CN104909726B - Microporous ceramic for tungsten refining as well as preparation method and application thereof - Google Patents
Microporous ceramic for tungsten refining as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a microporous ceramic for tungsten refining as well as a preparation method and application thereof. The method comprises the following steps: putting the components of a microporous ceramic formula into a ball milling tank, sealing and performing ball milling to obtain ball-milled powder; adding a mixed solution, and uniformly mixing and stirring into a mud form; performing extrusion moulding in a gypsum mould, and taking out for later use; drying naturally and then drying in an oven, wherein the oven temperature is set at 50-60 DEG C at first, and the temperature is increased by 5-10 DEG C every half hour and gradually rises to a constant temperature of 70-80 DEG C to obtain dried products; tightly wrapping the dried products with kraft paper one by one; and fixing the products on a silicon carbide board, and sintering in a high-temperature electric furnace according to a set thermal regulation process to obtain the microporous ceramic for tungsten refining. According to the invention, the microporous ceramic material is applied to wet-process tungsten refining, a reaction kettle as well as the steps of filtration and separation are saved, sodium tungstate is automatically filtered and separated by an efficient microwave heating technology, and the invention has the advantages of high efficiency, low cost, energy conservation and environmental protection.
Description
Technical field
The present invention relates to a kind of ceramics and preparation method and application, and in particular to a kind of micropore ceramics for refining tungsten and
Its preparation method and application.
Background technology
China is referred to as " tungsten kingdom " by World Mining Industry circle, and tungsten concentrate yield and outlet all occupy first place in the world.China's Chemical analysis
Mostly with tungsten concentrate or tungsten contained material as raw material, using hydrometallurgical processes.Modern wet method refining tungstenio originally all adopts following process
Flow process：Grinding tungsten ore into powder, allow tungsten ore powder and high-concentration sodium hydroxide in reactor react at high temperature under high pressure generate sodium tungstate,
It is separated by filtration Tungstenic Slag and extracts tungstate radicle generation ammonium paratungstate with sodium tungstate, using anion exchange resin.Due to current side
Method must carry out extraction reaction at high temperature under high pressure using reactor, and reactant liquor cooled and filtered again, heat utilization rate are low, corrosion
Seriously, plant maintenance updates relatively costly.
Micropore ceramics are a kind of silicate products, and the raw material for using is barren clay, abandoned mine slag and fly ash in electric power plant, glass
Glass factory leftover bits and pieces etc., this will to environmental protection, economizing on resources plays an important role.And micropore ceramics are a kind of structures of functional type
Ceramics.Micropore ceramics have adsorptivity, breathability, corrosion resistance, Environmental compatibility, biocompatibility etc., are widely used in each
Filtration, the filtration of gas and fixed biology zymophore and the biocompatibility carrier of liquid is planted, is especially obtained in environmental project
Substantial amounts of application is arrived, such as in terms of water for industrial use, the process of domestic water, dirty water purification etc..
Micropore ceramics be a kind of pore structure of micropore ceramics material and open porosity for the application of micropore ceramics material,
Vital impact is played.The consumption for increasing porogen can improve the porosity of ceramics, but can cause under ceramics strength
Drop so that product produce the phenomenon of cracking after firing, percent defective is greatly promoted, additionally, for different raw materials is matched somebody with somebody
Crucial determiner plays also for the final products performance of micropore ceramics material in side, the technique of sintering.
The content of the invention
The present invention overcomes defect of the prior art, there is provided it is a kind of for refine micropore ceramics of tungsten and preparation method thereof and should
With.The present invention provides a kind of micropore ceramics for refining tungsten, is particularly burnt till by the composition of raw materials and preparation technology created
Thermal regulation, prepares a kind of new micropore ceramics.
Technical solution of the present invention is as follows.
A kind of preparation method for refining the micropore ceramics of tungsten, comprises the steps：
（1）Micropore ceramics formula components are taken, is put in ball grinder, sealed ball milling, obtain the powder after ball milling；
（2）The powder after ball milling is weighed, mixed solution is added, is stirred into pureed, be put into gypsum mold extrusion molding, taken out
It is standby；The mixed solution is the mixed solution of organic solvent and water, and concentration of volume percent of the organic solvent in water is 30%
~50%；The organic solvent is water-miscible alcohols；
（3）By step（2）Products obtained therefrom dries naturally, dries in placing into baking oven, and oven temperature setting is opened by 50 ~ 60 DEG C
Begin, 5 ~ 10 DEG C are raised per half an hour, be gradually increased to 70 ~ 80 DEG C of constant temperature, the product after being dried；
（4）With the product after kraft paper one by one hard-pressed bale drying；
（5）Product after the drying that kraft paper is wrapped up is fixed on carborundum plate, is put in high-temperature electric resistance furnace by setting heat
Work systematic procedure burns till, and obtains the micropore ceramics for refining tungsten.
In said method, in the sealing ball milling, micropore ceramics formula components are 1 with the mass ratio of mill ball：2~3；Institute
Ball-milling Time is stated for 5 ~ 7 h.
In said method, step（2）In, the alcohols is isopropanol.
In said method, step（2）In, the extrusion molding is cast or the cup type for being squeezed into bottom lock.
In said method, step（3）In, the time dried naturally is 20-30h；The time dried in the baking oven
For 20-30h.
In said method, step（5）In, the thermal regulation program includes following several stages：
First stage：1.0-2.5 DEG C of heating rate/min, 180-220 DEG C of target temperature, time of staying 0-60
min；
Second stage：3.5 DEG C/min of heating rate 1.5-, 550-650 DEG C of target temperature, time of staying 0-60
min；
Phase III：1.0-3.0 DEG C of heating rate/min, 830-850 DEG C of target temperature, time of staying 20-40
min；
Fourth stage：3.0-4.0 DEG C of heating rate/min, 1335-1350 DEG C of target temperature, time of staying 20-40
min。
A kind of micropore ceramics for refining tungsten, the micropore ceramics formula components are as follows according to mass percent meter：
Aluminium oxide 39%-42%
Albite 19%-21%
Quartzy 12%-13%
Activated carbon 8%-10%
Calcium Carbonate 6%-7%
Rice flour 4%-6%
High viscous sodium carboxymethyl cellulose 2%-5%.
Preferably, the water absorption rate of the micropore ceramics is 35% ~ 40%；The aperture of the micropore ceramics is 30 ~ 60 m.
A kind of micropore ceramics are applied to wet method refining tungsten, comprise the steps：
Tungsten ore sample is added in the micropore ceramics of tubulose, while adding 12 water with the ratio of 2 mMs of every gram of tungsten ore powder
Sodium phosphate（Na3PO4·12H2O）The micropore ceramic tube for having installed tungsten ore sample and inhibitor is positioned over polytetrafluoroethyl-ne by inhibitor
In the counteracting tank of alkene, in the middle of counteracting tank and micropore ceramic tube, 4.0 M NaOH solutions, closed digestion tank are added to disappear using microwave
Politef counteracting tank was risen to 135-150 DEG C from room temperature in 15 minutes by Xie Yi, and insulation stops 15 min, slightly cools down,
Counteracting tank closed cover is opened, micropore ceramic tube is taken out, is obtained through the filtered sodium tungstate of micropore ceramic tube.The sodium tungstate is carried
Rate is taken more than 92%, then only adds for continuous 2 times NaOH solution without inhibitor to extract, extraction rate reached to 99%.
The performance of micropore ceramics is closely related with formula and preparation method, and different composition of raw materials are for preparation process
The requirement of sintering temperature is also different, the change of any one formula material, the parameter during preparation method（Particularly fire
Temperature）Also change therewith, the present invention needs to prepare the micropore ceramics with certain pore size in addition, be applied to wet method refining tungsten,
Therefore it is stricter for the requirement of the preparation technology in preparation process, while the proportioning between each material in composition of raw materials
And an important parameter.
The selection of the preparation method in the present invention, wherein mixed solution is for molding and the performance of final products, product
Pore size play critical decisive action, the selection of alcohols and the concentration pair of alcohols in the mixed solution in the present invention
Forming by a firing in product, porosity, pore size all play an important role, and inventor has found only have by substantial amounts of checking
In concentration range of the present invention, desired micropore ceramics of the invention can be just obtained（Water absorption rate is in 35%-40%）If not existing
In the range of this, even if using same recipe and preparation method, also cannot get the product.
The sintering temperature of present invention original creation, i.e., in the thermal regulation program for referring in said method, the effect of four-stage is not
Together, first stage main purpose is sizing, and second stage main target is that, by combustion of organic matter pore-creating, the phase III is mainly made
With being to finely tune pore-creating by decomposing Calcium Carbonate, fourth stage is to form new mineral solid i.e. micropore ceramics.
Compared with prior art, advantage of the invention is that：
Micropore ceramics of the present invention have the characteristics of water absorption rate is good, and intensity is high, the formula of preparation method bonded products of the present invention,
Corresponding firing temperature is given originally, the characteristics of the method has simple to operate, percent defective is low in preparation process.The present invention
Utilize micropore ceramics material and tungsten is refined for wet method, save reactor and filtration, separating step, using efficient microwave heating skill
Art, automatic fitration, isolates sodium tungstate, has the advantages that efficiency high, low cost, energy-conserving and environment-protective relative to prior art, is adapted to
Industrial applications.
Specific embodiment
Make further concrete detailed description to the present invention with reference to specific embodiment, but embodiments of the present invention are not
It is limited to this, for especially not dated technological parameter, can refer to routine techniquess is carried out.
Embodiment 1
Micropore ceramics formula components are as follows according to mass percent meter：Aluminium oxide 42%；Albite 19%；Quartz 12%；It is living
Property charcoal 10%；Calcium Carbonate 7%；Rice flour 6%；High viscous sodium carboxymethyl cellulose 4%；The gross mass of formula be 500g, the matter of each component
Amount is respectively：Aluminium oxide 210g；Albite 95g；Quartzy 60g；Activated carbon 50g；Calcium Carbonate 35g；Rice flour 30g；High viscous carboxymethyl
Sodium cellulosate 20g.
Prepare in following manner：
（1）The composition of above-mentioned formula is taken, is put it in ball grinder, according to formula material：Ball mass ratio is 1：2 additions are ground
Abrading-ball, seals 6 h of ball milling, obtains the good powder of ball milling；
（2）By the good powder of ball milling, the mixed solution of water and isopropanol is added（Percent by volume of the organic solvent in water
Concentration is 30%）300mL is mixed and is stirred evenly into pureed, is put into gypsum mold and is squeezed into cast（Bottom lock）, carefully take out standby；
（3）Allow cast sample to dry naturally one day, dry one day in placing into baking oven, oven temperature is set by 50 DEG C,
5 DEG C are raised per half an hour, 70 DEG C of constant temperature are gradually increased to；
（4）With the cast sample after the drying of kraft paper hard-pressed bale；
（5）The cast sample that kraft paper is wrapped up is fixed on into carborundum plate, is put in high-temperature electric resistance furnace by setting thermal regulation journey
The fired microporous ceramics of sequence.Wherein, the thermal regulation program of micropore ceramics is as follows：
First stage：2.0 DEG C/min of heating rate, 200 DEG C of target temperature is 0 in the target temperature time of staying
min；Second stage：2.5 DEG C/min of heating rate, 600 DEG C of target temperature, in 0 min of the target temperature time of staying；3rd
Stage：2.0 DEG C/min of heating rate, 835 DEG C of target temperature, in 30 min of the target temperature time of staying；Fourth stage：Rise
3.5 DEG C/min of warm speed, 1350 DEG C of target temperature, in 30 min of the target temperature time of staying.
By test, the water absorption rate of micropore ceramics obtained by the present embodiment is 38%.
Embodiment 2
Micropore ceramics formula components are as follows according to mass percent meter：Aluminium oxide 39%；Albite 20%；Quartz 13%；It is living
Property charcoal 10%；Calcium Carbonate 7%；Rice flour 6%；High viscous sodium carboxymethyl cellulose 5%；The gross mass of formula is 500g；The matter of each component
Amount is respectively：Aluminium oxide 195g；Albite 100g；Quartzy 65g；Activated carbon 50g；Calcium Carbonate 35g；Rice flour 30g；High viscous carboxylic first
Base sodium cellulosate 25g.
Prepare in following manner：
（1）The composition of the above-mentioned formula of precise, puts it in ball grinder, according to formula material：Ball mass ratio is 1：3
Mill ball is added, 5 h of ball milling is sealed, is obtained the good powder of ball milling；
（2）By the good powder of ball milling, the mixed solution of water and isopropanol is added（Percent by volume of the organic solvent in water
Concentration is 50%）300mL is mixed and is stirred evenly into pureed, is put into gypsum mold and is squeezed into cup type, carefully takes out standby；
（3）Allow cast or cup type sample to dry naturally 30h, dry one day in placing into baking oven, oven temperature is set by 55
DEG C start, per half an hour raise 7 DEG C, be gradually increased to 75 DEG C of constant temperature；
（4）With the cup type sample after kraft paper one by one hard-pressed bale drying；
（5）The cup type sample that kraft paper is wrapped up is fixed on into carborundum plate, is put in high-temperature electric resistance furnace by setting thermal regulation journey
The fired microporous ceramics of sequence.Micropore ceramics burn till thermal regulation：
First stage：2.5 DEG C/min of heating rate, 220 DEG C of target temperature, in 5 min of the target temperature time of staying；
Second stage：3.0 DEG C/min of heating rate, 650 DEG C of target temperature, in 3 min of the target temperature time of staying；3rd rank
Section：2.0 DEG C/min of heating rate, 840 DEG C of target temperature, in 25 min of the target temperature time of staying；Fourth stage：Heat up
3.0 DEG C/min of speed, 1335 DEG C of target temperature, in 30 min of the target temperature time of staying.
By test, the water absorption rate of micropore ceramics obtained by the present embodiment is 37%.
Embodiment 3
Micropore ceramics formula components are as follows according to mass percent meter：Aluminium oxide 41%；Albite 21%；Quartz 12%；It is living
Property charcoal 8%；Calcium Carbonate 7%；Rice flour 6%；High viscous sodium carboxymethyl cellulose 5%；The gross mass of formula is 500g；The quality of each component
Respectively：Aluminium oxide 205g；Albite 105g；Quartzy 60g；Activated carbon 40g；Calcium Carbonate 35g；Rice flour 30g；High viscous carboxymethyl
Sodium cellulosate 25g.
Prepare in following manner：
（1）The composition of above-mentioned formula is taken, is put it in ball grinder, according to formula material：Ball mass ratio is 1：2 additions are ground
Abrading-ball, seals 6 h of ball milling；
（2）The good powder of ball milling is weighed, the mixed solution of water and isopropanol is added（Volume basis of the organic solvent in water
Specific concentration is 40%）300mL is mixed and is stirred evenly into pureed, is put into gypsum mold and is squeezed into cast（Bottom lock）, carefully take out standby
With；
（3）Allow cast sample to dry naturally one day, dry one day in placing into baking oven, oven temperature is set by 60 DEG C,
10 DEG C are raised per half an hour, 80 DEG C of constant temperature are gradually increased to；
（4）With the cast sample after the drying of kraft paper hard-pressed bale；
（5）The cast sample that kraft paper is wrapped up is fixed on into carborundum plate, is put in high-temperature electric resistance furnace by setting thermal regulation journey
The fired microporous ceramics of sequence.Wherein, the thermal regulation program of micropore ceramics is as follows：
First stage：1.0 DEG C/min of heating rate, 180 DEG C of target temperature, in the target temperature time of staying 10
min；Second stage：1.5 DEG C/min of heating rate, 550 DEG C of target temperature, in 10 min of the target temperature time of staying；The
Three stages：1.0 DEG C/min of heating rate, 830 DEG C of target temperature, in 40 min of the target temperature time of staying；Fourth stage：
3.0 DEG C/min of heating rate, 1350 DEG C of target temperature, in 30 min of the target temperature time of staying.
By test, the water absorption rate of micropore ceramics obtained by the present embodiment is 37%.
Embodiment 4
The cast micropore ceramics that Example 1 is prepared, 10.0g white tungsten fine ores powder is added in cast micropore ceramics,
Ten phosphate dihydrate sodium are added with the ratio of 2 mMs of every gram of tungsten ore powder simultaneously（Na3PO4·12H2O）Inhibitor, will install
The micropore ceramic tube of tungsten ore sample and inhibitor is positioned in the counteracting tank of politef, in the middle of counteracting tank and micropore ceramic tube
Filling 200mL, politef was cleared up in 15 minutes by 4.0 M NaOH solutions, closed digestion tank using microwave dissolver
Tank rises to 140 DEG C from room temperature, and insulation stops 15 min, slightly cools down, and opens counteracting tank closed cover, takes out micropore ceramic tube, disappears
It is to pass through the filtered sodium tungstate of micropore ceramic tube in solution tank, extraction ratio is 93%.Only add NaOH solution continuous 2 times again
Without inhibitor extracts the extraction ratio that can reach 99%.（The application effect of 3 gained micropore ceramics of embodiment 2 and embodiment with it is above-mentioned
Effect is similar）；It can be seen that, the micropore ceramics of present invention gained greatly improve the energy resource consumption that wet method refines tungsten process, Yi Ji great
Time used by the big regular industrial refining tungsten for shortening, it is adapted to industrial applications.
Comparative example 1
The formula of this comparative example is consistent with embodiment 1 with preparation method, and simply the rice flour in formula is replaced using flour, system
Standby product not molding out, is non-porous cake mass.It can be seen that, adopt rice flour as composition of raw materials composition for product in the present invention
The importance of the molding of product, as the content of protein in flour is larger, and viscosity is too high so that final products do not reach wanted
Result.
Comparative example 2
The preparation method of this comparative example is consistent with embodiment 1, and in formula, each constituent mass content is：Aluminium oxide 33%；Sodium
Anhydrite 20.8%；Quartz 21.6%；Activated carbon 11.6%；Calcium Carbonate 7.5%；Rice flour 5%；High viscous sodium carboxymethyl cellulose 0.5%, always
Quality be 500g, the product water absorption rate for preparing be 11.28%.
Comparative example 3
The preparation method of this comparative example is consistent with embodiment 1, and in formula, each constituent mass content is：Aluminium oxide 41.7%；
Albite 20.8%；Quartz 13.3%；Activated carbon 11.2%；Calcium Carbonate 7.5%；Rice flour 5%；High viscous sodium carboxymethyl cellulose 0.5%,
Total quality is 500g, and the product water absorption rate for preparing is 51.05%, and products obtained therefrom is in spongy, and surface powder is more, firmly
Degree is inadequate, it is impossible to meet the application requirement of refining tungsten.
Comparative example 4
The formula of this comparative example is consistent with embodiment 1 with preparation method, simply in the thermal regulation program of micropore ceramics
Triphasic target temperature is 780 DEG C, and the final temperature of fourth stage is 1360 DEG C, and the product for obtaining is bulk product, can not
Penetrating micropore, it is impossible to meet the application requirement of refining tungsten.
The above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not to the present invention
Embodiment restriction.For those of ordinary skill in the field, can also make on the basis of the above description
The change or variation of other multi-forms.There is no need to be exhaustive to all of embodiment.It is all the present invention
Any modification, equivalent and improvement made within spirit and principle etc., should be included in the protection of the claims in the present invention
Within the scope of.
Claims (8)
1. a kind of application for refining the micropore ceramics of tungsten, it is characterised in that the micropore ceramics are applied to wet method refining tungsten, including
Following steps：
Tungsten ore sample is added in the micropore ceramics of tubulose, while adding ten phosphate dihydrates with the ratio of 2 mMs of every gram of tungsten ore powder
Sodium（Na3PO4·12H2O）The micropore ceramic tube for having installed tungsten ore sample and inhibitor is positioned over politef by inhibitor
In counteracting tank, 4.0 M NaOH solutions are added in the middle of counteracting tank and micropore ceramic tube, closed digestion tank, using microwave dissolver
Politef counteracting tank is risen to into 135-150 DEG C from room temperature in 15 minutes, insulation stops 15 min, slightly cools down, opened
Counteracting tank closed cover, takes out micropore ceramic tube, obtains through the filtered sodium tungstate of micropore ceramic tube；
The preparation method of the micropore ceramics is：
（1）Micropore ceramics formula components are taken, is put in ball grinder, sealed ball milling, obtain the powder after ball milling；
（2）The powder after ball milling is weighed, mixed solution is added, is stirred into pureed, be put into gypsum mold extrusion molding, taken out standby
With；The mixed solution is the mixed solution of organic solvent and water, concentration of volume percent of the organic solvent in water be 30% ~
50%；The organic solvent is water-miscible alcohols；
（3）By step（2）Products obtained therefrom dries naturally, dries in placing into baking oven, oven temperature is set by 50 ~ 60 DEG C,
5 ~ 10 DEG C are raised per half an hour, 70 ~ 80 DEG C of constant temperature, the product after being dried is gradually increased to；
（4）With the product after kraft paper one by one hard-pressed bale drying；
（5）Product after the drying that kraft paper is wrapped up is fixed on carborundum plate, is put in high-temperature electric resistance furnace by setting thermal technology's system
Degree program is burnt till, and obtains the micropore ceramics for refining tungsten；
The micropore ceramics formula components are as follows according to mass percent meter：
Aluminium oxide 39%-42%
Albite 19%-21%
Quartzy 12%-13%
Activated carbon 8%-10%
Calcium Carbonate 6%-7%
Rice flour 4%-6%
High viscous sodium carboxymethyl cellulose 2%-5%.
2. apply according to claim 1, it is characterised in that in the sealing ball milling, micropore ceramics formula components and grinding
The mass ratio of ball is 1：2~3；The Ball-milling Time is 5 ~ 7 h.
3. apply according to claim 1, it is characterised in that step（2）In, the alcohols is isopropanol.
4. apply according to claim 1, it is characterised in that step（2）In, the extrusion molding is to be squeezed into bottom lock
Cast or cup type.
5. apply according to claim 1, it is characterised in that step（3）In, the time dried naturally is 20-30h；
The time dried in the baking oven is 20-30h.
6. apply according to claim 1, it is characterised in that step（5）In, the thermal regulation program includes following several
Stage：
First stage：1.0-2.5 DEG C of heating rate/min, 180-220 DEG C of target temperature, time of staying 0-60 min；
Second stage：3.5 DEG C/min of heating rate 1.5-, 550-650 DEG C of target temperature, time of staying 0-60 min；
Phase III：1.0-3.0 DEG C of heating rate/min, 830-850 DEG C of target temperature, time of staying 20-40 min；
Fourth stage：3.0-4.0 DEG C of heating rate/min, 1335-1350 DEG C of target temperature, time of staying 20-40 min.
7. application according to claim 1, it is characterised in that the water absorption rate of the micropore ceramics is 35% ~ 40%；It is described micro-
The aperture of hole ceramics is 30 ~ 60 m.
8. apply according to claim 1, it is characterised in that the sodium tungstate extraction ratio is more than 92%, then continuous 2 times only add
NaOH solution without inhibitor is extracted, extraction rate reached to 99%.
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