CN107804851A - The preparation method of white carbon - Google Patents
The preparation method of white carbon Download PDFInfo
- Publication number
- CN107804851A CN107804851A CN201711182993.9A CN201711182993A CN107804851A CN 107804851 A CN107804851 A CN 107804851A CN 201711182993 A CN201711182993 A CN 201711182993A CN 107804851 A CN107804851 A CN 107804851A
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- China
- Prior art keywords
- white carbon
- preparation
- absorption tower
- ammonolysis
- albite
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Classifications
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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
- C01B33/126—Preparation of silica of undetermined type
-
- 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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/186—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof from or via fluosilicic acid or salts thereof by a wet process
Abstract
The present invention relates to a kind of preparation method of white carbon, comprise the following steps：Albite decomposes：Albite, fluorite, 98% sulfuric acid are reacted under 100 DEG C~200 DEG C and self-generated pressure and obtain the gaseous products containing silicon fluoride；Gas absorbs：The gaseous products are led into hydrolysis generation hydrolyzate in absorption tower；Ammonolysis：The hydrolyzate is passed through ammonolysis kettle, pH value is adjusted by the method for adding ammoniacal liquor, ripening after neutralization, obtains dirty solution；Rough white carbon：The dirty solution is filtered, wash, drying, obtain white carbon crude product；Refined white carbon：The white carbon crude product and water are mixed, stirring so that ammonium fluoride is substantially soluble in water；Filtering, dry and pure white carbon is made.The above method is simple to operate, and equipment requirement is low, and has the advantages of energy-saving and environmental protection, cost is low.
Description
Technical field
The present invention relates to a kind of preparation method of white carbon, more particularly, to a kind of side using albite production of silica white
Method.
Background technology
White carbon is the general name of white powder X-ray amorphous silicic acid and silicate product, is primarily referred to as precipitating dioxy
SiClx, aerosil and superfine silicon dioxide gel, also including powdered synthetic aluminium silicate and calcium silicates etc..
The traditional preparation methods of white carbon mainly have two kinds of vapor phase method and the precipitation method.
Vapor phase method hydrolyzes the silica that smoke-like is made using silicon tetrachloride gas under Hydrogen Oxygen air-flow high temperature.Reaction
Formula is：SiCl4+2H2+O2=SiO2+4HCl；The advantages of vapor phase method, is reaction condition easy to control, and product purity is high, decentralization
High, particle is thin and is formed spherical, and surface hydroxyl is few, thus the nanometer with excellent reinforcement, thickening and thixotropic property and particle
Effect, its shortcoming are high expensives, are actually also exactly that this point limits its extensive use, therefore, at present such as rubber row
Industry, still largely using traditional precipitation method production of silica white.
The precipitation method, i.e., using soluble silicate and the method for inorganic acid neutralization-precipitation reaction come production of silica white.The precipitation method
Prepare that production technology, the equipment of white carbon are simple, and dispersant and raw material are easy to get, and flow is simple, and scale of investment is little, but energy consumption
Height, higher to environmental requirement, Product Activity is not high, and particle is difficult to control, and affinity is poor, and reinforcing property is low, and particle surface is hydrophilic
Bonding is serious, weakens the adhesion of product.With the continuous improvement of environmental consciousness, a large amount of losses of social resources, one is proposed
The low white carbon preparation method of kind energy-saving and environmental protection, cost, more seems with important positive effect.
The content of the invention
The present invention is in view of the shortcomings of the prior art, propose a kind of new method for preparing white carbon.
The technical solution adopted in the present invention is：A kind of preparation method of white carbon, comprises the following steps：
Albite decomposes：By albite, fluorite, 98% sulfuric acid according to 1：1.55~2.57：3.28~4.62 quality
Than mixing, and reaction obtains solid residue and the gaseous products containing silicon fluoride under 100 DEG C~200 DEG C and self-generated pressure；
Gas absorbs hydrolysis：The gaseous products containing silicon fluoride are led in I and II absorption tower successively, hydrolyzed
Obtain the hydrolyzate containing fluosilicic acid；
Ammonolysis：The hydrolyzate is passed through in ammonolysis kettle, pH value is adjusted by the method for adding ammoniacal liquor；It is old after neutralization
Change is handled, and obtains dirty solution；
Rough white carbon：By the dirty solution, it is transported in filter press and filters, obtain white carbon, dries, obtain after washing
White carbon crude product；
Refined white carbon：By the white carbon crude product and water according to less than or equal to 1：1 mass ratio is added in container, in temperature
Degree is stirred more than 1 hour more than or equal to 40 DEG C and under negative pressure state so that ammonium fluoride is substantially soluble in water；Filtering, dry, system
Obtain white carbon finished product.
Based on the preparation method of above-mentioned white carbon, the albite decomposition step includes：To institute at 100 DEG C~200 DEG C
State albite and the fluorite preheats 15 minutes~30 minutes, remove moisture therein, obtain dry albite and fluorite
Raw material；98% sulfuric acid is added to again to react 2 hours~5 hours in the albite and fluorite raw material of the drying and contained
Calcium sulfate, the solid residue of sodium sulphate and aluminum sulfate and the gaseous products containing silicon fluoride.In this step, the reaction temperature
Degree can be 100 DEG C, 150 DEG C, 180 DEG C, 200 DEG C, preferably 120 DEG C~200 DEG C；The reaction time is preferably 2.5 hours
~4 hours.
Based on the preparation method of above-mentioned white carbon, the gas, which absorbs hydrolysing step, to be included：
Led to after the gaseous products removing dust filter filtering in the first grade absorption tower through the first grade absorption tower
Middle absorbing liquid is absorbed, entered after hydrolysis in one-level concentrated phase collecting tank, and the concentrated phase thing that the one-level concentrated phase collecting tank is collected is transported to
Ammonolysis and ripening are carried out in ammonolysis kettle；
The liquid flooding that the one-level concentrated phase collecting tank is collected is returned the one-level through pump and inhaled to first order absorption circulating slot
Receive and continue to absorb in tower；
The tail gas come out by the first grade absorption tower enters the two-level absorption tower through absorbing liquid in the two-level absorption tower
Absorb, continue to hydrolyze, the liquid after the two-level absorption tower hydrolysis enters two level concentrated phase and absorbs groove, and the two level concentrated phase absorbs groove
The concentrated phase thing of collection, which is transported in the ammonolysis kettle, carries out ammonolysis and ripening；
Detect the fluorinion concentration in the silicate fluoride solution in the first order absorption circulating slot, the two level absorption cycle groove
When reaching 10mol/L, absorbing liquid reaches saturation, and the absorbing liquid is also transported in the ammonolysis kettle and carried out at ammonolysis and ageing
Reason；
Wherein, the absorbing liquid in the I and II absorption tower is respectively that the ethanol that mass concentration is 10%~30% is water-soluble
Liquid, hydrolysis temperature is respectively 70 DEG C~90 DEG C in the I and II absorption tower.
Based on the preparation method of above-mentioned white carbon, in the aminolysis step, the hydrolyzate is adjusted by adding ammoniacal liquor
PH value be 7~8.
Based on the preparation method of above-mentioned white carbon, in the aminolysis step, time of the ripening for 1 hour~
2 hours, the temperature control of the ripening was at 70 DEG C~85 DEG C.
Based on the preparation method of above-mentioned white carbon, in the step of refined white carbon, the white carbon crude product and institute
The mass ratio for stating water can be 1：1、1：2、1：3、1：4、1：5, it is preferable that the mass ratio of the white carbon crude product and the water is
1：2~5.
Based on the preparation method of above-mentioned white carbon, in the step of refined white carbon, the temperature can be 40 DEG C,
50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, it is preferable that the temperature is 50 DEG C~65 DEG C.
Based on the preparation method of above-mentioned white carbon, in the step of refined white carbon, the negative pressure is 10 pa~70
Pa, it is preferable that the negative pressure is 40 pas.
Based on the preparation method of above-mentioned white carbon, in the step of refined white carbon, institute is carried out by stirring vane
State and be stirred, the rotating speed of the stirring vane is 50 revs/min~350 revs/min, such as can be 50 revs/min, 100
Rev/min, 150 revs/min, 200 revs/min, 250 revs/min, 300 revs/min, 350 revs/min, it is preferable that it is described to stir
The rotating speed for mixing blade is 150 revs/min~350 revs/min.
Based on the preparation method of above-mentioned white carbon, in the step of refined white carbon, the mixing time can be 1
Hour, 1.5 hours, 2.0 hours, 2.5 hours, 3.0 hours, 3.5 hours, it is preferable that the mixing time be 2.0 hours~
3.5 hour.
Compared with prior art, the present invention utilizes the gaseous products warp containing silicon fluoride caused by albite decomposition reaction
Hydrolysis, ammonolysis reaction production of silica white, the complicated processes from solid phase separation are avoided, reduce environmental pollution；And utilize hard charcoal
Black not soluble in water and ammonium fluoride is dissolved in the characteristic of water, white carbon crude product is mixed with water again, while ammonium fluoride is recovered by filtration
The higher white carbon black product of purity is obtained, aforesaid operations are simple, cost is low, environmental pollution is small.The albite decomposition technique
For reaction temperature at 100 DEG C~200 DEG C, reaction condition is gentle, and the requirement to equipment is than relatively low, raising albite overall availability.
Embodiment
Below by embodiment, technical scheme is described in further detail.
Embodiment 1
The present embodiment provides a kind of preparation method of white carbon, comprises the following steps：
Albite decomposes：First albite and fluorite are preheated 30 minutes at 100 DEG C, adding 98% sulfuric acid makes three
Person reacts 5 hours under 100 DEG C and self-generated pressure, obtains the solid residue containing calcium sulfate, sodium sulphate and aluminum sulfate with containing
The gaseous products of silicon fluoride, wherein, albite, fluorite, the mass ratio of 98% sulfuric acid are 1：1.55：3.28 reaction principle
For：
CaF2+H2SO4=2HF+CaSO4,
2NaAlSi3O8+24HF+4H2SO4=Na2SO4+Al2 (SO4) 3+6SiF4 ↑+16H2O；
Gas absorbs hydrolysis：After the gaseous products removing dust filter is filtered, it is passed through in first grade absorption tower through institute
State the absorbing liquid in first grade absorption tower to absorb, after hydrolysis enter in one-level concentrated phase collecting tank, the one-level concentrated phase collecting tank is collected
Concentrated phase thing be transported in ammonolysis kettle and carry out ammonolysis and ripening, wherein, hydrolysis principle is：3SiF4+2H2O=
2H2SiF6+SiO2↓；The liquid flooding that the one-level concentrated phase collecting tank is collected is returned described to first order absorption circulating slot through pump
Continue to absorb in first grade absorption tower；The tail gas come out by the first grade absorption tower enters two-level absorption tower through the two-level absorption tower
In absorbing liquid absorb, continue to hydrolyze, the liquid after two-level absorption tower hydrolysis enters two level concentrated phase and absorbs groove, the two level
Concentrated phase absorbs the concentrated phase thing that groove is collected and is transported to progress ammonolysis and ripening in the ammonolysis kettle；The two level concentrated phase collecting tank
The liquid flooding of collection is returned in the two-level absorption tower through pump to two level absorption cycle groove and continues to absorb；Detect described one
When the fluorinion concentration in silicate fluoride solution in level absorption cycle groove, the two level absorption cycle groove reaches 10mol/L, absorb
Liquid reaches saturation, and the absorbing liquid is also transported in the ammonolysis kettle and carries out ammonolysis and ripening, wherein, described one, two
Absorbing liquid in level absorption tower is respectively the ethanol water that mass concentration is 20%, and temperature is hydrolyzed in the I and II absorption tower
Degree is respectively 75 DEG C；
Ammonolysis：The hydrolyzate is passed through ammonolysis kettle, pH value is adjusted by the method for adding ammoniacal liquor, makes pH=7.2；Neutralize
After, it is aged 1.5 hours under the conditions of 80 DEG C, obtains dirty solution；Reaction principle is：H2SiF6+6NH3+2H2O=6NH4F+
SiO2↓；
Rough white carbon：By the dirty solution, it is transported in filter press and filters, obtain white carbon, dries, obtain after washing
White carbon crude product；
Refined white carbon：By white carbon crude product and water according to 1：1 mass ratio is added in container, in 40 DEG C and 10 pa negative pressure
Under the conditions of, rotating vane is small with the mixed liquor of white carbon and water described in 350 revs/min of rotating speed Stirring, Stirring 1
When so that ammonium fluoride is substantially soluble in water；Filtering, dry and pure white carbon is made.
Embodiment 2
The present embodiment provides a kind of preparation method of white carbon, comprises the following steps：
Albite decomposes：The specific reality that the embodiment of the present embodiment step is decomposed with albite in embodiment 1
It is essentially identical to apply mode, difference is：The preheating temperature is 150 DEG C, and the preheating time is 20 minutes；The reaction temperature
For 150 DEG C, the reaction time is 3.5 hours；Wherein, albite, fluorite, the mass ratio of 98% sulfuric acid are 1：2：4；
Gas absorbs hydrolysis：The specific reality that the embodiment of the present embodiment step absorbs with gas in embodiment 1
It is essentially identical to apply mode, difference is：Hydrolysis temperature is respectively 80 DEG C in the I and II absorption tower；
Ammonolysis：Embodiment basic phase of the embodiment of the present embodiment step with ammonolysis in embodiment 1
Together, difference is：The hydrolyzate adjusts pH=7.4 with ammoniacal liquor, and digestion time is 2 hours, and Aging Temperature is controlled at 85 DEG C；
Rough white carbon：The embodiment of the present embodiment step is the same as the specific reality that white carbon is prepared in embodiment 1
It is identical to apply mode；
Refined white carbon：The embodiment of the present embodiment step is gone with ammonium fluoride in white carbon in embodiment 1
The embodiment removed is essentially identical, and difference is：The mass ratio of white carbon crude product and water is 1：3, temperature is 50 DEG C, negative pressure
For 40 pas, rotating speed is 150 revs/min, and mixing time is 2.0 hours.
Embodiment 3
The present embodiment provides a kind of preparation method of white carbon, comprises the following steps：
Albite decomposes：The specific reality that the embodiment of the present embodiment step is decomposed with albite in embodiment 1
It is essentially identical to apply mode, difference is：Pre-warmed temperature is 200 DEG C, and the pre-warmed time is 15 minutes；The temperature of reaction is
200 DEG C, the time of reaction is 2 hours；
Gas absorbs hydrolysis：The specific reality that the embodiment of the present embodiment step absorbs with gas in embodiment 1
It is essentially identical to apply mode, difference is：Temperature is respectively 85 DEG C in the I and II absorption tower；
Ammonolysis：Embodiment basic phase of the embodiment of the present embodiment step with ammonolysis in embodiment 1
Together, difference is：The hydrolyzate adjusts pH=7.7 with ammoniacal liquor, and digestion time is 1 hour, and Aging Temperature is controlled at 75 DEG C；
Rough white carbon：The embodiment of the present embodiment step is the same as the specific reality that white carbon is prepared in embodiment 1
It is identical to apply mode；
Refined white carbon：The embodiment of the present embodiment step is gone with ammonium fluoride in white carbon in embodiment 1
The embodiment removed is essentially identical, and difference is：The mass ratio of white carbon crude product and water is 1：5, temperature is 65 DEG C, negative pressure
For 70 pas, rotating speed is 50 revs/min, and mixing time is 3.5 hours.
Finally it should be noted that：The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof；To the greatest extent
The present invention is described in detail with reference to preferred embodiments for pipe, those of ordinary skills in the art should understand that：Still
The embodiment of the present invention can be modified or equivalent substitution is carried out to some technical characteristics；Without departing from this hair
The spirit of bright technical scheme, it all should cover among the claimed technical scheme scope of the present invention.
Claims (10)
1. a kind of preparation method of white carbon, comprises the following steps：
Albite decomposes：By albite, fluorite, 98% sulfuric acid according to 1：1.55~2.57：3.28~4.62 mass ratio mixes
Close, and reaction obtains solid residue and the gaseous products containing silicon fluoride under 100 DEG C~200 DEG C and self-generated pressure；
Gas absorbs hydrolysis：The gaseous products containing silicon fluoride are led in I and II absorption tower successively, hydrolysis obtains
Hydrolyzate containing fluosilicic acid；
Ammonolysis：The hydrolyzate is passed through in ammonolysis kettle, pH value is adjusted by the method for adding ammoniacal liquor；After neutralization at ageing
Reason, obtains dirty solution；
Rough white carbon：The dirty solution is transported in filter press and filtered, white carbon precipitation is obtained, dries, obtain after washing
White carbon crude product；
Refined white carbon：By the white carbon crude product and water according to less than or equal to 1：1 mass ratio is added in container, big in temperature
It is stirred under equal to 40 DEG C and negative pressure state more than 1 hour so that ammonium fluoride is substantially soluble in water；Filtering, dry, be made white
Carbon black finished product.
2. the preparation method of white carbon according to claim 1, it is characterised in that：The step of albite decomposes is wrapped
Include：The albite and fluorite are preheated 15 minutes~30 minutes at 100 DEG C~200 DEG C, moisture therein is removed, obtains
Dry albite and fluorite raw material；It is small that 98% sulfuric acid is added to reaction 2 in the albite and fluorite raw material of the drying
When~obtain within 5 hours the solid residue containing calcium sulfate, sodium sulphate, aluminum sulfate and ferric sulfate and the gas generation containing silicon fluoride
Thing.
3. the preparation method of white carbon according to claim 1, it is characterised in that：The gas absorbs the step of hydrolyzing and wrapped
Include：
Led to after the gaseous products removing dust filter filtering in the first grade absorption tower through being inhaled in the first grade absorption tower
Receive liquid to absorb, after hydrolysis enter in one-level concentrated phase collecting tank, the concentrated phase thing that the one-level concentrated phase collecting tank is collected is transported to ammonolysis
Ammonolysis and ripening are carried out in kettle；
The liquid flooding that the one-level concentrated phase collecting tank is collected returns the first grade absorption tower to first order absorption circulating slot through pump
In continue to absorb；
Absorbed by the tail gas that the first grade absorption tower comes out into the two-level absorption tower through absorbing liquid in the two-level absorption tower,
Continue to hydrolyze, the liquid after the two-level absorption tower hydrolysis enters two level concentrated phase and absorbs groove, and the two level concentrated phase absorbs groove and collected
Concentrated phase thing be transported in the ammonolysis kettle and carry out ammonolysis and ripening；
The fluorinion concentration detected in the silicate fluoride solution in the first order absorption circulating slot, the two level absorption cycle groove reaches
During 10mol/L, absorbing liquid reaches saturation, and the absorbing liquid is also transported in the ammonolysis kettle and carries out ammonolysis and ripening；
Wherein, the absorbing liquid in the I and II absorption tower be respectively mass concentration be 10%~30% ethanol water, institute
It is respectively 70 DEG C~90 DEG C to state hydrolysis temperature in I and II absorption tower.
4. the preparation method of white carbon according to claim 1, it is characterised in that：In the aminolysis step, by adding
The pH value for entering the ammoniacal liquor regulation hydrolyzate is 7~8.
5. the preparation method of white carbon according to claim 1, it is characterised in that：It is described old in the aminolysis step
The time for changing processing is 1 hour~2 hours, and the temperature control of the ripening is at 70 DEG C~85 DEG C.
6. the preparation method of white carbon according to claim 1, it is characterised in that：The refined white carbon the step of
In, the mass ratio of the white carbon crude product and the water is 1：1~5.
7. the preparation method of white carbon according to claim 1, it is characterised in that：The refined white carbon the step of
In, the temperature is 40 DEG C~65 DEG C.
8. the preparation method of white carbon according to claim 1, it is characterised in that：The refined white carbon the step of
In, the negative pressure is the pa of 10 pas~70.
9. the preparation method of the white carbon according to claim 1 or 8, it is characterised in that：In the step of the refined white carbon
In rapid, by stirring vane carry out described in be stirred, the rotating speed of the stirring vane is 50 revs/min~350 revs/min.
10. the preparation method of white carbon according to claim 9, it is characterised in that：The refined white carbon the step of
In, the mixing time is 1.0 hours~3.5 hours.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445219A (en) * | 2014-11-28 | 2015-03-25 | 嵩县中科孵化器有限公司 | Preparation method of white carbon black |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445219A (en) * | 2014-11-28 | 2015-03-25 | 嵩县中科孵化器有限公司 | Preparation method of white carbon black |
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