performance for totally, influenceing whisker.Melting-quenching method needs raw material to pass through
After high-temperature fusion and quenching, then subsequent material pass through into multiple high temp calcination processing, make made from whisker in crystallization process
Easy conglomeration and blocking, energy consumption is big, and production cost is too high.Hydro-thermal method needs HTHP, condition harshness.Sinter rule and crystalline substance be present
The problems such as palpus size is whard to control, whisker separation is difficult.
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, technique is simple and without two
The preparation method of crystal whisker of hexa potassium titanate based on titaniferous waste material caused by secondary waste material, with this method prepare based on titaniferous waste material
The crystallinity height and size uniform of crystal whisker of hexa potassium titanate.
To achieve the above object, the step of the technical solution adopted by the present invention is：
The first step, titaniferous waste material being heat-treated 2 ~ 4 hours under the conditions of 1000 ~ 1300 DEG C, 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, then it is heat-treated 1 under the conditions of 1200 ~ 1400 DEG C and in reducing atmosphere
~ 3 hours, crush, grinding to granularity is less than 0.088mm, obtains grinding material B.
3rd step, grinding material B, 10 ~ 30wt% Anhydrous potassium carbonate and the 10 ~ 30wt% potassium acetate by 40 ~ 60wt%
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 crystal whisker of hexa potassium titanate based on titaniferous waste material is made.
The titaniferous waste material：Ti contents are more than 52wt%, and Al, Ni, V, Co, Cr, Ca, Si content sum are less than 0.9wt%；
The grain graininess 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 reducing atmosphere is hydrogen atmosphere or is carbon monoxide atmosphere.
The granularity of the Anhydrous potassium carbonate is less than 0.088mm；K in the Anhydrous potassium carbonate2CO3Content be more than 99wt%.
The purity of the potassium acetate is more than 99wt%, and the grain graininess of the potassium acetate is less than 0.088mm.
Due to there is following good effect compared with prior art using above-mentioned technical proposal, the present invention：
(1) the present invention is on the basis of the composition of titaniferous waste material, structure and its thing accompany the research such as temperature evolution, by the system of product
Standby process substep controls：The regulation of raw material character, formation interphase and whisker grow.By the granularity of considered critical raw material,
The technical parameter of the preparation process such as granularity, treatment temperature, processing time and the atmosphere of intermediate product, it is the shape of crystal whisker of hexa potassium titanate
Necessary requirement is provided into growing up, thus the crystallinity height and size of the prepared crystal whisker of hexa potassium titanate based on titaniferous waste material
Uniformly.
(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 Anhydrous potassium carbonate
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, production cost are low and are produced without secondary slugs.
Crystal whisker of hexa potassium titanate based on titaniferous waste material prepared by the present invention is after testing：A diameter of 0.5 ~ 2 μm, length is 8 ~ 30
μm；Whisker size is uniform, and crystallinity is high.
Therefore, the present invention has the characteristics of technique is simple, production cost is low and is produced without secondary slugs, it is prepared based on
The crystallinity height and size uniform of the crystal whisker of hexa potassium titanate of titaniferous waste material.
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, Si content sum are less than 0.9wt%；Titaniferous
The grain graininess of 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 Anhydrous potassium carbonate is less than 0.088mm；K in the Anhydrous potassium carbonate2CO3Content be more than 99wt%.
The purity of the potassium acetate is more than 99wt%, and the grain graininess of the potassium acetate is less than 0.088mm.
Embodiment 1
A kind of crystal whisker of hexa potassium titanate based on titaniferous waste material and preparation method thereof.It is the step of preparation method described in the present embodiment：
The first step, titaniferous waste material being heat-treated 2 ~ 4 hours under the conditions of 1000 ~ 1300 DEG C, 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, then it is heat-treated 1 under the conditions of 1200 ~ 1400 DEG C and in reducing atmosphere
~ 3 hours, crush, grinding to granularity is less than 0.088mm, obtains grinding material B.
3rd step, grinding material B, 20 ~ 30wt% Anhydrous potassium carbonate and the 20 ~ 30wt% potassium acetate by 40 ~ 50wt%
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 crystal whisker of hexa potassium titanate based on titaniferous waste material is made.
The reducing atmosphere is hydrogen atmosphere.
Crystal whisker of hexa potassium titanate manufactured in the present embodiment based on titaniferous waste material is after testing：A diameter of 0.5 ~ 1.5 μm, length is
10~30μm；Whisker size is uniform, and crystallinity is high.
Embodiment 2
A kind of crystal whisker of hexa potassium titanate based on titaniferous waste material and preparation method thereof.It is the step of preparation method described in the present embodiment：
The first step, titaniferous waste material being heat-treated 2 ~ 4 hours under the conditions of 1000 ~ 1300 DEG C, 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, then it is heat-treated 1 under the conditions of 1200 ~ 1400 DEG C and in reducing atmosphere
~ 3 hours, crush, grinding to granularity is less than 0.088mm, obtains grinding material B.
3rd step, grinding material B, 10 ~ 20wt% Anhydrous potassium carbonate and the 20 ~ 30wt% potassium acetate by 50 ~ 60wt%
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 crystal whisker of hexa potassium titanate based on titaniferous waste material is made.
The reducing atmosphere is carbon monoxide atmosphere.
Crystal whisker of hexa potassium titanate manufactured in the present embodiment based on titaniferous waste material is after testing：A diameter of 0.5 ~ 1.5 μm, length is
10~25μm；Whisker size is uniform, and crystallinity is high.
Embodiment 3
A kind of crystal whisker of hexa potassium titanate based on titaniferous waste material and preparation method thereof.It is the step of preparation method described in the present embodiment：
The first step, titaniferous waste material being heat-treated 2 ~ 4 hours under the conditions of 1000 ~ 1300 DEG C, 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, then it is heat-treated 1 under the conditions of 1200 ~ 1400 DEG C and in reducing atmosphere
~ 3 hours, crush, grinding to granularity is less than 0.088mm, obtains grinding material B.
3rd step, grinding material B, 20 ~ 30wt% Anhydrous potassium carbonate and the 10 ~ 20wt% potassium acetate by 50 ~ 60wt%
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 crystal whisker of hexa potassium titanate based on titaniferous waste material is made.
The reducing atmosphere is carbon monoxide atmosphere.
Crystal whisker of hexa potassium titanate manufactured in the present embodiment based on titaniferous waste material is after testing：A diameter of 0.5 ~ 1.5 μm, length is
15~30μm；Whisker size is uniform, and crystallinity is high.
Embodiment 4
A kind of crystal whisker of hexa potassium titanate based on titaniferous waste material and preparation method thereof.It is the step of preparation method described in the present embodiment：
The first step, titaniferous waste material being heat-treated 2 ~ 4 hours under the conditions of 1000 ~ 1300 DEG C, 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, then it is heat-treated 1 under the conditions of 1200 ~ 1400 DEG C and in reducing atmosphere
~ 3 hours, crush, grinding to granularity is less than 0.088mm, obtains grinding material B.
3rd step, grinding material B, 20 ~ 30wt% Anhydrous potassium carbonate and the 20 ~ 30wt% potassium acetate by 40 ~ 50wt%
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 crystal whisker of hexa potassium titanate based on titaniferous waste material is made.
The reducing atmosphere is hydrogen atmosphere.
Crystal whisker of hexa potassium titanate manufactured in the present embodiment based on titaniferous waste material is after testing：A diameter of 1 ~ 2 μm, length is 8 ~ 30
μm；Whisker size is uniform, and crystallinity is high.
Present embodiment has following good effect compared with prior art：
(1) present embodiment, will on the Research foundation that the composition of titaniferous waste material, structure and its thing accompany temperature evolution etc.
The preparation process substep of product controls：The regulation of raw material character, formation interphase and whisker grow.Pass through considered critical raw material
The preparation process such as granularity, the granularity of intermediate product, treatment temperature, processing time and atmosphere technical parameter, be potassium hexatitanate
The formation of whisker provides necessary requirement with growing up, thus the crystallinity of the prepared crystal whisker of hexa potassium titanate based on titaniferous waste material
High 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 potassium, 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, production cost are low and without secondary slugs
Produce.
Crystal whisker of hexa potassium titanate based on titaniferous waste material prepared by present embodiment is after testing：It is a diameter of 0.5 ~ 2 μm, long
Spend for 8 ~ 30 μm；Whisker size is uniform, and crystallinity is high.
Therefore, present embodiment has the characteristics of technique is simple, production cost is low and is produced without secondary slugs, made
The crystallinity height and size uniform of the standby crystal whisker of hexa potassium titanate based on titaniferous waste material.
Claims (7)
1. a kind of preparation method of the crystal whisker of hexa potassium titanate based on titaniferous waste material, it is characterised in that the step of the preparation method
It is：
The first step, titaniferous waste material being heat-treated 2 ~ 4 hours under the conditions of 1000 ~ 1300 DEG C, grinding to granularity is less than 0.045mm,
Obtain grinding material A；
Second step, the thermosetting resin mixing by the 50 ~ 70wt% grinding material A, 10 ~ 20wt% titanium dioxide and 10 ~ 30wt%
Uniformly, compressing under the conditions of 50 ~ 100MPa, then heat treatment 1 ~ 3 is small under the conditions of 1200 ~ 1400 DEG C and in reducing atmosphere
When, crush, grinding to granularity is less than 0.088mm, obtains grinding material B；
3rd step, the potassium acetate mixing by the 40 ~ 60wt% grinding material B, 10 ~ 30wt% Anhydrous potassium carbonate and 10 ~ 30wt%
Uniformly, grind 0.5 ~ 1 hour；Then it is heat-treated 1 ~ 3 hour under the conditions of 400 ~ 600 DEG C, it is hot under the conditions of 800 ~ 1000 DEG C
Processing 1 ~ 3 hour, grinding to granularity is less than 0.088mm, and the crystal whisker of hexa potassium titanate based on titaniferous waste material is made.
2. the preparation method of the crystal whisker of hexa potassium titanate according to claim 1 based on titaniferous waste material, it is characterised in that described
Titaniferous waste material：Ti contents are more than 52wt%, and Al, Ni, V, Co, Cr, Ca, Si content sum are less than 0.9wt%；Of titaniferous waste material
Grain granularity is less than 0.088mm.
3. the preparation method of the crystal whisker of hexa potassium titanate according to claim 1 based on titaniferous waste material, it is characterised in that described
The granularity of titanium dioxide is less than 0.088mm；TiO in the titanium dioxide2Content be more than 99wt%.
4. the preparation method of the crystal whisker of hexa potassium titanate according to claim 1 based on titaniferous waste material, it is characterised in that described
Reducing atmosphere is hydrogen atmosphere or is carbon monoxide atmosphere.
5. the preparation method of the crystal whisker of hexa potassium titanate according to claim 1 based on titaniferous waste material, it is characterised in that described
The granularity of Anhydrous potassium carbonate is less than 0.088mm；K in the Anhydrous potassium carbonate2CO3Content be more than 99wt%.
6. the preparation method of the crystal whisker of hexa potassium titanate according to claim 1 based on titaniferous waste material, it is characterised in that described
The purity of potassium acetate is more than 99wt%, and the grain graininess of the potassium acetate is less than 0.088mm.
A kind of 7. crystal whisker of hexa potassium titanate based on titaniferous waste material, it is characterised in that the crystal whisker of hexa potassium titanate based on titaniferous waste material
It is prepared by the preparation method of the crystal whisker of hexa potassium titanate based on titaniferous waste material according to any one of claim 1 ~ 6
Crystal whisker of hexa potassium titanate based on titaniferous waste material.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101694009A (en) * | 2009-10-01 | 2010-04-14 | 中钢集团洛阳耐火材料研究院有限公司 | Method for auxiliary synthesis of potassium titanate crystal whisker by using high-energy ball mill method |
| 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 CN201711147946.0A patent/CN107815733A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101694009A (en) * | 2009-10-01 | 2010-04-14 | 中钢集团洛阳耐火材料研究院有限公司 | Method for auxiliary synthesis of potassium titanate crystal whisker by using high-energy ball mill method |
| 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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