CN109928422A - A kind of method that fused salt prepares potassium titanate crystal - Google Patents
A kind of method that fused salt prepares potassium titanate crystal Download PDFInfo
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- CN109928422A CN109928422A CN201810919847.8A CN201810919847A CN109928422A CN 109928422 A CN109928422 A CN 109928422A CN 201810919847 A CN201810919847 A CN 201810919847A CN 109928422 A CN109928422 A CN 109928422A
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- potassium titanate
- fused salt
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Abstract
The invention discloses a kind of methods that fused salt prepares potassium titanate crystal, using titanium dioxide as raw material.Molten salt system selects sodium chloride, potassium chloride, sodium fluoride ternary system, and after being warming up to 800 DEG C, constant temperature 4h is sufficiently reacted, is cooled to room temperature after the reaction was completed, cleaned with hot distilled water, potassium titanate can be obtained.The direct step of the method for the present invention produces potassium titanate, simplifies production process, reduces energy consumption, helps to improve potassium titanate production efficiency.
Description
Technical field
The invention belongs to high temperature resistant precise materials technical fields, and in particular to a kind of fused salt prepares the side of potassium titanate crystal
Method.
Background technique
Potassium titanate has good electric conductivity, heat resistance and wear resistance, can be used for metal material composite lifting performance
Make brake block, high temperature resistant precise materials, it can also be used to make welding rod, application is very extensive.The main production of existing potassium titanate
Mode includes: hydro-thermal method, fusion method, solution method, flux method, chilling sintering crystallisation, slow cooling sintering crystallisation and KDC
Method.
The prior art generally uses potassium hydroxide and titanium dioxide or potassium carbonate and titanium dioxide is that raw material produces potassium titanate,
Sintering process is to react two kinds of raw materials between 600 DEG C to 1200 DEG C, but technique is coarse, and production effect is bad；KDC method is
It improves and is formed on the basis of sintering process, after raw material is slurried sintering generates metatitanic acid under the conditions of 1000 DEG C to 1200 DEG C again
Potassium；Fusion method is that quenching prepares potassium titanate after two kinds of materials to be heated to melting.Fusion method, solution method, chilling sintering crystallisation,
The product quality that slow cooling sintering crystallisation and KDC method are produced is preferable, but reaction temperature is higher, and energy consumption is larger, is unfavorable for
Energy-saving and emission-reduction；Cosolvent rule is that the cosolvents such as potassium permanganate are added in the feed, reduces preparation temperature.Flux method production
Potassium titanate product quality is preferable, but cosolvent price is higher, economical difference, and large-scale industrial production is limited；Hydro-thermal method is
The conditions such as comprehensively control reaction time, pressure, temperature, pH value generate potassium titanate in a high pressure reaction kettle, and process is relatively complicated.Water
Although thermal method is more energy saving, governing factor is more in production process, is unfavorable for industrialized production, while meeting in production process
PH value is constantly regulate, causes largely to waste.Also make cost increase in production process simultaneously.
Summary of the invention
The purpose of the present invention is intended to provide a kind of method that fused salt prepares potassium titanate crystal.
The present invention is realized especially by following technical scheme:
A kind of method that fused salt prepares potassium titanate crystal, comprising the following steps:
1) in proportion by NaCl, KCl, NaF and TiO2It is sufficiently mixed uniformly, is placed in vacuum oven and removes moisture removal；
2) it will be placed in heat up in resistance furnace by dry mix reagent and heat, make TiO2Dissolution equilibrium shape can be reached
State；
3) it is cooled to room temperature, is cleaned with hot distilled water after the reaction was completed, potassium titanate can be obtained.
Further, NaCl, KCl, NaF and TiO in the step (1)2Molar ratio be 2:2.5:2.5:1.
Further, vacuum drying condition in the step (1) are as follows: dried for 24 hours at a temperature of 473K.
Further, mix reagent be heated to after in-furnace temperature is 800 DEG C in the step (2), it is permanent
Warm 4h.
It is calculated by thermodynamic software HSC6.0, at 500 DEG C, reaction spontaneous can be carried out, and generate potassium fluotitanate and titanium
Sour potassium.For guarantee melting salt system be completely dissolved, in fused salt reaction process, temperature of molten salt be 800 DEG C, the time be 0.5~
1.5h。
The invention has the benefit that
The present invention can a direct step produce potassium titanate, avoid extremely cold process after first sintering, it is difficult to reduce production technology
It spends, while temperature control reduces energy consumption compared to conventional method at 800 DEG C, when can adjust heat preservation according to product requirement difference
Between etc., reach different production requirements.Potassium titanate production efficiency is helped to improve, production process is simplified, reduces energy consumption,
Acid or alkali dangerous goods are not used in the process, and it is environmentally protective to contain only potassium fluotitanate, potassium titanate and sodium chloride in product.This
Outside, the salt in molten salt system is that relatively conventional salt is safer, and cost is relatively low for raw materials for production.
Detailed description of the invention
Fig. 1 is the XRD detection figure that potassium titanate crystal is prepared in the embodiment of the present invention.
Specific embodiment
Below in conjunction with specific embodiment of the present invention, technical solution of the present invention is clearly and completely described, is shown
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Molten-salt growth method prepares potassium titanate, using titanium dioxide as raw material.Molten salt system selects sodium chloride, potassium chloride, sodium fluoride three
First system, i.e. NaCl-KCl-NaF-TiO2, can guarantee to have compared with low melting point using the NaCl-KCl system of equimolar ratio；Its
Secondary addition NaF is more advantageous to TiO2Dissolution.
The molar ratio of described NaCl, KCl, NaF and TiO2 are 2:2.5:2.5:1.
In proportion by NaCl, KCl, NaF and TiO2Corundum crucible is poured into after being sufficiently mixed uniformly, is put into resistance furnace and adds
Fused salt when in-furnace temperature reaches 800 DEG C, then is kept the temperature 4h by heat, is made containing TiO2Dissolution equilibrium state can be reached.By thermodynamics
Software HSC6.0 is calculated, and at 500 DEG C, reaction spontaneous can be carried out, and generates potassium fluotitanate and potassium titanate.
Explanation is further explained to the technology of the present invention below with reference to specific preparation process.
After analytically pure NaCl, analytically pure KCl, analytically pure NaF and titanium dioxide are ground refinement with agate mortar,
It is placed in vacuum oven and dries at a temperature of 473K for 24 hours to remove residual moisture in reagent, be then sealed stand-by.
By 35.0941g NaCl, 55.9605g KCl, 31.5195g NaF and 23.9696g TiO2It is sufficiently mixed uniformly
After pour into corundum crucible, be then placed in heating in resistance, when stove displays temperature reaches 400 DEG C of set temperature, chemical reaction
Start spontaneous progress, resistance furnace is warming up to 800 DEG C, so that raw material is in complete molten condition, then fused salt is kept the temperature 4h, make TiO2
It is reacted completely with NaF and KCl.
It is cooled to room temperature after fully reacting, it, can be clear by product hot distilled water since sodium chloride is water-soluble in product
It washes, salt and potassium fluotitanate is all washed away, then filter out potassium titanate.
The whole logical argon gas protection of experiment, argon gas first pass through the gas destilling tower equipped with discoloration silica gel before being passed through in furnace,
Argon gas is dried.Argon gas is passed through by the argon inlet mouth of furnace bottom, is discharged by the gas outlet of furnace roof, outlet, which is passed through, fills hydrogen
The solution of sodium oxide molybdena is discharged into environment after going out purification.The bell that stove is respectively provided with stainless steel up and down guarantees the air-tightness of stove,
Bell is oxidized in the high temperature environment in order to prevent, and the cooling of cycle water is passed through in bell, extends the service life of bell.
XRD detection is carried out to fused salt product as shown in Figure 1, (Rigaku, Ultima IV) is it can be seen from the figure that have
Novel substance potassium titanate generates.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (4)
1. a kind of method that fused salt prepares potassium titanate crystal, which comprises the following steps:
1) in proportion by NaCl, KCl, NaF and TiO2It is sufficiently mixed uniformly, is placed in vacuum oven and removes moisture removal；
2) it will be placed in heat up in resistance furnace by dry mix reagent and heat, make TiO2Dissolution equilibrium state can be reached；
3) it is cooled to room temperature, is cleaned with hot distilled water after the reaction was completed, potassium titanate can be obtained.
2. the method that a kind of fused salt according to claim 1 prepares potassium titanate crystal, which is characterized in that the step
(1) NaCl, KCl, NaF and TiO in2Molar ratio be 2:2.5:2.5:1.
3. the method that a kind of fused salt according to claim 1 prepares potassium titanate crystal, which is characterized in that the step
(1) vacuum drying condition in are as follows: dried for 24 hours at a temperature of 473K.
4. the method that a kind of fused salt according to claim 1 prepares potassium titanate crystal, which is characterized in that the step
(2) mix reagent be heated to after in-furnace temperature is 800 DEG C in, constant temperature 4h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113264551A (en) * | 2021-05-19 | 2021-08-17 | 句容亿格纳米材料厂 | Preparation method of potassium titanate and application of potassium titanate in welding electrode |
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