CN106044782A - Method for separating silicon dioxide in wollastonite raw ore - Google Patents
Method for separating silicon dioxide in wollastonite raw ore Download PDFInfo
- Publication number
- CN106044782A CN106044782A CN201610382334.9A CN201610382334A CN106044782A CN 106044782 A CN106044782 A CN 106044782A CN 201610382334 A CN201610382334 A CN 201610382334A CN 106044782 A CN106044782 A CN 106044782A
- Authority
- CN
- China
- Prior art keywords
- quality
- silicon dioxide
- wollastonite
- raw ore
- added
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a method for separating silicon dioxide in wollastonite raw ore. The method comprises the steps that the wollastonite raw ore is subjected to smashing, ball milling and magnetic separation to obtain a material A; water is added into the material A, the pH is adjusted, oxidized paraffinum sodium salt and stearic acid are added for flotation, and a material B is obtained; the material B is added into an oxalic acid solution with the pH being 1-3 after being calcined, and filtering, washing and drying are carried out to obtain a material C; the material C is added into water, ammonium chloride is added, ammonium chloride is added after microwave heating, the pH is adjusted to range from 0.6 to 1.2, and sol is obtained; a surface active agent is added into the sol, the pH is adjusted to range from 3 to 4, hydrochloric acid is added, the pH is adjusted to range from 0.6 to 1.2, and a material D is obtained; the material D, sodium fluoride, sodium hydroxide, hydrochloric acid and nitrilotrimethylene triphosphonic acid are added into water for a hydrothermal reaction. According to the method for separating silicon dioxide in the wollastonite raw ore, the steps are simple, and obtained silicon dioxide is high in yield and purity, good in stability and capable of being applied to multiple fields.
Description
Technical field
The present invention relates to silicon dioxide extractive technique field, particularly relate to the separation of silicon dioxide in a kind of wollastonite raw ore
Method.
Background technology
Wollastonite is needle-like or feather salt, resistance is high, dielectric constant is low, hygroscopicity is low, good dispersion, viscosity are low,
Draw ratio is big, owing to wollastonite mine has glaze dispensing, low Jie that above-mentioned excellent performance makes it be widely used in ceramic industry
Electroceramics raw material, the cast steel covering slag of steel and iron industry, electric welding industry, coating, pigment industry, plastic, rubber industry, glass workers and peasants
The fields such as industry, building material industry, national defense industry.
The chemical molecular formula of wollastonite is CaSiO3, structural formula is Ca3[Si3O9], theoretical chemistry composition: CaO:
48.25%, SiO2:51.75%, can be as the source of silicon dioxide.But owing to wollastonite is during being formed, wherein
Ca sometimes by the displacement of Fe, Mn, Ti, Sr plasma portion in isomorph body, and be mixed with a small amount of Al and trace K, Na, and
Temperature, the condition such as pressure when wollastonite is formed are different, and the wollastonite difference on composition causing different regions is very big, existing
The technique extraction effect utilizing wollastonite mine to extract silicon dioxide in technology is not fine, there is extraction ratio the highest, purity difference
Shortcoming, limits the application of gained silicon dioxide.
Summary of the invention
The technical problem existed based on background technology, the present invention proposes the separation of silicon dioxide in a kind of wollastonite raw ore
Method, its step is simple, and the silicon dioxide productivity obtained and purity are high, and good stability can meet the application of multiple fields.
The separation method of silicon dioxide in a kind of wollastonite raw ore that the present invention proposes, comprises the following steps:
S1, add in ball mill after wollastonite crushing raw ore, the modulation that adds water, add grinding aid ball milling 20-50min, its
In, the quality of grinding aid is the 0.05-0.1wt% of wollastonite ore quality；Ball milling is 3000-in magnetic separation strength after terminating
The magnetic separator of 4500kA/m carries out magnetic separation and obtains material A；
S2, material A being added water is configured to the ore pulp that concentration is 15-25wt%, and the pH value of regulation ore pulp is 8-10, adds oxygen
Fossil waxes soap and stearic acid flotation 20-45min, then through washing, being dried to obtain material B；Wherein, the oxidation that every liter of ore pulp adds
The quality of paraffin soap is 1-2kg, and the stearic quality of every liter of ore pulp addition is 30-50g；
S3, will material B calcine after add in the oxalic acid solution that pH value is 1-3, wherein, the volume of material B and oxalic acid solution
Ratio is 1:6-10, ultrasonic 30-80min at 80-95 DEG C, through filtering, wash, be dried to obtain material C, wherein, ultrasonic power
For 1000-2000W；
S4, being added to the water by material C and be configured to the suspension that mass fraction is 15-20wt%, add ammonium chloride, every liter hangs
The quality of the ammonium chloride added in supernatant liquid is 10-25g, and microwave heating, to 60-80 DEG C, stirs 10-25min, is subsequently adding hydrochloric acid
Regulation pH value is 0.6-1.2, reacts 5-15min, is filtrated to get colloidal sol；Adding surfactant in colloidal sol, wherein, live in surface
The 0.5-1wt% that consumption is colloidal sol quality of property agent, the pH value of regulation system is 3-4, is subsequently adding salt acid for adjusting pH value and is
0.6-1.2, ultrasonic 5-10min, filter, wash, be dried to obtain material D；
S5, it is that the hydrochloric acid of 25-35%, ATMP add by material D, sodium fluoride, sodium hydroxide, mass fraction
Entering during mix homogeneously is placed on hydrothermal reaction kettle in water, react 15-20h at 100-135 DEG C, wherein the quality of sodium fluoride is thing
The 3-6wt% of material D mass, the quality of sodium hydroxide is the 1-2.5wt% of material D mass, the quality of ATMP
For the 1-2.5wt% of material D mass, mass fraction is the 4-15wt% that quality is material D mass of the hydrochloric acid of 25-35%；Instead
Through cooling down, filter, wash, being dried to obtain silicon dioxide after should terminating.
Preferably, in S1, during wollastonite crushing raw ore, it is crushed to particle diameter≤0.5mm.
Preferably, in S1, described grinding aid is isoamyl alcohol, sodium stearate, sodium naphthenate, cycloalkylsulfonic acid sodium, chlorination
One or more mixture in sodium, dodecylbenzene sodium sulfonate, 18-amine., manganese dioxide, amyl acetate.
Preferably, in S1, magnetic separation strength is 3500-4000kA/m, and feed ore concentration is 30-40wt%, and rotating speed is 150-
180r/min。
Preferably, in S3, described calcining is two-section calcining, and the temperature of a section calcining is 600-800 DEG C, a section calcining
Time is 30-60min, and the temperature of two section calcinings is 950-1200 DEG C, and the time of two section calcinings is 1-1.5h.
Preferably, in S4, the power of microwave heating is 1000-1500W.
Preferably, in S4, the mass fraction of hydrochloric acid is 13-25wt%.
Preferably, in S4, described surfactant is polyvinyl alcohol, Polyethylene Glycol, polyvinylpyrrolidone, Ji Wusi
One or more mixture in alcohol, stearic acid, citric acid, oleic acid.
In wollastonite raw ore of the present invention in the separation method of silicon dioxide, first by wollastonite crushing raw ore, effectively
Associated mineral and wollastonite mine are separated；Add grinding aid ball milling, reduce the surface energy of wollastonite particles, accelerate ball milling effect
Rate, reduces power consumption and improves the separating effect of impurity and wollastonite simultaneously；Carry out magnetic separation afterwards, effectively removes wollastonite
Magnetic impurity ore particle in raw ore；Add oxidized paraffin wax soap and stearic acid carries out flotation, by controlling the technological parameter of flotation, make
Oxidized paraffin wax soap captures carbonate mineral and is removed；Add in oxalic acid solution after calcining and carry out acidleach, along with the urgency of temperature
Cold anxious heat, Ore makes impurity therein be more easy to cruelly be leaked at enlarged volume and the process reduced, in oxalic acid, oxalic acid can with cruelly
The foreign ion reactions such as the iron ion of leakage, aluminium ion, under the effect of ultrasonic wave added, improve except ferrum, except the efficiency of aluminum rate, with
Time improve the whiteness of gained silicon dioxide, stability and thermostability；Under the effect of ammonium chloride, the ginseng reacted by control
Number, makes wollastonite and hydrochloric acid reaction obtain colloidal sol, and colloidal sol is hydrolyzed to silicon dioxide further, improves the productivity of silicon dioxide,
Wherein, due to the existence of microwave, make ore particle crack, specific surface area increase, make hydrochloric acid be more easy to go deep into, inside ore particle, adding
With the reaction chance of impurity in Ore, promote the carrying out of reaction；Add sodium fluoride, sodium hydroxide, hydrochloric acid and aminotrimethylene
Phosphonic acids carries out hydro-thermal reaction and eliminates the trace impurity units such as the lithium in silicon dioxide, sodium, potassium, boron, phosphorus further silicon dioxide
Element, further increases the purity of silicon dioxide.
Detailed description of the invention
Below, by specific embodiment, technical scheme is described in detail.
Embodiment 1
The separation method of silicon dioxide in a kind of wollastonite raw ore that the present invention proposes, comprises the following steps:
S1, add in ball mill after wollastonite crushing raw ore, the modulation that adds water, add grinding aid ball milling 50min, wherein,
The quality of grinding aid is the 0.05wt% of wollastonite ore quality；Ball milling is the magnetic separator of 4500kA/m in magnetic separation strength after terminating
In carry out magnetic separation and obtain material A；
S2, material A being added water is configured to the ore pulp that concentration is 15wt%, and the pH value of regulation ore pulp is 10, adds oxidation stone
Wax soap and stearic acid flotation 20min, then through washing, being dried to obtain material B；Wherein, the oxidized paraffin wax soap that every liter of ore pulp adds
Quality be 2kg, the stearic quality that every liter of ore pulp adds is 30g；
S3, will material B calcine after add in the oxalic acid solution that pH value is 3, wherein, the volume ratio of material B and oxalic acid solution
For 1:6, ultrasonic 30min at 95 DEG C, through filtering, wash, be dried to obtain material C, wherein, ultrasonic power is 2000W；
S4, material C is added to the water it is configured to the suspension that mass fraction is 15wt%, add ammonium chloride, every liter of suspension
The quality of the ammonium chloride added in liquid is 25g, microwave heating to 60 DEG C, stirs 25min, and being subsequently adding salt acid for adjusting pH value is
0.6, react 15min, be filtrated to get colloidal sol；Adding surfactant in colloidal sol, wherein, the consumption of surfactant is colloidal sol
The 0.5wt% of quality, the pH value of regulation system is 4, is subsequently adding hydrochloric acid, and regulation pH value is 0.6, and ultrasonic 10min filters, washes
Wash, be dried to obtain material D；
S5, be the hydrochloric acid of 35% by material D, sodium fluoride, sodium hydroxide, mass fraction, ATMP adds
During mix homogeneously is placed on hydrothermal reaction kettle in water, reacting 20h at 100 DEG C, wherein the quality of sodium fluoride is material D mass
3wt%, the quality of sodium hydroxide is the 2.5wt% of material D mass, and the quality of ATMP is material D mass
1wt%, mass fraction is the 4wt% that quality is material D mass of the hydrochloric acid of 35%；React after terminating through cooling down, filter, washing
Wash, be dried to obtain silicon dioxide.
Embodiment 2
The separation method of silicon dioxide in a kind of wollastonite raw ore that the present invention proposes, comprises the following steps:
S1, add in ball mill after wollastonite crushing raw ore, the modulation that adds water, add grinding aid ball milling 20min, wherein,
The quality of grinding aid is the 0.1wt% of wollastonite ore quality；Ball milling is the magnetic separator of 3000kA/m in magnetic separation strength after terminating
In carry out magnetic separation and obtain material A；
S2, material A being added water is configured to the ore pulp that concentration is 25wt%, and the pH value of regulation ore pulp is 8, adds oxidized paraffin wax
Soap and stearic acid flotation 45min, then through washing, being dried to obtain material B；Wherein, the oxidized paraffin wax soap that every liter of ore pulp adds
Quality is 1kg, and the stearic quality of every liter of ore pulp addition is 50g；
S3, will material B calcine after add in the oxalic acid solution that pH value is 1, wherein, the volume ratio of material B and oxalic acid solution
For 1:10, ultrasonic 80min at 80 DEG C, through filtering, wash, be dried to obtain material C, wherein, ultrasonic power is 1000W；
S4, material C is added to the water it is configured to the suspension that mass fraction is 20wt%, add ammonium chloride, every liter of suspension
The quality of the ammonium chloride added in liquid is 10g, microwave heating to 80 DEG C, stirs 10min, and being subsequently adding salt acid for adjusting pH value is
1.2, react 5min, be filtrated to get colloidal sol；Adding surfactant in colloidal sol, wherein, the consumption of surfactant is colloidal sol
The 1wt% of quality, the pH value of regulation system is 3, and being subsequently adding salt acid for adjusting pH value is 1.2, ultrasonic 5min, filters, washs, does
Dry obtain material D；
S5, be the hydrochloric acid of 25% by material D, sodium fluoride, sodium hydroxide, mass fraction, ATMP adds
During mix homogeneously is placed on hydrothermal reaction kettle in water, reacting 15h at 135 DEG C, wherein the quality of sodium fluoride is material D mass
6wt%, the quality of sodium hydroxide is the 1wt% of material D mass, and the quality of ATMP is material D mass
2.5wt%, mass fraction is the 15wt% that quality is material D mass of the hydrochloric acid of 25%；Reaction terminate after through cooling, filter,
Wash, be dried to obtain silicon dioxide.
Embodiment 3
The separation method of silicon dioxide in a kind of wollastonite raw ore that the present invention proposes, comprises the following steps:
S1, by wollastonite crushing raw ore to particle diameter≤0.5mm, add water and be modulated into the slip that mass fraction is 15wt%, so
In rear addition ball mill, adding isoamyl alcohol ball milling 25min, wherein, the quality of isoamyl alcohol is wollastonite ore quality
0.06wt%；Ball milling carries out magnetic separation in the magnetic separator that magnetic separation strength is 3800kA/m after terminating and obtains material A；Mistake in magnetic separation
Cheng Zhong, feed ore concentration is 30wt%, and rotating speed is 180r/min；
S2, material A being added water is configured to the ore pulp that concentration is 18wt%, and the pH value of regulation ore pulp is 9, adds oxidized paraffin wax
Soap and stearic acid flotation 28min, then through washing, being dried to obtain material B；Wherein, the oxidized paraffin wax soap that every liter of ore pulp adds
Quality is 1.2kg, and the stearic quality of every liter of ore pulp addition is 43g；
S3, material B carrying out two-section calcining, wherein, the temperature of a section calcining is 800 DEG C, and the time of a section calcining is
30min, the temperature of two section calcinings is 1200 DEG C, and the time of two section calcinings is 1h, is subsequently adding in the oxalic acid solution that pH value is 1,
Wherein, material B is 1:9 with the volume ratio of oxalic acid solution, and ultrasonic 70min at 86 DEG C, through filtering, wash, being dried to obtain material
C, wherein, ultrasonic power is 1200W；
S4, material C is added to the water it is configured to the suspension that mass fraction is 16wt%, add ammonium chloride, every liter of suspension
The quality of the ammonium chloride added in liquid is 22g, is heated to 66 DEG C with the power microwave of 1000W, stirs 22min, is subsequently adding matter
Measuring the salt acid for adjusting pH value that mark is 25wt% is 0.8, reacts 12min, is filtrated to get colloidal sol；Surface activity is added in colloidal sol
Agent, wherein, the consumption of surfactant is the 0.6wt% of colloidal sol quality, and the pH value of regulation system is 4, is subsequently adding quality and divides
Number is 0.9 for the salt acid for adjusting pH value of 25wt%, and ultrasonic 9min filters, washs, is dried to obtain material D；Described surfactant
For polyvinyl alcohol, Polyethylene Glycol, polyvinylpyrrolidone, tetramethylolmethane, stearic acid, citric acid, oleic acid by any weight ratio
Mixture；
S5, be the hydrochloric acid of 32% by material D, sodium fluoride, sodium hydroxide, mass fraction, ATMP adds
During mix homogeneously is placed on hydrothermal reaction kettle in water, reacting 19h at 108 DEG C, wherein the quality of sodium fluoride is material D mass
4wt%, the quality of sodium hydroxide is the 2.2wt% of material D mass, and the quality of ATMP is material D mass
1.6wt%, mass fraction is the 7wt% that quality is material D mass of the hydrochloric acid of 32%；React after terminating through cooling down, filter, washing
Wash, be dried to obtain silicon dioxide.
Embodiment 4
The separation method of silicon dioxide in a kind of wollastonite raw ore that the present invention proposes, comprises the following steps:
S1, by wollastonite crushing raw ore to particle diameter≤0.5mm, add water and be modulated into the slip that mass fraction is 25wt%, so
In rear addition ball mill, adding grinding aid ball milling 40min, wherein, the quality of grinding aid is wollastonite ore quality
0.07wt%；Ball milling carries out magnetic separation in the magnetic separator that magnetic separation strength is 4200kA/m after terminating and obtains material A；Wherein, described
Grinding aid be isoamyl alcohol, sodium stearate, sodium naphthenate, cycloalkylsulfonic acid sodium, sodium chloride, dodecylbenzene sodium sulfonate, 18-amine.,
Manganese dioxide, amyl acetate are by the mixture of any weight ratio；During magnetic separation, feed ore concentration is 40wt%, and rotating speed is
150r/min；
S2, material A being added water is configured to the ore pulp that concentration is 22wt%, and the pH value of regulation ore pulp is 8.5, adds oxidation stone
Wax soap and stearic acid flotation 40min, then through washing, being dried to obtain material B；Wherein, the oxidized paraffin wax soap that every liter of ore pulp adds
Quality be 1.8kg, the stearic quality that every liter of ore pulp adds is 36g；
S3, material B carrying out two-section calcining, wherein, the temperature of a section calcining is 600 DEG C, and the time of a section calcining is
60min, the temperature of two section calcinings is 950 DEG C, and the time of two section calcinings is 1.5h, is subsequently adding in the oxalic acid solution that pH value is 2,
Wherein, material B is 1:7 with the volume ratio of oxalic acid solution, and ultrasonic 45min at 93 DEG C, through filtering, wash, being dried to obtain material
C, wherein, ultrasonic power is 1700W；
S4, material C is added to the water it is configured to the suspension that mass fraction is 18wt%, add ammonium chloride, every liter of suspension
The quality of the ammonium chloride added in liquid is 16g, is heated to 73 DEG C with the power microwave of 1500W, stirs 16min, is subsequently adding matter
Measuring the salt acid for adjusting pH value that mark is 13wt% is 1.1, reacts 8min, is filtrated to get colloidal sol；Polyethylene Glycol is added in colloidal sol
And polyvinylpyrrolidone, wherein, the consumption of Polyethylene Glycol is the 0.5wt% of colloidal sol quality, the consumption of polyvinylpyrrolidone
For the 0.3wt% of colloidal sol quality, the pH value of regulation system is 3, is subsequently adding the salt acid for adjusting pH value that mass fraction is 13wt%
It is 0.7, ultrasonic 7min, filters, washs, is dried to obtain material D；
S5, be the hydrochloric acid of 28% by material D, sodium fluoride, sodium hydroxide, mass fraction, ATMP adds
During mix homogeneously is placed on hydrothermal reaction kettle in water, reacting 17h at 130 DEG C, wherein the quality of sodium fluoride is material D mass
5wt%, the quality of sodium hydroxide is the 1.5wt% of material D mass, and the quality of ATMP is material D mass
2.1wt%, mass fraction is the 12wt% that quality is material D mass of the hydrochloric acid of 28%；Reaction terminate after through cooling, filter,
Wash, be dried to obtain silicon dioxide.
Embodiment 5
The separation method of silicon dioxide in a kind of wollastonite raw ore that the present invention proposes, comprises the following steps:
S1, by wollastonite crushing raw ore to particle diameter≤0.5mm, add water and be modulated into the slip that mass fraction is 20wt%, so
In rear addition ball mill, adding cycloalkylsulfonic acid sodium ball milling 38min, wherein, the quality of cycloalkylsulfonic acid sodium is wollastonite raw ore
The 0.08wt% of quality；Ball milling carries out magnetic separation in the magnetic separator that magnetic separation strength is 4000kA/m after terminating and obtains material A, its
In, the feed ore concentration of magnetic separation is 35wt%, and rotating speed is 160r/min；
S2, material A being added water is configured to the ore pulp that concentration is 22wt%, and the pH value of regulation ore pulp is 9, adds oxidized paraffin wax
Soap and stearic acid flotation 38min, then through washing, being dried to obtain material B；Wherein, the oxidized paraffin wax soap that every liter of ore pulp adds
Quality is 1.6kg, and the stearic quality of every liter of ore pulp addition is 40g；
S3, material B carrying out two-section calcining, wherein, the temperature of a section calcining is 700 DEG C, and the time of a section calcining is
50min, the temperature of two section calcinings is 1000 DEG C, and the time of two section calcinings is 1.3h, is subsequently adding the oxalic acid solution that pH value is 2
In, wherein, material B is 1:8 with the volume ratio of oxalic acid solution, and ultrasonic 50min at 90 DEG C, through filtering, wash, being dried to obtain thing
Material C, wherein, ultrasonic power is 1500W；
S4, material C is added to the water it is configured to the suspension that mass fraction is 18wt%, add ammonium chloride, every liter of suspension
The quality of the ammonium chloride added in liquid is 20g, is heated to 70 DEG C with the power microwave of 1300W, stirs 20min, is subsequently adding matter
Measuring the salt acid for adjusting pH value that mark is 20wt% is 1, reacts 10min, is filtrated to get colloidal sol；Polyvinyl pyrrole is added in colloidal sol
Alkanone, tetramethylolmethane, stearic acid, wherein, the consumption of polyvinylpyrrolidone is the 0.3wt% of colloidal sol quality, tetramethylolmethane
The 0.3wt% that consumption is the 0.2wt% of colloidal sol quality, stearic consumption is colloidal sol quality, the pH value of regulation system is 3, so
Rear addition mass fraction be the salt acid for adjusting pH value of 20wt% be 1, ultrasonic 8min, filter, wash, be dried to obtain material D；
S5, be the hydrochloric acid of 30% by material D, sodium fluoride, sodium hydroxide, mass fraction, ATMP adds
During mix homogeneously is placed on hydrothermal reaction kettle in water, reacting 18h at 125 DEG C, wherein the quality of sodium fluoride is material D mass
4.5wt%, the quality of sodium hydroxide is the 2.1wt% of material D mass, and the quality of ATMP is material D mass
2wt%, mass fraction is the 12wt% that quality is material D mass of the hydrochloric acid of 30%；Reaction terminate after through cooling, filter,
Wash, be dried to obtain silicon dioxide.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope that the invention discloses, according to technical scheme and
Inventive concept equivalent or change in addition, all should contain within protection scope of the present invention.
Claims (8)
1. the separation method of silicon dioxide in a wollastonite raw ore, it is characterised in that comprise the following steps:
S1, add in ball mill after wollastonite crushing raw ore, the modulation that adds water, add grinding aid ball milling 20-50min, wherein, help
The quality of grinding agent is the 0.05-0.1wt% of wollastonite ore quality；Ball milling is 3000-4500kA/m in magnetic separation strength after terminating
Magnetic separator in carry out magnetic separation and obtain material A；
S2, material A being added water is configured to the ore pulp that concentration is 15-25wt%, and the pH value of regulation ore pulp is 8-10, adds oxidation stone
Wax soap and stearic acid flotation 20-45min, then through washing, being dried to obtain material B；Wherein, the oxidized paraffin wax that every liter of ore pulp adds
The quality of soap is 1-2kg, and the stearic quality of every liter of ore pulp addition is 30-50g；
S3, by material B calcine after add pH value be 1-3 oxalic acid solution in, wherein, material B with the volume ratio of oxalic acid solution is
1:6-10, ultrasonic 30-80min at 80-95 DEG C, through filtering, wash, be dried to obtain material C, wherein, ultrasonic power is
1000-2000W；
S4, material C is added to the water it is configured to the suspension that mass fraction is 15-20wt%, add ammonium chloride, every liter of suspension
The quality of the ammonium chloride of middle addition is 10-25g, and microwave heating, to 60-80 DEG C, stirs 10-25min, is subsequently adding hydrochloric acid regulation
PH value is 0.6-1.2, reacts 5-15min, is filtrated to get colloidal sol；Surfactant, wherein, surfactant is added in colloidal sol
The 0.5-1wt% that consumption is colloidal sol quality, the pH value of regulation system is 3-4, and being subsequently adding salt acid for adjusting pH value is 0.6-
1.2, ultrasonic 5-10min, filter, wash, be dried to obtain material D；
S5, it is that the hydrochloric acid of 25-35%, ATMP add water by material D, sodium fluoride, sodium hydroxide, mass fraction
Middle mix homogeneously is placed in hydrothermal reaction kettle, reacts 15-20h at 100-135 DEG C, and wherein the quality of sodium fluoride is material D
The 3-6wt% of quality, the quality of sodium hydroxide is the 1-2.5wt% of material D mass, and the quality of ATMP is thing
The 1-2.5wt% of material D mass, mass fraction is the 4-15wt% that quality is material D mass of the hydrochloric acid of 25-35%；Reaction knot
Shu Houjing cools down, filters, washs, is dried to obtain silicon dioxide.
The separation method of silicon dioxide in wollastonite raw ore the most according to claim 1, it is characterised in that in S1, by silicon
During lime stone crushing raw ore, it is crushed to particle diameter≤0.5mm.
The separation method of silicon dioxide in wollastonite raw ore the most according to claim 1 or claim 2, it is characterised in that in S1, institute
State grinding aid be isoamyl alcohol, sodium stearate, sodium naphthenate, cycloalkylsulfonic acid sodium, sodium chloride, dodecylbenzene sodium sulfonate, 18
One or more mixture in amine, manganese dioxide, amyl acetate.
4. according to the separation method of silicon dioxide in wollastonite raw ore according to any one of claim 1-3, it is characterised in that
In S1, magnetic separation strength is 3500-4000kA/m, and feed ore concentration is 30-40wt%, and rotating speed is 150-180r/min.
5. according to the separation method of silicon dioxide in wollastonite raw ore according to any one of claim 1-3, it is characterised in that
In S3, described calcining is two-section calcining, and the temperature of a section calcining is 600-800 DEG C, and the time of a section calcining is 30-60min, two
The temperature of section calcining is 950-1200 DEG C, and the time of two section calcinings is 1-1.5h.
6. according to the separation method of silicon dioxide in wollastonite raw ore according to any one of claim 1-5, it is characterised in that
In S4, the power of microwave heating is 1000-1500W.
7. according to the separation method of silicon dioxide in wollastonite raw ore according to any one of claim 1-6, it is characterised in that
In S4, the mass fraction of hydrochloric acid is 13-25wt%.
8. according to the separation method of silicon dioxide in wollastonite raw ore according to any one of claim 1-7, it is characterised in that
In S4, described surfactant be polyvinyl alcohol, Polyethylene Glycol, polyvinylpyrrolidone, tetramethylolmethane, stearic acid, citric acid,
One or more mixture in oleic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610382334.9A CN106044782A (en) | 2016-06-01 | 2016-06-01 | Method for separating silicon dioxide in wollastonite raw ore |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610382334.9A CN106044782A (en) | 2016-06-01 | 2016-06-01 | Method for separating silicon dioxide in wollastonite raw ore |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106044782A true CN106044782A (en) | 2016-10-26 |
Family
ID=57171812
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610382334.9A Pending CN106044782A (en) | 2016-06-01 | 2016-06-01 | Method for separating silicon dioxide in wollastonite raw ore |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106044782A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108069429A (en) * | 2017-12-25 | 2018-05-25 | 湖南省农产品加工研究所 | Preprocess method prepared by a kind of biomass silica-base material |
| CN110272058A (en) * | 2019-07-01 | 2019-09-24 | 中南大学 | A kind of MCM-41 ordered mesoporous material and preparation method thereof |
| CN112938989A (en) * | 2021-03-17 | 2021-06-11 | 江苏微纳光膜科技有限公司 | High-purity silicon dioxide for optical coating and preparation process thereof |
| CN113680463A (en) * | 2021-07-02 | 2021-11-23 | 中国科学院重庆绿色智能技术研究院 | Process control agent for improving binary optical absorbent composite efficiency |
| CN113684379A (en) * | 2021-08-30 | 2021-11-23 | 崇义章源钨业股份有限公司 | Method for decomposing wolframite concentrate and application |
| CN115092939A (en) * | 2022-06-16 | 2022-09-23 | 江西广源化工有限责任公司 | Preparation method of wollastonite powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539129A (en) * | 2013-10-30 | 2014-01-29 | 武汉大学 | Purification method of silicon dioxide |
-
2016
- 2016-06-01 CN CN201610382334.9A patent/CN106044782A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539129A (en) * | 2013-10-30 | 2014-01-29 | 武汉大学 | Purification method of silicon dioxide |
Non-Patent Citations (2)
| Title |
|---|
| 张银年等: "硅灰石矿提纯新工艺研究", 《矿产保护与利用》 * |
| 王延吉等: "硅灰石合成高比表面积多孔二氧化硅及其表征", 《华东地质学院学报》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108069429A (en) * | 2017-12-25 | 2018-05-25 | 湖南省农产品加工研究所 | Preprocess method prepared by a kind of biomass silica-base material |
| CN110272058A (en) * | 2019-07-01 | 2019-09-24 | 中南大学 | A kind of MCM-41 ordered mesoporous material and preparation method thereof |
| CN112938989A (en) * | 2021-03-17 | 2021-06-11 | 江苏微纳光膜科技有限公司 | High-purity silicon dioxide for optical coating and preparation process thereof |
| CN112938989B (en) * | 2021-03-17 | 2023-07-25 | 江苏微纳光膜科技有限公司 | High-purity silicon dioxide for optical coating and preparation process thereof |
| CN113680463A (en) * | 2021-07-02 | 2021-11-23 | 中国科学院重庆绿色智能技术研究院 | Process control agent for improving binary optical absorbent composite efficiency |
| CN113684379A (en) * | 2021-08-30 | 2021-11-23 | 崇义章源钨业股份有限公司 | Method for decomposing wolframite concentrate and application |
| CN115092939A (en) * | 2022-06-16 | 2022-09-23 | 江西广源化工有限责任公司 | Preparation method of wollastonite powder |
| CN115092939B (en) * | 2022-06-16 | 2024-04-09 | 江西广源化工有限责任公司 | Preparation method of wollastonite powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106044782A (en) | Method for separating silicon dioxide in wollastonite raw ore | |
| CN103194603B (en) | Preparation method of high-purity vanadium pentoxide | |
| CN100584755C (en) | With kaolin is the method for feedstock production superfine white carbon black and nano aluminium oxide | |
| CN101555551B (en) | Method for comprehensively recovering Fe, Cu and Si from copper smelting slag | |
| Yahui et al. | Preparation of rutile titanium dioxide pigment from low-grade titanium slag pretreated by the NaOH molten salt method | |
| CN107574711B (en) | Production method of titanium dioxide for decorative paper | |
| CN103754885B (en) | The method of porous silica is prepared in a kind of acidleach | |
| CN107447113A (en) | A kind of method that iron and aluminium are separated from red mud and/or iron content solid waste | |
| CN103643031A (en) | Method of mixing and roasting vanadium-containing material | |
| CN110358932A (en) | A kind of high silicate zinc concentrate hydrometallurgical processes | |
| CN102515221A (en) | Method for extracting alumina and amorphous silica from fly ash or coal gangue | |
| CN103088205A (en) | Beryllium oxide production process | |
| CN115216645A (en) | Method for extracting lithium from electrolytic aluminum waste slag by mixed salt calcination method | |
| CN103922396B (en) | The technique of rutile titanium white powder produced by a kind of low-grade titanium ore | |
| CN104512896B (en) | A kind of method utilizing aluminous fly-ash to prepare white carbon and white carbon | |
| CN106745318B (en) | A kind of method using iron vitriol slag one-step synthesis magnetic ferroferric oxide | |
| CN101607721B (en) | Method for preparing highly pure magnesium hydroxide and magnesium hexa-silicate by using olivine tailing mine | |
| CN105502426A (en) | Method for preparing water glass through extracting silicon oxide from chrysotile tailings by strong-base roasting method | |
| CN105936507B (en) | A method of utilizing wollastonite raw ore extraction of highly pure silica | |
| CN107640785B (en) | A kind of preparation method of plastic masterbatch titanium dioxide | |
| RU2236374C2 (en) | Silicon-containing binder preparation method | |
| CN107128975B (en) | A method of chromite prepares potassium bichromate crystal in microwave field | |
| CN101774648A (en) | Method for preparing high-purity iron oxide and trisodium phosphate by ferro-phosphorus alkalization process | |
| CN103787341A (en) | Method for producing white carbon black from obsidian | |
| CN111849207B (en) | Method for improving blue value of vanadium-zirconium blue pigment |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161026 |
|
| RJ01 | Rejection of invention patent application after publication |