CN107311223A - A kind of sheet magnesium titanate potassium and preparation method thereof - Google Patents
A kind of sheet magnesium titanate potassium and preparation method thereof Download PDFInfo
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- CN107311223A CN107311223A CN201710445477.4A CN201710445477A CN107311223A CN 107311223 A CN107311223 A CN 107311223A CN 201710445477 A CN201710445477 A CN 201710445477A CN 107311223 A CN107311223 A CN 107311223A
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- magnesium titanate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention discloses a kind of sheet magnesium titanate potassium and preparation method thereof, and specific preparation process is as follows：Take titanium dioxide, potassium carbonate, the magnesium hydroxide hybrid reaction in V-type batch mixer；Compound is put into sintering reaction in sintering furnace；After thing cooling to be sintered, it is placed in soaking and stirring in acetum and disperses；After gained mixture is filtered, gained solid is placed in water agitator treating；After gained mixture is filtered, gained solid is dried in drying machine, milling obtains sheet magnesium titanate potassium.Magnesium titanate potassium purity prepared by the inventive method is higher, and allows raw material to serve as fluxing agent by controlling material rate and technique in preparation process, all raw materials is involved in reaction, and the purity of finished product is high, saves production cost.
Description
Technical field
The invention belongs to magnesium titanate potassium field of material technology, and in particular to a kind of sheet magnesium titanate potassium and preparation method thereof.
Background technology
Magnesium titanate potassium is a kind of novel high-performance inorganic material, causes special structure to assign its unique physical chemistry special
Property, it can be used as friction material, reinforcing material, ion exchange material, catalytic carrier and heat-insulating material etc., with wide
Application prospect.As friction material of new generation, use of the magnesium titanate potassium in brake block can not only greatly improve brake
Can, and brake noise, the service life for significantly improving feel when touching on the brake, greatly improving brake block etc. can be reduced.
Ceramic brake containing magnesium titanate potassium is widely used abroad, and a popularization raised bench is also at present in China
Section, but too high production cost governs large-scale promotion application of the magnesium titanate potassium in China market for a long time.
Existing magnesium titanate potassium preparation method is generally flux growth metrhod, i.e., add fluxing agent in the feed and help crystal life
Long, fluxing agent is in certain circumstances typically liquid, and the best growing environment of crystal is liquid phase environment, but in flux growth metrhod
Fluxing agent be not involved in reaction, be finally still to remove, complex process, thereby increases and it is possible to have a fluxing agent residual, industrial production cost is high.
CN201510348036.3 discloses a kind of hollow-core construction magnesium titanate potassium crystal whisker materials and preparation method thereof.Its technical side
Case is：Mixed by titaniferous materials, containing magnesium raw material and bonding agent, shaping is ground after heat treatment, it is 0.088~1mm's to obtain granularity
A materials and granularity are less than 0.088mm B materials；Potassium raw material, titaniferous materials and bonding agent will be contained again to mix, shaping, after heat treatment
Grinding, obtains the C materials that granularity is less than 0.088mm；Then A materials, B materials, C materials and raw material containing potassium are mixed, heat treatment
Grinding, obtains grinding material afterwards；Additional C materials, raw material containing potassium and water in the most backward grinding material, stirring are pressed into base substrate, will
Body drying, washes after heat treatment, filters, dry, hollow-core construction magnesium titanate potassium crystal whisker materials are made.The technical scheme is not right
Fluxing agent or bonding agent residue problem propose corresponding processing mode.
CN201110161396.4 discloses a kind of method that direct utilization magnesia prepares magnesium titanate, belongs to inorganic material
Expect preparing technical field.This method is mainly characterized by：Directly using magnesia, titanium-containing compound and potassium carbonate as raw material, mix
Close it is uniform after, by mixture at 900~1300 DEG C high-temperature calcination 30 minutes~24 hours, one-step synthesis prepares magnesium titanate
(K2MgTi4O10, i.e.,：K2O·MgO·4TiO2), the magnesium titanate that is obtained after calcining is size-reduced to can obtain finished product.This method is deposited
In following problem：The raw material reaction of the technical scheme is not complete enough, and be milled obtained finished product residual part material after direct sintering；
Corrosion is serious because of caustic corrosion for mould, pollutes raw material；And the platelet magnesium titanate shape obtained is not regular enough, lack of homogeneity, tool
There is certain limitation.
CN 201610825274.3 discloses a kind of synthetic method that magnesium titanate platelet is synthesized by sheet-shaped material, will contain
Titanium material, raw material containing potassium and material by wet type mixing is carried out in aqueous containing magnesium raw material；Water soluble emulsifier is added simultaneously, and mixing is equal
It is even；Into Rollingscratchboarddrier, well mixed sheet-shaped material is obtained；Sheet-shaped material is in high temperature furnace, with 1~2 DEG C/min
Heating rate, be warming up to 900~1100 DEG C, stop 3~6 hours, natural cooling；Classification is crushed in impact grinding, that is, is obtained
Finished product.Residual fraction water soluble emulsifier in finished product prepared by the program, with certain limitation.
The content of the invention
In view of the shortcomings of the prior art, it is contemplated that disclosing a kind of sheet magnesium titanate potassium and preparation method thereof, the party is used
Magnesium titanate potassium purity prepared by method is higher, and allows raw material to serve as fluxing by controlling material rate and technique in preparation process
Agent, makes all raw materials be involved in reaction, saves production cost.
To achieve the above object, the technical solution adopted by the present invention is as follows：
On the one hand, the present invention provides a kind of preparation method of sheet magnesium titanate potassium, comprises the following steps that：
Step one：Take titanium dioxide, potassium carbonate, the magnesium hydroxide hybrid reaction in V-type batch mixer；
Step 2：Step one gained compound is put into sintering reaction in sintering furnace；
Step 3：Disperse after after sinter cooling in step 2, being placed in soaking and stirring in acetum；
Step 4：After mixture filtering obtained by step 3, gained solid is placed in water agitator treating；
Step 5：After mixture filtering obtained by step 4, gained solid is dried in drying machine, milling obtains sheet titanium
Sour magnesium potassium.
Further, the present invention is provided in a kind of preparation method of sheet magnesium titanate potassium, step one, the titanium dioxide,
Potassium carbonate, the mass ratio of magnesium hydroxide are 60~65%：25~30%：5~15%.
Further, the present invention is provided in a kind of preparation method of sheet magnesium titanate potassium, step one, the hybrid reaction
Time is 2~4 hours, preferably 2 hours.
Further, the present invention is provided in a kind of preparation method of sheet magnesium titanate potassium, step 2, the sintering reaction
Temperature is 1000~1500 DEG C, and the time of sintering reaction is 1~10 hour.It is further preferred that the temperature of sintering reaction is
1050~1350 DEG C, the time of sintering reaction is 5 hours.
Further, the present invention is provided in a kind of preparation method of sheet magnesium titanate potassium, step 3, the soaking and stirring point
The scattered time is 0.5~2 hour, further, it is preferable to be 1h.
Further, the present invention is provided in a kind of preparation method of sheet magnesium titanate potassium, step 4, and stirring is washed in the water
The time washed is 0.5~2 hour, further, it is preferable to be 1h.
Further, the present invention is provided in a kind of preparation method of sheet magnesium titanate potassium, step 5, the temperature of the drying
For 150~250 DEG C, the granularity of the products obtained therefrom of milling is 200 mesh.Further, it is preferable to which the temperature of drying is 200 DEG C.
On the other hand, the present invention provides a kind of sheet magnesium titanate potassium prepared by method of the present invention.
Beneficial effect：
The present invention provides a kind of sheet magnesium titanate potassium and preparation method thereof, and its technique is simple, raw material type is few, raw material is easy
, gained sheet magnesium titanate potassium yield is high, good dispersion, and crystallinity is high, and pattern is uniform, and technique is adapted to industrialized production.
Products obtained therefrom is the flat crystal of about 20 μm of average diameter, without other fluxing agent impurity, and purity is high, and size is equal
It is even.
Relatively disclosed patent CN201110161396.4, sheet magnesium titanate potassium purity prepared by the present invention is higher, finally
The crystal growth of sintering is complete.
Relatively disclosed patent CN201610825274.3, the preparation method that the present invention is provided is simpler, and purity is higher.
Figure of description
Fig. 1 schemes (30 μm) for the SEM of sheet magnesium titanate potassium of the embodiment of the present invention.
Fig. 2 schemes (10 μm) for the SEM of sheet magnesium titanate potassium of the embodiment of the present invention.
Fig. 3 is the XRD of sheet magnesium titanate potassium of the embodiment of the present invention.
Embodiment
With reference to embodiment, the invention will be further described, not to the limitation of its protection domain.
Embodiment 1
A kind of preparation method of sheet magnesium titanate potassium, is comprised the following steps that：
Step one：Take titanium dioxide, potassium carbonate, magnesium hydroxide hybrid reaction 2 hours in V-type batch mixer, the dioxy
It is 60% to change titanium, potassium carbonate, the mass ratio of magnesium hydroxide：30%：10%；
Step 2：Step one gained compound is put into sintering reaction in sintering furnace；, the temperature of the sintering reaction is
1050 DEG C, the time of sintering reaction is 5 hours；
Step 3：Disperse 1h after after sinter cooling in step 2, being placed in soaking and stirring in acetum；
Step 4：After mixture filtering obtained by step 3, gained solid is placed in water agitator treating 1h；
Step 5：After mixture filtering obtained by step 4, gained solid is dried in drying machine, milling obtains sheet titanium
Sour magnesium potassium；The temperature of the drying is 200 DEG C, and the granularity of the products obtained therefrom of milling is 200 mesh.
Embodiment 2
A kind of preparation method of sheet magnesium titanate potassium, is comprised the following steps that：
Step one：Take titanium dioxide, potassium carbonate, magnesium hydroxide hybrid reaction 4 hours in V-type batch mixer, the dioxy
It is 65% to change titanium, potassium carbonate, the mass ratio of magnesium hydroxide：25%：10%；
Step 2：Step one gained compound is put into sintering reaction in sintering furnace；The temperature of the sintering reaction is
1000~1050 DEG C, the time of sintering reaction is 10 hours；
Step 3：After after sinter cooling in step 2, soaking and stirring in acetum is placed in scattered 2 hours；
Step 4：After mixture filtering obtained by step 3, gained solid is placed in water agitator treating 2 hours,
Step 5：After mixture filtering obtained by step 4, gained solid is dried in drying machine, milling obtains sheet titanium
Sour magnesium potassium；The temperature of the drying is 150 DEG C, and the granularity of the products obtained therefrom of milling is 200 mesh.
Embodiment 3
A kind of preparation method of sheet magnesium titanate potassium, is comprised the following steps that：
Step one：Take titanium dioxide, potassium carbonate, magnesium hydroxide hybrid reaction 3 hours in V-type batch mixer, the dioxy
It is 60% to change titanium, potassium carbonate, the mass ratio of magnesium hydroxide：25%：15%；
Step 2：Step one gained compound is put into sintering reaction in sintering furnace；The temperature of the sintering reaction is
1350~1500 DEG C, the time of sintering reaction is 1 hour；
Step 3：Disperse after after sinter cooling in step 2, being placed in soaking and stirring in acetum；The soaking and stirring
The scattered time is 0.5 hour；
Step 4：After mixture filtering obtained by step 3, gained solid is placed in water agitator treating；Stirred in the water
The time of washing is 0.5 hour；
Step 5：After mixture filtering obtained by step 4, gained solid is dried in drying machine, milling obtains sheet titanium
Sour magnesium potassium；The temperature of the drying is 250 DEG C, and the granularity of the products obtained therefrom of milling is 200 mesh.
Embodiment 4
A kind of preparation method of sheet magnesium titanate potassium, is comprised the following steps that：
Step one：Take titanium dioxide, potassium carbonate, magnesium hydroxide hybrid reaction 2 hours in V-type batch mixer, the dioxy
It is 65% to change titanium, potassium carbonate, the mass ratio of magnesium hydroxide：30%：5%；
Step 2：Step one gained compound is put into sintering reaction in sintering furnace；, the temperature of the sintering reaction is
1050~1350 DEG C, the time of sintering reaction is 5 hours；
Step 3：After after sinter cooling in step 2, soaking and stirring in acetum is placed in scattered 1 hour；
Step 4：After mixture filtering obtained by step 3, gained solid is placed in water agitator treating 1 hour；
Step 5：After mixture filtering obtained by step 4, gained solid is dried in drying machine, milling obtains sheet titanium
Sour magnesium potassium；The temperature of the drying is 200 DEG C, and the granularity of the products obtained therefrom of milling is 200 mesh.
Embodiment 5
A kind of preparation method of sheet magnesium titanate potassium, is comprised the following steps that：
Step one：Take titanium dioxide, potassium carbonate, magnesium hydroxide hybrid reaction 2 hours in V-type batch mixer, the dioxy
It is 60% to change titanium, potassium carbonate, the mass ratio of magnesium hydroxide：30%：10%；
Step 2：Step one gained compound is put into sintering reaction in sintering furnace；, the temperature of the sintering reaction is
1050~1350 DEG C, the time of sintering reaction is 10 hours；
Step 3：After after sinter cooling in step 2, soaking and stirring in acetum is placed in scattered 1 hour；
Step 4：After mixture filtering obtained by step 3, gained solid is placed in water agitator treating 1 hour；
Step 5：After mixture filtering obtained by step 4, gained solid is dried in drying machine, milling obtains sheet titanium
Sour magnesium potassium；The temperature of the drying is 200 DEG C, and the granularity of the products obtained therefrom of milling is 200 mesh.
Sheet magnesium titanate potassium prepared by the present invention is by the strict temperature and washing process that control each step, both beneficial to each
Close contact and reaction between feed particles, also beneficial to the growth and development of flat crystal, are directly served as using raw material and helped
Flux, all materials both participate in reaction, not only reduce the removal step of impurity that fluxing agent is brought, also ensure product purity and
Technique it is simple.
Sheet magnesium titanate potassium crystalline material prepared by the method for the present invention is by detection, XRD as shown in figure 3, specific brilliant
The parameter of body is as follows：Crystal average diameter is about 25 μm, and thick 1~5 μm, purity is 99.9%；Piece prepared by the method for the present invention
The SEM of shape magnesium titanate potassium is schemed as shown in Fig. 1~2.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (10)
1. a kind of preparation method of sheet magnesium titanate potassium, it is characterised in that comprise the following steps that：
Step one：Take titanium dioxide, potassium carbonate, the magnesium hydroxide hybrid reaction in V-type batch mixer；
Step 2：Step one gained compound is put into sintering reaction in sintering furnace；
Step 3：Disperse after after sinter cooling in step 2, being placed in soaking and stirring in acetum；
Step 4：After mixture filtering obtained by step 3, gained solid is placed in water agitator treating；
Step 5：After mixture filtering obtained by step 4, gained solid is dried in drying machine, milling obtains sheet magnesium titanate
Potassium.
2. the preparation method of sheet magnesium titanate potassium according to claim 1, it is characterised in that in step one, the dioxy
It is 60~65% to change titanium, potassium carbonate, the mass ratio of magnesium hydroxide：25~30%：5~15%.
3. the preparation method of sheet magnesium titanate potassium according to claim 1, it is characterised in that in step one, the mixing
The time of reaction is 2~4 hours.
4. the preparation method of sheet magnesium titanate potassium according to claim 1, it is characterised in that in step 2, the sintering
The temperature of reaction is 1000~1500 DEG C, and the time of sintering reaction is 1~10 hour.
5. the preparation method of sheet magnesium titanate potassium according to claim 4, it is characterised in that the temperature of the sintering reaction
For 1050~1350 DEG C, the time of sintering reaction is 5 hours.
6. the preparation method of sheet magnesium titanate potassium according to claim 1, it is characterised in that in step 3, the immersion
The time of dispersed with stirring is 0.5~2 hour.
7. the preparation method of sheet magnesium titanate potassium according to claim 1, it is characterised in that in step 4, in the water
The time of agitator treating is 0.5~2 hour.
8. the preparation method of sheet magnesium titanate potassium according to claim 1, it is characterised in that in step 5, the drying
Temperature be 150~250 DEG C, the granularity of the products obtained therefrom of milling is 200 mesh.
9. the preparation method of sheet magnesium titanate potassium according to claim 8, it is characterised in that the temperature of the drying is
200℃。
10. sheet magnesium titanate potassium prepared by any described method of claim 1~9.
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| CN201710445477.4A CN107311223B (en) | 2017-06-13 | 2017-06-13 | A kind of sheet magnesium titanate potassium and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115636436A (en) * | 2022-11-03 | 2023-01-24 | 青岛科技大学 | Preparation method of lamellar titanic acid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6677041B1 (en) * | 1999-03-16 | 2004-01-13 | Otsuka Chemical Co., Ltd. | Platy potassium titanate, process for producing the same, and friction material |
-
2017
- 2017-06-13 CN CN201710445477.4A patent/CN107311223B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6677041B1 (en) * | 1999-03-16 | 2004-01-13 | Otsuka Chemical Co., Ltd. | Platy potassium titanate, process for producing the same, and friction material |
Non-Patent Citations (1)
| Title |
|---|
| YAN-NI TAN ET AL.: ""Synthesis of platy potassium magnesium titanate and its application in removal of copper ions from aqueous solution"", 《TRANS. NONFERROUS MET. SOC. CHINA》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115636436A (en) * | 2022-11-03 | 2023-01-24 | 青岛科技大学 | Preparation method of lamellar titanic acid |
| CN115636436B (en) * | 2022-11-03 | 2023-11-10 | 青岛科技大学 | Preparation method of lamellar titanic acid |
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| CN107311223B (en) | 2019-01-22 |
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