CN107416845B - A kind of method that potassium feldspar produces white silica gel - Google Patents
A kind of method that potassium feldspar produces white silica gel Download PDFInfo
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- CN107416845B CN107416845B CN201710744706.2A CN201710744706A CN107416845B CN 107416845 B CN107416845 B CN 107416845B CN 201710744706 A CN201710744706 A CN 201710744706A CN 107416845 B CN107416845 B CN 107416845B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/152—Preparation of hydrogels
- C01B33/154—Preparation of hydrogels by acidic treatment of aqueous silicate solutions
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- 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
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- 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
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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Abstract
The invention discloses a kind of methods that potassium feldspar produces white silica gel, belong to chemical production field.K-feldspar powder is mixed with nitric acid solution and carries out microwave hydrothermal pretreatment.Then the pretreated K-feldspar powder of nitric acid microwave hydrothermal is mixed with KOH aqueous solution, carries out microwave hydrothermal reaction, is filtered, washed, is dried, obtain acid-soluble lithium aluminium silicate rod-shaped particle.Obtained acid-soluble lithium aluminium silicate rod-shaped particle is dissolved in sulfuric acid solution and carries out microwave hydrothermal, is filtered, washed, dried, obtain white silica gel.The technology of the present invention compares existing potassium feldspar comprehensive utilization technique, the reaction time is shortened, reduces reaction temperature, KOH concentration, acid concentration, and then saved production cost and the energy, it has been greatly reduced potassium feldspar simultaneously during comprehensive utilization to the corrosion of equipment, has been expected to realize industrialized production.
Description
Technical field
The invention belongs to chemical production fields, and in particular to a kind of method that potassium feldspar produces white silica gel.
Background technique
The potash feldspar ore in China is that potassium content is higher, distribution is most wide, the maximum water-insoluble potassium resource of reserves.How in room
It is one of China's important topic that the potassium in potassium feldspar, which is transformed into solubility by insolubility, under temperature.Domestic potassium feldspar resource is rich
Richness, but iron-content is exceeded, and therefore, potash feldspar deferrization is the key that purification.Currently, potassium feldspar can pass through microwave hydrothermal desiliconization skill
Art prepares kaliophilite, the potassium in Lai Shixian potassium feldspar from insolubility to solvable sex reversal, such as patent (patent No.:
201010543249.9) K-feldspar powder and KOH 2~8h of hydro-thermal reaction under conditions of 220~280 DEG C are disclosed, it can desiliconization
Obtain kalsilite powder.Patent (patent No.: 201110064828.X) discloses at 40~80 DEG C, with 20~40% sulphur
Acidleach mentions the potassium in kalsilite.However these techniques are more or less all in place of Shortcomings, it such as can not be to mention potassium merely
Residue afterwards finds that reasonable utilization approach, potassium feldspar resource comprehensive utilization process is cumbersome, technological temperature is relatively high, high concentration
Acid or alkali to the corrosion of equipment and pollution environment the disadvantages of.
Summary of the invention
In order to overcome the problems of the above-mentioned prior art, it is an object of the invention to a kind of potassium feldspars to produce white silica gel
Method, this method is easy to operate, can be realized potassium feldspar purification, and can at a lower temperature, in the short period, by acid not
Molten potassium feldspar is transformed into acid-soluble lithium aluminium silicate, realizes potassium feldspar comprehensive utilization of resources.
The present invention is to be achieved through the following technical solutions:
The method that a kind of potassium feldspar disclosed by the invention produces white silica gel, comprising the following steps:
1) K-feldspar powder is mixed to progress microwave hydrothermal pretreatment with nitric acid solution and obtains pre- place after being filtered, washed
The K-feldspar powder of reason；
Wherein, the K-feldspar powder is that potassium feldspar ore is long through broken and ball milling, the potassium of 200 mesh of partial size < obtained
Mountain flour body；
2) pretreated K-feldspar powder is mixed with KOH aqueous solution, carries out microwave hydrothermal reaction, is filtered, washed, is done
It is dry, obtain acid-soluble lithium aluminium silicate rod-shaped particle；
3) obtained acid-soluble lithium aluminium silicate rod-shaped particle is dissolved in progress microwave hydrothermal reaction in sulfuric acid solution, passed through
Filter, washing, drying, obtain white silica gel.
Preferably, in step 1), the amount ratio of K-feldspar powder and nitric acid solution is 1g:(6~12) mL.
Preferably, the concentration of the nitric acid solution is 0.1~1mol/L.
Preferably, in step 1), the pretreated temperature of microwave hydrothermal is 100~150 DEG C, and the processing time is 1~4h.
Preferably, in step 2), the concentration of KOH aqueous solution is 1~4mol/L.
Preferably, in step 2), the temperature of microwave hydrothermal reaction is 100~150 DEG C, and the reaction time is 2~4h.
Preferably, the length of acid-soluble lithium aluminium silicate particle made from step 2) is 3~5 μm, and diameter is 0.2~0.5 μm.
Preferably, in step 3), sulfuric acid solution concentration is 0.1~1mol/L.
Preferably, the dosage of sulfuric acid solution are as follows: 20~40 milliliters of sulfuric acid solutions of every gram of K-feldspar powder.
Preferably, in step 3), the temperature of microwave hydrothermal reaction is 60~150 DEG C, and the reaction time is 0.5~2h.
Compared with prior art, the invention has the following beneficial technical effects:
The method that a kind of potassium feldspar disclosed by the invention produces white silica gel, K-feldspar powder and nitric acid solution are mixed into
The pretreatment of row microwave hydrothermal, can make K-feldspar powder under lower KOH concentration and microwave hydrothermal temperature, quick desiliconization transformation
At acid soluble lithium aluminium silicate rod-shaped particle, while pre-processing some impurity elements that can remove inside powder, for example, iron, calcium,
Magnesium, manganese etc..The present invention makes K-feldspar powder that can obtain white by the reaction of three step low temperature (100~150 DEG C) microwave hydrothermal,
Microwave hydrothermal technology (220~280 DEG C) are comprehensively utilized compared to existing potassium feldspar, reduce reaction temperature, KOH concentration, acid concentration,
Accident risk is also reduced, the corrosion to equipment is reduced, is more suitable industrialized production.
Detailed description of the invention
Fig. 1 is the XRD spectra of K-feldspar powder Yu acid-soluble lithium aluminium silicate rod-shaped particle prepared by the present invention；A is in figure
K-feldspar powder, b are acid-soluble lithium aluminium silicate rod-shaped particle；
Fig. 2 is the SEM photograph of K-feldspar powder；
Fig. 3 is the SEM photograph of acid-soluble lithium aluminium silicate rod-shaped particle prepared by the present invention；
Fig. 4 is white silica gel powder photo prepared by the present invention.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Embodiment 1
5g K-feldspar powder is mixed with 30ml concentration for 0.1mol/L nitric acid solution, it is pre- in 100 DEG C of progress microwave hydrothermals
1h is handled, after being filtered, washed, pretreated K-feldspar powder is mixed with the KOH aqueous solution that 30ml concentration is 1mol/L,
Then after carrying out microwave hydrothermal reaction 2h under conditions of 100 DEG C, be filtered, washed, dried, obtain length be 3~5 μm, it is straight
The lithium aluminium silicate rod-shaped particle that diameter is 0.2~0.5 μm.
By obtained acid-soluble lithium aluminium silicate rod-shaped particle be dissolved in 100ml concentration be 0.1mol/L sulfuric acid solution in,
60 DEG C of progress microwave hydrothermal 0.5h, are filtered, washed, are dried, obtain white silica gel.
Embodiment 2
5g K-feldspar powder is mixed with 30ml concentration for 1mol/L nitric acid solution, is located in advance in 120 DEG C of progress microwave hydrothermals
2h is managed, after being filtered, washed, pretreated K-feldspar powder is mixed with the KOH aqueous solution that 30ml concentration is 2mol/L, so
It after carrying out microwave hydrothermal reaction 4h under conditions of 150 DEG C afterwards, is filtered, washed, dried, obtaining length is 3~5 μm, diameter
For 0.2~0.5 μm of lithium aluminium silicate rod-shaped particle.
By obtained acid-soluble lithium aluminium silicate rod-shaped particle be dissolved in 100ml concentration be 0.1mol/L sulfuric acid solution in,
100 DEG C of progress microwave hydrothermal 0.5h, are filtered, washed, are dried, obtain white silica gel.
Embodiment 3
5g K-feldspar powder is mixed with 60ml concentration for 1mol/L nitric acid solution, is located in advance in 150 DEG C of progress microwave hydrothermals
1h is managed, after being filtered, washed, pretreated K-feldspar powder is mixed with the KOH aqueous solution that 60ml concentration is 1mol/L, so
It after carrying out microwave hydrothermal reaction 2h under conditions of 130 DEG C afterwards, is filtered, washed, dried, obtaining length is 3~5 μm, diameter
For 0.2~0.5 μm of lithium aluminium silicate rod-shaped particle.
By obtained acid-soluble lithium aluminium silicate rod-shaped particle be dissolved in 150ml concentration be 0.5mol/L sulfuric acid solution in,
150 DEG C of progress microwave hydrothermal 1h, are filtered, washed, are dried, obtain white silica gel.
Embodiment 4
5g K-feldspar powder is mixed with 50ml concentration for 0.5mol/L nitric acid solution, it is pre- in 130 DEG C of progress microwave hydrothermals
3h is handled, after being filtered, washed, pretreated K-feldspar powder is mixed with the KOH aqueous solution that 40ml concentration is 4mol/L,
Then after carrying out microwave hydrothermal reaction 2h under conditions of 150 DEG C, be filtered, washed, dried, obtain length be 3~5 μm, it is straight
The lithium aluminium silicate rod-shaped particle that diameter is 0.2~0.5 μm.
It is in 1mol/L sulfuric acid solution, 100 that obtained acid-soluble lithium aluminium silicate rod-shaped particle, which is dissolved in 200ml concentration,
DEG C carry out microwave hydrothermal 1h, be filtered, washed, dried, obtain white silica gel.
Embodiment 5
5g K-feldspar powder is mixed with 60ml concentration for 1mol/L nitric acid solution, is located in advance in 150 DEG C of progress microwave hydrothermals
4h is managed, after being filtered, washed, pretreated K-feldspar powder is mixed with the KOH aqueous solution that 60ml concentration is 4mol/L, so
It after carrying out microwave hydrothermal reaction 4h under conditions of 150 DEG C afterwards, is filtered, washed, dried, obtaining length is 3~5 μm, diameter
For 0.2~0.5 μm of lithium aluminium silicate rod-shaped particle.
It is in 2mol/L sulfuric acid solution, 120 that obtained acid-soluble lithium aluminium silicate rod-shaped particle, which is dissolved in 200ml concentration,
DEG C carry out microwave hydrothermal 2h, be filtered, washed, dried, obtain white silica gel.
In conclusion the present invention is pre-processed by the nitric acid microwave hydrothermal of K-feldspar powder, K-feldspar powder can be made
Under lower KOH concentration and microwave hydrothermal temperature, quick desiliconization is transformed into acid soluble lithium aluminium silicate rod-shaped particle.This silicic acid
Aluminium potassium rod-shaped particle can be dissolved in progress microwave hydrothermal processing in dilution heat of sulfuric acid at room temperature, be filtered, washed, dried,
Obtain white silica gel.
Referring to Fig. 1, a from Fig. 1 is it is found that the diffraction maximum and standard PDF card of K-feldspar powder are the diffraction maximum of 72-1114
It coincide；From b in Fig. 1 it is found that the lithium aluminium silicate that the diffraction maximum of product obtained by the present invention and standard PDF card are 31-0965
Diffraction maximum is consistent.Referring to fig. 2, as can be seen from Figure 2,2 μm of the partial size < of K-feldspar powder of the present invention, and have irregular
Pattern；Referring to Fig. 3, as can be seen from Figure 3, lithium aluminium silicate particle prepared by the present invention shows Rod-like shape, the length is 3~5 μm,
Diameter is 0.2~0.5 μm.Referring to fig. 4, as can be seen from Figure 4, silica gel powder prepared by the present invention is white.
In conclusion largely limiting its comprehensive utilization since potassium feldspar is difficult to dissolve in mineral acid.This hair
The bright nitric acid microwave hydrothermal by K-feldspar powder pre-processes, and K-feldspar powder can be made in lower KOH concentration and Microwave Water
At hot temperature, quick desiliconization is transformed into acid soluble lithium aluminium silicate rod-shaped particle.This lithium aluminium silicate rod-shaped particle is at room temperature
It can be dissolved in dilution heat of sulfuric acid, carry out microwave hydrothermal reaction, be filtered, washed, dried, obtain white silica gel.
Above said content is that a further detailed description of the present invention in conjunction with specific preferred embodiments, is not
Whole or unique embodiment, those of ordinary skill in the art are by reading description of the invention to technical solution of the present invention
Any equivalent transformation taken, all are covered by the claims of the invention.
Claims (10)
1. a kind of method that potassium feldspar produces white silica gel, which comprises the following steps:
1) K-feldspar powder and nitric acid solution are mixed in progress microwave hydrothermal pretreatment at 100~150 DEG C, through being filtered, washed
Afterwards, pretreated K-feldspar powder is obtained；
Wherein, the K-feldspar powder is by potassium feldspar ore through broken and ball milling, the feldspar in powder of 200 mesh of partial size < obtained
Body；
2) pretreated K-feldspar powder is mixed with KOH aqueous solution, microwave hydrothermal reaction is carried out at 100~150 DEG C, passed through
Filter, washing, drying, obtain acid-soluble lithium aluminium silicate rod-shaped particle；
3) obtained acid-soluble lithium aluminium silicate rod-shaped particle is dissolved in sulfuric acid solution, Microwave Water is carried out at 60~150 DEG C
Thermal response is filtered, washed, is dried, obtains white silica gel.
2. the method that potassium feldspar according to claim 1 produces white silica gel, which is characterized in that in step 1), potassium feldspar
Powder and the amount ratio of nitric acid solution are 1g:(6~12) mL.
3. the method that potassium feldspar according to claim 1 or 2 produces white silica gel, which is characterized in that the nitric acid solution
Concentration be 0.1~1mol/L.
4. the method that potassium feldspar according to claim 1 produces white silica gel, which is characterized in that in step 1), Microwave Water
The processing time of Grape berry is 1~4h.
5. the method that potassium feldspar according to claim 1 produces white silica gel, which is characterized in that in step 2), KOH is water-soluble
The concentration of liquid is 1~4mol/L.
6. the method that potassium feldspar according to claim 1 produces white silica gel, which is characterized in that in step 2), Microwave Water
The reaction time of thermal response is 2~4h.
7. the method that potassium feldspar according to claim 1 produces white silica gel, which is characterized in that acid made from step 2) is molten
Property lithium aluminium silicate particle length be 3~5 μm, diameter be 0.2~0.5 μm.
8. the method that potassium feldspar according to claim 1 produces white silica gel, which is characterized in that in step 3), sulfuric acid is molten
Liquid concentration is 0.1~1mol/L.
9. the method that a kind of potassium feldspar according to claim 1 or 8 produces white silica gel, which is characterized in that sulfuric acid solution
Dosage are as follows: 20~40 milliliters of sulfuric acid solutions of every gram of K-feldspar powder.
10. the method that a kind of potassium feldspar according to claim 1 produces white silica gel, which is characterized in that micro- in step 3)
The reaction time of wave hydro-thermal reaction is 0.5~2h.
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| CN108083288A (en) * | 2018-02-24 | 2018-05-29 | 洛南县大秦钾矿有限公司 | A kind of method of low-quality potash feldspar deferrization purification |
| CN109019620A (en) * | 2018-08-31 | 2018-12-18 | 贺州市骏鑫矿产品有限责任公司 | A kind of method of low-quality potash feldspar deferrization purification |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1765837A (en) * | 2005-09-12 | 2006-05-03 | 鄂州市长润农业生态技术有限公司 | Potash feldspar wet method decomposition and production process |
| CN103787421A (en) * | 2013-12-24 | 2014-05-14 | 贵州远盛钾业科技有限公司 | Comprehensive utilization method of sylvine-containing rock |
| CN105621426A (en) * | 2016-03-25 | 2016-06-01 | 陕西大秦钾业有限公司 | Low-temperature microwave hydrothermal desiliconization method for potassium feldspar |
| CN106745085A (en) * | 2016-11-30 | 2017-05-31 | 东至天孚化工有限公司 | A kind of potassium sulfate preparation method based on potassium feldspar |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1765837A (en) * | 2005-09-12 | 2006-05-03 | 鄂州市长润农业生态技术有限公司 | Potash feldspar wet method decomposition and production process |
| CN103787421A (en) * | 2013-12-24 | 2014-05-14 | 贵州远盛钾业科技有限公司 | Comprehensive utilization method of sylvine-containing rock |
| CN105621426A (en) * | 2016-03-25 | 2016-06-01 | 陕西大秦钾业有限公司 | Low-temperature microwave hydrothermal desiliconization method for potassium feldspar |
| CN106745085A (en) * | 2016-11-30 | 2017-05-31 | 东至天孚化工有限公司 | A kind of potassium sulfate preparation method based on potassium feldspar |
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