CN108912742A - A kind of modified white carbon black preparation method - Google Patents
A kind of modified white carbon black preparation method Download PDFInfo
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- CN108912742A CN108912742A CN201810573443.8A CN201810573443A CN108912742A CN 108912742 A CN108912742 A CN 108912742A CN 201810573443 A CN201810573443 A CN 201810573443A CN 108912742 A CN108912742 A CN 108912742A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/3081—Treatment with organo-silicon compounds
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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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
- C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/16—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The present invention relates to white carbon black technical fields, and in particular, to a kind of modified white carbon black preparation method includes the following steps：S1：Sodium silicate solid is added in dissolver, water is added and is sealed dissolver, the stopping when steam pressure being passed through in steam to dissolver reaches 120~150cm mercury column, after the dissolution of whole sodium metasilicate, forming specific gravity is 1.36~1.38g/cm3Dilute sodium silicate solution, and above-mentioned dilute sodium silicate solution is put into reaction kettle, in this way, in modified white carbon black preparation method provided by the present application, sodium silicate solid is added in dissolver, water is added and seals dissolver, the steam pressure being passed through in steam to dissolver, the steam being passed through can accelerate the dissolution of sodium silicate solid, and the pressure value being passed through between 120~150cm when, can not only accelerating solid sodium metasilicate it is heated, improve molecular activity, shorten the dissolution period.
Description
Technical field：
The present invention relates to white carbon black technical fields, and in particular, to a kind of modified white carbon black preparation method.
Background technique：
White carbon black is the important supporting material of rubber industry, because its microstructure is similar with the morphology of the aggregate with carbon black, and
There is similar reinforcing property in rubber, therefore referred to as white carbon black.First generation white carbon black is traditional or is the white of " standard "
Kind of carbon black.The second generation is referred to as " high-performance reinforced white carbon black ", i.e. Hengsil-988 high-performance reinforced white carbon black, it is one
Kind has the novel supporting material for being suitable for green tire compared with polymolecularity.Energy-saving and environmental protection are the two principal themes of today's society.
In the prior art using during preparing white carbon black by precipitation method, production cost is higher, is mainly reflected in for waste water
Processing cost on, direct emission certainly will will cause environmental pollution, and not meet the theory of modernization industry, existing precipitating legal system
During standby white carbon black, complex procedures, not only energy consumption is high and ratio defective product is low, when preparing white carbon black by precipitation method, with the concentrated sulfuric acid plus silicon
Sour sodium reacts in a heated condition, then obtains finished product after the processes such as precipitating, filtering and drying and will form certain waste water, this is useless
Water is mainly produced in filtering water-washing process, this effluent part main polluted factors is pH, SS, and annual output is 5000 tons white
In process of production, the waste water for resulting from filtering washing reaches 53730m to carbon black3/ a, directly excluding in these waste water can be to environment
It causes damages, even more causes the waste of water resource, while also improving water consumption, increase and use water cost, and using filter press
When filtering out mother liquor, direct emission mother liquor be can cause environmental pollution.
Summary of the invention：
The application is to be solved to provide a kind of preparation method of modified white carbon black, and the solution prior art precipitation method prepare white
The problem that carbon black yield rate is low, pollution rate is high；
The application another the technical problem to be solved is that a kind of primary sedimentation basin is provided, solve waste water in the prior art
Processing cost is high, the big problem of processing difficulty；
The application another the technical problem to be solved is that a kind of secondary sedimentation tank is provided, realize the circulation benefit to waste water
With reduction production cost.
Technical problems to be solved in this application are implemented with the following technical solutions：A kind of preparation side of modified white carbon black
Method includes the following steps：
S1：Sodium silicate solid is added in dissolver, water is added and seals dissolver, is passed through steam to dissolution
Stopping when steam pressure in device reaches 120~150cm mercury column, after the dissolution of whole sodium metasilicate, is formed specific gravity for 1.36~
1.38g/cm3Dilute sodium silicate solution, and above-mentioned dilute sodium silicate solution is put into reaction kettle；
S2：It is 1.2~1.35g/cm that 98% concentrated sulfuric acid is slowly delivered to dilution in thinning tank to form specific gravity by pipeline3
Dilute sulfuric acid, the dilute sulfuric acid that above-mentioned preparation is formed is with 10~11m3/ h is delivered in reaction kettle, and controlling reaction temperature is 30
It is mixed at~32 DEG C, until standing progress aging in 1~3 hour and life when the pH value of solution in reaction kettle reaches 6.0~7.5
At crystal seed, then stirring forms mixed solution；
S3：High-temperature water vapor is passed through in the mixed solution of step S2 and is heated, when solution temperature heats in reaction kettle
When to 70~80 DEG C, stopping is passed through high-temperature water vapor, and additions specific gravity is 1.36~1.38g/cm3Dilute sodium metasilicate, work as reaction kettle
When interior pH value of solution is 11.0~11.5, stop that dilute sodium metasilicate is added；
S4：High-temperature water vapor is passed through in the solution after step S3 reaction again and is heated, when solution temperature in reaction kettle
When being heated to 88~94 DEG C, stopping is passed through high-temperature water vapor, and by 98% sulfuric acid with 0.52~0.7m3The flow rate of/h is added molten
In liquid, when the pH value of solution in reaction kettle is 3.0~5.0, synthesis terminates, and has sediment precipitation in reaction kettle；
S5：By sediment through filtering, mashing, the primary white carbon black of dry formation；
S6：The primary white carbon black normal hexane prepared in step S5 is fully dispersed, couplingization reagent is then added, in nothing
Under the conditions of water, it is stirred to react 6~48 hours with 20~80 DEG C；Reaction was completed, is successively washed with normal hexane, ethyl alcohol, with 30~200
DEG C drying；The molar ratio of primary white carbon black and couplingization reagent is 1:(0.01~0.1), wherein the couplingization reagent is six
Methyl disilazane.
Preferably, the sediment filtration step in the step S5 includes：Suspension after reacting in step S4 is used
Then plus water washing filter cake filter filters out mother liquor and recycles sodium sulphate, until detecting filtrate with to saturation barium hydroxide solution
Until without precipitating, filter cake blanking is dried up with compressed air.
It preferably, further include being recycled to the waste water after washing, including the waste water of generation will be filtered in step S5
It is delivered in sedimentation basin, and quick lime is added and is neutralized, the supernatant on sedimentation basin upper layer is delivered to step after precipitating
It recycles in S5, and will periodically be sold outside the calcium sulfate for precipitating formation in sedimentation basin dehydration.
In the application, the sedimentation basin includes primary sedimentation basin and secondary sedimentation tank, and the primary sedimentation basin upper end is equipped with
The first pipe of transport wastewater, primary sedimentation basin right end are equipped with feed inlet for launching quick lime, the first pipe into
The mouth of a river is arranged at the upper end of feed inlet, and primary sedimentation basin is equipped with secondary sedimentation tank far from the side of feed inlet, described secondary heavy
Shallow lake pond is connected to primary sedimentation basin via second pipe, and the supernatant liquor formed after primary sedimentation basin neutralization precipitation is delivered to secondary
Sedimentation basin, the secondary clear liquid in the upper layer that supernatant liquor is formed after secondary sedimentation tank precipitates again recycle.
Preferably, the primary sedimentation bottom of pond portion is equipped with landslide, and the landslide higher-end is arranged at feed inlet, come down compared with
Bottom end is arranged in bottom end of the primary sedimentation basin far from feed inlet side, the primary sedimentation basin close to the side of secondary sedimentation tank also
Equipped with the savings pond for collecting calcium sulfate, primary sedimentation basin is equipped with the valve being located at close to secondary sedimentation tank side.
Preferably, the landslide upper end is additionally provided with for waste water and quick lime to be directed in the middle part of primary sedimentation basin together
Guide channel.
Preferably, control switch is equipped on the first pipe and second pipe.
Preferably, also horizontal in the middle part of the secondary sedimentation tank to be equipped with drainage tube, the circumferential side wall of the drainage tube is equipped with logical
Hole, described drainage tube one end are connected to one end of second pipe.
In the application, buffer gear is additionally provided in the secondary sedimentation tank, the buffer gear is arranged in secondary sedimentation tank
Close to one end of second pipe, buffer gear includes plummer, and the plummer is connected firmly in secondary sedimentation tank close to second pipe
One end, plummer upper surface is disposed with convergence platform along secondary sedimentation tank side wall, and the carrying platform upper surface is far from
One end of two pipelines is additionally provided with baffler, and the baffler lower end is equipped with transfer passage, and the transfer passage is located at secondary precipitation
At the middle layer turbidity screen in pond.
Preferably, the convergence platform, group partition and plummer have been enclosed cushion chamber.
Preferably, it is additionally provided with tilting table in the cushion chamber, the whole rectangular triangular pyramidal shape of the tilting table, tilting table
Two right-angle sides be embedded in convergence platform and the right angle that is enclosed of plummer.
Preferably, the convergence platform and plummer are generally rectangular-shaped, on tilting table perpendicular to plummer and recline
It is the high length of 0.5~0.65 times of convergence platform in the length of the right-angle side of convergence platform.
Preferably, the secondary sedimentation tank is additionally provided with outlet far from one end of second pipe, and the outlet is located at two
The secondary clear liquid middle position in the upper layer of secondary sedimentation basin, the outlet are equipped with control switch.
Preferably, the step S5 recycles the step of sodium sulphate from mother liquor and includes：
T1：Concentration is evaporated to mother liquor, until the concentration of sodium sulphate reaches 25~30 Baume degrees；
T2：The metabisulfite solution secondary filter that concentration obtained in step T1 reaches 25~30 Baume degrees, which is obtained concentration, is
The sodium sulphate refined soln of 25~30 Baume degrees；
T3：The sodium sulphate refined soln that concentration is 25~30 Baume degrees is evaporated crystallization, anhydrous sodium sulfate is made；
T4：The anhydrous sodium sulfate that crystallization generates is separated by automatic discharge centrifuge, and mother liquor return continues concentration knot
It is brilliant.
Compared with prior art, the application has the beneficial effect that：
1, in modified white carbon black preparation method provided by the present application, sodium silicate solid is added in dissolver, is added
Water simultaneously seals dissolver, and the steam pressure being passed through in steam to dissolver, the steam being passed through can accelerate solid silicic acid
The dissolution of sodium, the and when pressure value being passed through is between 120~150cm, can not only accelerating solid sodium metasilicate it is heated, improve point
Sub- activity, shortens the dissolution period；
It 2, is that directly the concentrated sulfuric acid is diluted and then is delivered in reaction kettle again in the application, for the ease of control reaction
PH value in kettle controls dilute sulfuric acid conveying speed in 10~11m3/ h, can be accurately by reaction by lasting mixing
PH value in kettle control solved 6.0~7.5 in the prior art using pH in the Production of Silica by Precipitated Technology of sulfuric acid not
The problem of preferably controlling；
3, in the application, in order to improve the yield rate of traditional white carbon black, be in step s 4 directly by 98% sulfuric acid with
0.52~0.7m3The flow rate of/h is added in solution, and the concentrated sulfuric acid for being added 98% not only discharges a large amount of heat in the solution, reduces high
The usage amount of temperature steam, and the sulfuric acid is to release inside solution exothermic, solution can be made integrally to be heated evenly, and improves aging
Process and promotion high finished product rate, overcome the prior art to keep solution uneven heating even using dilute sulfuric acid, cause high-temperature vapor dosage
High and low yield rate problem；Primary white carbon black is modified processing simultaneously, the BET of white carbon black itself can be further enhanced
Specific surface area；
4, in the application, the waste water that generation is filtered in step S5 is delivered in sedimentation basin, and is added in quick lime progress
And processing reduces pollution of the waste water to environment so that the acidic materials in waste water are neutralized, and will after precipitating in the application
The supernatant on sedimentation basin upper layer is delivered in step S5 and recycles, and further improves the rate of recovery of waste water, is reducing waste water
On the basis of discharge amount, the use cost of the water in step S5 is reduced, further decreases production cost, while will periodically sink
The calcium sulfate dehydration that precipitating is formed in the pond of shallow lake is outer to sell, and recycles the calcium sulfate in waste water, turns waste into wealth, not only conforms with modern industry reason
It reads, the calcium sulfate sold can further decrease the cost of production white carbon black technique；
5, in the application, step S5 recycles sodium sulphate from mother liquor, is the waste heat of boiler tail gas using production high-temperature steam
It is concentrated by evaporation metabisulfite solution, reproduction anhydrous sodium sulfate not only takes full advantage of the energy, even more obtained anhydrous sodium sulfate；
6, primary sedimentation basin provided by the present application, is with the acidic materials in quick lime and in waste water and to generate calcium sulfate heavy
It forms sediment, achievees the purpose that reduce contaminated wastewater, primary sedimentation basin right end is equipped with the feed inlet for launching quick lime, first pipe
Water inlet is arranged at the upper end of feed inlet, quick lime be before not putting into primary sedimentation basin just and waste water come into full contact with it is mixed
It closes, the hot gas generated in reaction process is discharged directly at feed inlet, and sufficiently the waste liquid after reaction enters primary sedimentation basin
It is interior, it directly generates a large amount of thermal conductivities with waste water in this way, having evaded quick lime and causes lower rolling waterborne in primary sedimentation basin, precipitating effect
Fruit is poor, the long problem of sedimentation cycle；
7, in the application, primary sedimentation bottom of pond portion is equipped with landslide, and landslide higher-end is arranged at feed inlet, comes down compared with bottom end
Bottom end of the primary sedimentation basin far from feed inlet side is set, and the precipitating that waste water and quick lime reaction generate can be slided along landslide
Move to bottom end on the left of primary sedimentation basin, and and the cooperation of savings pond, calcium sulfate after precipitating can savings is slid by valve
In pond, calcium sulfate is avoided the primary sedimentation basin bottom deposit, bad processing the problem of；
8, in the application, primary sedimentation basin avoids waste water from putting into primary sedimentation basin band to further increase sedimentation effect
The interference come, landslide upper end are additionally provided with the guide channel for being directed to waste water and quick lime together in the middle part of primary sedimentation basin,
Waste water and quick lime reaction generate heat enter primary sedimentation basin in when, being limited in guide channel, waste water, quick lime with
And corresponding reactant is limited in guide channel the impact of waste water in primary sedimentation basin, will not interfere other than guide channel
Wastewater sedimentation elsewhere, and the output end of guide channel is located at primary sedimentation basin middle position, that is to say, that primary heavy
In the superposed layer in shallow lake pond, superposed layer upper layer is supernatant liquor, is delivered to the waste water at this, quick lime and reactant and is sunk
It forms sediment, it is ensured that supernatant liquor is interference-free, guarantees sedimentation effect；
9, in the application, in order to reduce contaminated wastewater, by supernatant liquor be delivered to secondary sedimentation tank carry out secondary precipitation, two
Waste water is equally divided into three layers in secondary sedimentation basin, the beds of precipitation including upper layer secondary clear liquid, intermediate superposed layer and lower layer, and two
The circumferential side wall of drainage tube in the middle part of secondary sedimentation basin is equipped with through-hole, which is exactly to be arranged at superposed layer, can be equipped with
Through-hole slowly supernatant liquor can be delivered in secondary sedimentation tank precipitate so that the secondary clear liquid of superposed layer and upper layer
It will not mix, reduce sedimentation effect；
10, in the application, in order to reduce from the primary sedimentation basin supernatant liquor that comes of conveying to being generated in secondary sedimentation tank
It impacts and influences, buffer structure is additionally provided in secondary sedimentation tank, buffer gear includes plummer, and it is logical that baffler lower end is equipped with conveying
Road, transfer passage are located at the middle layer superposed layer of secondary sedimentation tank, and the water come from primary sedimentation basin conveying is limited in a group partition
In the chamber being enclosed with secondary sedimentation tank, it will not be impacted to being generated in external secondary sedimentation tank, the supernatant liquor of inflow
Ensure that the secondary clear liquid in upper layer is interference-free via the middle layer superposed layer that transfer passage is delivered to secondary sedimentation tank, guarantees precipitating effect
Fruit；
11, in the application, convergence platform, group partition and plummer have been enclosed cushion chamber, the cushion chamber and remittance
Poly- platform combines and forms step-like structure, enters secondary sink to reduce supernatant liquor and fall in convergence platform and flow into transfer passage
The superposed layer problem in shallow lake pond, the sediment flowed into the supernatant liquor of convergence platform can slowly flow into slow along convergence platform surface
It rushes chamber and is deposited on secondary precipitation bottom of pond portion；
12, in the application, in order to play buffer function, so that supernatant liquor flows slowly into the superposed layer of secondary sedimentation tank,
Tilting table is additionally provided in cushion chamber, integrally rectangular triangular pyramidal shape, two right-angle sides of tilting table are embedded flat in convergence tilting table
The right angle that platform and plummer are enclosed, the sloping platform being equipped with not only reduce rushing when supernatant liquor enters cushion chamber
It hits, which will lead to the distribution at random of the sediment in supernatant liquor, extend the sedimentation time, reduce sedimentation effect, and can also
So that supernatant liquor is possessed the power for entering secondary sedimentation tank superposed layer, the sediment in supernatant liquor is avoided to accumulate in cushion chamber
It inside results in blockage, that is to say, that the sloping platform being equipped with enables to the sediment in supernatant liquor along sloping platform surface
Movement, when supernatant liquor enters superposed layer, the sediment in supernatant liquor can directly carry out precipitating and enter the beds of precipitation, and it is heavy to improve
Shallow lake effect.
Detailed description of the invention：
Fig. 1 is sedimentation basin structural schematic diagram of the present invention；
Fig. 2 is secondary sedimentation tank structural schematic diagram；
Fig. 3 is buffer gear structural schematic diagram；
Fig. 4 is buffer gear structural schematic diagram；
In figure：10~primary sedimentation basin；11~first pipe；12~feed inlet；13~supernatant liquor；14~landslide；15
~savings pond；16~valve；17~guide channel；18~drainage tube；20~secondary sedimentation tank；21~second pipe；22~on
The secondary clear liquid of layer；23~outlet；30~buffer gear；31~plummer；32~convergence platform；33~group partition；34~defeated
Send channel；35~cushion chamber；36~tilting table.
Specific embodiment：
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is furture elucidated.
Embodiment 1：
A kind of preparation method of modified white carbon black, includes the following steps：
S1：Sodium silicate solid is added in dissolver, water is added and seals dissolver, is passed through steam to dissolution
Stopping when steam pressure in device reaches 120cm mercury column, after the dissolution of whole sodium metasilicate, forming specific gravity is 1.37g/cm3It is dilute
Sodium silicate solution, and above-mentioned dilute sodium silicate solution is put into reaction kettle；
S2：It is 1.27g/cm that 98% concentrated sulfuric acid is slowly delivered to dilution in thinning tank to form specific gravity by pipeline3It is dilute
Sulfuric acid, the dilute sulfuric acid that above-mentioned preparation is formed is with 10.5m3/ h is delivered in reaction kettle, and is controlled mixed when reaction temperature is 31 DEG C
Stirring is closed, until standing progress aging in 2 hours when the pH value of solution in reaction kettle reaches 7 and generating crystal seed, then stirring forms mixed
Close solution；
S3：High-temperature water vapor is passed through in the mixed solution of step S2 and is heated, when solution temperature heats in reaction kettle
When to 75 DEG C, stopping is passed through high-temperature water vapor, and additions specific gravity is 1.37g/cm3Dilute sodium metasilicate, when the pH value of solution in reaction kettle
When being 11.25, stop that dilute sodium metasilicate is added；
S4：High-temperature water vapor is passed through in the solution after step S3 reaction again and is heated, when solution temperature in reaction kettle
When being heated to 91 DEG C, stopping is passed through high-temperature water vapor, and by 98% sulfuric acid with 0.61m3The flow rate of/h is added in solution, when anti-
When the pH value of solution in kettle being answered to be 4.0, synthesis terminates, and has sediment precipitation in reaction kettle；
S5：By sediment through filtering, mashing, the primary white carbon black of dry formation；
S6：The primary white carbon black normal hexane prepared in step S5 is fully dispersed, couplingization reagent is then added, in nothing
Under the conditions of water, it is stirred to react 6~48 hours with 20~80 DEG C；Reaction was completed, is successively washed with normal hexane, ethyl alcohol, with 30~200
DEG C drying；The molar ratio of primary white carbon black and couplingization reagent is 1:(0.01~0.1), wherein the couplingization reagent is six
Methyl disilazane.
Embodiment 2：
The present embodiment content and the content of embodiment 1 are essentially identical, and something in common repeats no more, the difference is that：Step
In rapid S1, sodium silicate solid is added in dissolver, water is added and seals dissolver, is passed through steam to dissolver
Stopping when interior steam pressure reaches 125cm mercury column, after the dissolution of whole sodium metasilicate, forming specific gravity is 1.37g/cm3Dilute silicic acid
Sodium solution, and above-mentioned dilute sodium silicate solution is put into reaction kettle.
Embodiment 3：
The present embodiment content and the content of embodiment 1 are essentially identical, and something in common repeats no more, the difference is that：Step
In rapid S1, sodium silicate solid is added in dissolver, water is added and seals dissolver, is passed through steam to dissolver
Stopping when interior steam pressure reaches 150cm mercury column, after the dissolution of whole sodium metasilicate, forming specific gravity is 1.37g/cm3Dilute silicic acid
Sodium solution, and above-mentioned dilute sodium silicate solution is put into reaction kettle.
Embodiment 4：
The present embodiment content and the content of embodiment 1 are essentially identical, and something in common repeats no more, the difference is that：Step
In rapid S1, sodium silicate solid is added in dissolver, water is added and seals dissolver, is passed through steam to dissolver
Stopping when interior steam pressure reaches 160cm mercury column, after the dissolution of whole sodium metasilicate, forming specific gravity is 1.37g/cm3Dilute silicic acid
Sodium solution, and above-mentioned dilute sodium silicate solution is put into reaction kettle.
Embodiment 5：
The present embodiment content and the content of embodiment 1 are essentially identical, and something in common repeats no more, the difference is that：Step
In rapid S1, sodium silicate solid is added in dissolver, water is added and seals dissolver, is passed through steam to dissolver
Stopping when interior steam pressure reaches 110cm mercury column.
It prepares the modified white carbon black to be formed to Examples 1 to 5 to test, test result is as shown in table 1：
Table 1
Embodiment 6：
The present embodiment content and 2 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that：Step
S4：High-temperature water vapor is passed through in the solution after step S3 reaction again and is heated, when solution temperature is heated to 91 in reaction kettle
DEG C when, stopping is passed through high-temperature water vapor, and by 98% sulfuric acid with 0.52m3The flow rate of/h is added in solution, when molten in reaction kettle
When the pH value of liquid is 4.0, synthesis terminates, and has sediment precipitation in reaction kettle.
Embodiment 7：
The present embodiment content and 2 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that：Step
S4：High-temperature water vapor is passed through in the solution after step S3 reaction again and is heated, when solution temperature is heated to 91 in reaction kettle
DEG C when, stopping is passed through high-temperature water vapor, and by 98% sulfuric acid with 0.61m3The flow rate of/h is added in solution, when molten in reaction kettle
When the pH value of liquid is 4.0, synthesis terminates, and has sediment precipitation in reaction kettle.
Embodiment 8：
The present embodiment content and 2 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that：Step
S4：High-temperature water vapor is passed through in the solution after step S3 reaction again and is heated, when solution temperature is heated to 91 in reaction kettle
DEG C when, stopping is passed through high-temperature water vapor, and by 98% sulfuric acid with 0.7m3The flow rate of/h is added in solution, when molten in reaction kettle
When the pH value of liquid is 4.0, synthesis terminates, and has sediment precipitation in reaction kettle.
Embodiment 9：
The present embodiment content and 2 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that：Step
S4：High-temperature water vapor is passed through in the solution after step S3 reaction again and is heated, when solution temperature is heated to 91 in reaction kettle
DEG C when, stopping is passed through high-temperature water vapor, and by 98% sulfuric acid with 0.4m3The flow rate of/h is added in solution, when molten in reaction kettle
When the pH value of liquid is 4.0, synthesis terminates, and has sediment precipitation in reaction kettle.
Embodiment 10：
The present embodiment content and 2 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that：Step
S4：High-temperature water vapor is passed through in the solution after step S3 reaction again and is heated, when solution temperature is heated to 91 in reaction kettle
DEG C when, stopping is passed through high-temperature water vapor, and by 98% sulfuric acid with 0.8m3The flow rate of/h is added in solution, when molten in reaction kettle
When the pH value of liquid is 4.0, synthesis terminates, and has sediment precipitation in reaction kettle.
Comparative example 1：
This comparative example is that application number CN201210476263.0 prepares the white carbon black to be formed.
The modified white carbon black that the preparation of embodiment 6~10 is formed is tested for the property, test result is as shown in table 2：
Table 2
Embodiment 11：
The present embodiment content and 6 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that：Such as Fig. 1
It is shown, it further include primary sedimentation basin 10,10 upper end of primary sedimentation basin is equipped with the first pipe 11 of transport wastewater, primary sedimentation basin 10
Right end is equipped with the feed inlet 12 for launching quick lime, and the water inlet of first pipe 11 is arranged at the upper end of feed inlet 12, and one
Secondary sedimentation basin 10 is equipped with secondary sedimentation tank 20, secondary sedimentation tank 20 and primary sedimentation basin 10 via the far from the side of feed inlet 12
Two pipelines 21 are connected to, and the supernatant liquor 13 formed after 10 neutralization precipitation of primary sedimentation basin is delivered to secondary sedimentation tank 20, and upper layer is clear
The secondary clear liquid 22 in the upper layer that liquid 13 is formed after secondary sedimentation tank 20 precipitates again recycles, in this way, provided by the present application one
Secondary sedimentation basin 10 is with the acidic materials in quick lime and in waste water and to generate calcium sulfate precipitation, and reaching reduces contaminated wastewater
Purpose, 10 right end of primary sedimentation basin are equipped with feed inlet 12 for launching quick lime, the water inlet setting of first pipe 11 into
At the upper end of material mouth 12, quick lime be before not putting into primary sedimentation basin 10 just and waste water come into full contact with mixing, reacted
The hot gas generated in journey is discharged directly at feed inlet 12, and sufficiently the waste liquid after reaction enters in primary sedimentation basin 10, in this way,
To evade quick lime directly to generate a large amount of thermal conductivities with waste water and cause lower rolling waterborne in primary sedimentation basin 10, sedimentation effect is poor,
The long problem of sedimentation cycle.
Embodiment 12：
As shown in Figure 1, the present embodiment content and 11 content of embodiment are essentially identical, something in common is no longer repeated, difference
Be in：10 bottom of primary sedimentation basin is equipped with landslide 14, and 14 higher-ends of landslide are arranged at feed inlet 12, and landslide 14 is set compared with bottom end
It sets in bottom end of the primary sedimentation basin 10 far from 12 side of feed inlet, primary sedimentation basin 10 is also set close to the side of secondary sedimentation tank 20
There is the savings pond 15 for collecting calcium sulfate, primary sedimentation basin 10 is equipped with the valve being located at close to 20 side of secondary sedimentation tank
16, in this way, 10 bottom of primary sedimentation basin is equipped with landslide 14 in the application, 14 higher-ends of landslide are arranged at feed inlet 12, landslide
14 are arranged in bottom end of the primary sedimentation basin 10 far from 12 side of feed inlet, the precipitating energy that waste water and quick lime reaction generate compared with bottom end
It is enough to slide onto 10 left side bottom end of primary sedimentation basin along landslide 14, and cooperate with savings pond 15, the calcium sulfate after precipitating can it
It is slid onto savings pond 15 by valve 16, avoids calcium sulfate 10 bottom deposit of primary sedimentation basin, bad processing the problem of.
Embodiment 13：
As shown in Figure 1, the present embodiment content and 12 content of embodiment are essentially identical, something in common is no longer repeated, difference
Be in：14 upper ends of coming down are additionally provided with guide channel for waste water and quick lime to be directed to the middle part of primary sedimentation basin 10 together
17, control switch is equipped on first pipe 11 and second pipe 21, in this way, in the application, primary sedimentation basin 10 is in order into one
Step improves sedimentation effect, avoids waste water investment 10 bring of primary sedimentation basin interference, 14 upper ends of landslide are additionally provided with for by waste water
It is directed to the guide channel 17 at 10 middle part of primary sedimentation basin together with quick lime, the heat that waste water and quick lime reaction generate is entering
When in primary sedimentation basin 10, it is limited in guide channel 17, waste water, quick lime and corresponding reactant are to primary sedimentation basin
The impact of waste water is limited in guide channel 17 in 10, and the waste water elsewhere other than guide channel 17 will not be interfered heavy
It forms sediment, and the output end of guide channel 17 is located at 10 middle position of primary sedimentation basin, that is to say, that the superposed layer of primary sedimentation basin 110
Interior, superposed layer upper layer is supernatant liquor 13, is delivered to the waste water at this, quick lime and reactant and is precipitated, it is ensured that on
Layer clear liquid 13 is interference-free, guarantees sedimentation effect.
Embodiment 14：
As shown in Figure 1, the present embodiment content and 13 content of embodiment are essentially identical, something in common is no longer repeated, difference
Be in：In the application, in order to reduce contaminated wastewater, supernatant liquor 13 is delivered to secondary sedimentation tank 20 and carries out secondary precipitation,
Waste water is equally divided into three layers in secondary sedimentation tank 20, including the heavy of upper layer secondary clear liquid 22, intermediate superposed layer and lower layer
Shallow lake layer, the circumferential side wall of the drainage tube 18 at 20 middle part of secondary sedimentation tank are equipped with through-hole, which is exactly to be arranged in superposed layer
Supernatant liquor 13 can slowly be delivered in secondary sedimentation tank 20 and precipitate by place, the through-hole that can be equipped with, so that suspending
Layer and the secondary clear liquid 22 in upper layer will not mix, and reduce sedimentation effect, specifically, side of the primary sedimentation basin 10 far from feed inlet 12
Equipped with secondary sedimentation tank 20, the secondary sedimentation tank 20 is connected to primary sedimentation basin 10 via second pipe 21, primary sedimentation basin
The supernatant liquor 13 formed after 10 neutralization precipitations is delivered to secondary sedimentation tank 20, and supernatant liquor 13 sinks again in secondary sedimentation tank 20
The secondary clear liquid 22 in the upper layer formed behind shallow lake recycles, also horizontal in the middle part of secondary sedimentation tank 20 to be equipped with drainage tube 18, drainage tube 18
Circumferential side wall be equipped with through-hole, 18 one end of drainage tube is connected to one end of second pipe 21.
Embodiment 15：
As shown in Fig. 2, the present embodiment content and 12 content of embodiment are essentially identical, something in common is no longer repeated, difference
Be in：Buffer gear 30 is additionally provided in secondary sedimentation tank 20, the setting of buffer gear 30 is in secondary sedimentation tank 20 close to the second pipe
The one end in road 21, buffer gear 30 include plummer 31, and plummer 31 is connected firmly in secondary sedimentation tank 20 close to second pipe 21
One end, 31 upper surface of plummer are disposed with convergence platform 32 along 20 side wall of secondary sedimentation tank, and 31 upper surface of carrying platform is separate
One end of second pipe 21 is additionally provided with baffler 33, and 33 lower end of baffler is equipped with transfer passage 34, and transfer passage 34 is located at secondary
At the superposed layer of sedimentation basin 20, in this way, in the application, it is right in order to reduce the supernatant liquor 13 to come from the conveying of primary sedimentation basin 10
Impact is generated in secondary sedimentation tank 20 and is influenced, buffer structure 30 is additionally provided in secondary sedimentation tank 20, and buffer gear 30 includes holding
Microscope carrier 31,33 lower end of baffler are equipped with transfer passage 34, and transfer passage 34 is located at the middle layer superposed layer of secondary sedimentation tank 20, from
The water that the conveying of primary sedimentation basin 10 comes is limited in the chamber that group partition 33 and secondary sedimentation tank 20 are enclosed, will not be external
Impact is generated in the secondary sedimentation tank 20 in portion, the supernatant liquor 13 of inflow is delivered to secondary sedimentation tank 20 via transfer passage 34
Middle layer superposed layer ensures that the secondary clear liquid 22 in upper layer is interference-free, guarantees sedimentation effect.
Embodiment 16：
As shown in figure 3, the present embodiment content and 15 content of embodiment are essentially identical, something in common is no longer repeated, difference
Be in：It further include that convergence platform 32, group partition 33 and plummer 31 have been enclosed cushion chamber 35, in this way, in the application,
Convergence platform 32, group partition 33 and plummer 31 have been enclosed cushion chamber 35, the cushion chamber 35 and convergence 32 knot of platform
Conjunction forms step-like structure, falls in convergence platform 32 to reduce supernatant liquor 13 and flows into transfer passage 34 into secondary precipitation
The superposed layer in pond 20 impacts big problem, and the sediment flowed into the supernatant liquor 13 of convergence platform 32 can be along convergence platform 32
Surface slowly flows into cushion chamber 35 and is deposited on 20 bottom of secondary sedimentation tank.
Embodiment 17：
As shown in figure 4, the present embodiment content and 16 content of embodiment are essentially identical, something in common is no longer repeated, difference
Be in：Tilting table 36, the whole rectangular triangular pyramidal shape of tilting table 36, two right angles of tilting table 36 are additionally provided in cushion chamber 35
While being embedded the right angle being enclosed in convergence platform 32 and plummer 31, platform 32 and the generally rectangle of plummer 31 are converged
Shape, on tilting table 36 perpendicular to plummer 31 and to stick on the length of the right-angle side of convergence platform 32 be 0.6 times of convergence platform
32 high length, secondary sedimentation tank 20 are additionally provided with outlet 23 far from one end of second pipe 21, and outlet 23 is located at secondary heavy
Secondary 22 middle position of clear liquid in the upper layer in shallow lake pond 20, outlet 23 are equipped with control switch, in this way, in the application, in order to rise
Tilting table is additionally provided in cushion chamber 35 to buffer function so that supernatant liquor 13 flows slowly into the superposed layer of secondary sedimentation tank 20
36, the whole rectangular triangular pyramidal shape of tilting table 36, two right-angle sides of tilting table 36 are embedded in convergence platform 32 and plummer 31
The right angle being enclosed, the sloping platform 36 being equipped with not only reduce impact when supernatant liquor 13 enters cushion chamber 35, should
Impact will lead to the sediment distribution at random in supernatant liquor 13, extend the sedimentation time, reduce sedimentation effect, and can also make
Layer clear liquid 13 possesses the power for entering 20 superposed layer of secondary sedimentation tank, and the sediment in supernatant liquor 13 is avoided to accumulate in buffering
It results in blockage in chamber 35, that is to say, that the sloping platform 36 being equipped with enables to the sediment in supernatant liquor 13 along inclination
35 apparent motion of platform, when supernatant liquor 13 enters superposed layer, the sediment in supernatant liquor 13 can directly be precipitated into
Enter the beds of precipitation, improves sedimentation effect.
Embodiment 18：
The present embodiment content and 17 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that：It is described
Step S5 recycles the step of sodium sulphate from mother liquor and includes：
T1：Concentration is evaporated to mother liquor, until the concentration of sodium sulphate reaches 27 Baume degrees；
T2：It is 27 waves that the metabisulfite solution secondary filter that concentration obtained in step T1 reaches 27 Baume degrees, which is obtained concentration,
The sodium sulphate refined soln of U.S. degree；
T3：The sodium sulphate refined soln that concentration is 27 Baume degrees is evaporated crystallization, anhydrous sodium sulfate is made；
T4：The anhydrous sodium sulfate that crystallization generates is separated by automatic discharge centrifuge, and mother liquor return continues concentration knot
It is brilliant.
Basic principles and main features and the features of the present invention of the invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement is both fallen in the range of claimed invention.The scope of protection of present invention is by appended claims
And its equivalent thereof.
Claims (4)
1. a kind of modified white carbon black preparation method, includes the following steps：
S1：Sodium silicate solid is added in dissolver, water is added and seals dissolver, is passed through steam to dissolver
Stopping when interior steam pressure reaches 120~150cm mercury column, after the dissolution of whole sodium metasilicate, is formed specific gravity for 1.36~
1.38g/cm3Dilute sodium silicate solution, and above-mentioned dilute sodium silicate solution is put into reaction kettle；
S2：It is 1.2~1.35g/cm that 98% concentrated sulfuric acid is slowly delivered to dilution in thinning tank to form specific gravity by pipeline3It is dilute
Sulfuric acid, the dilute sulfuric acid that above-mentioned preparation is formed is with 10~11m3/ h is delivered in reaction kettle, and controlling reaction temperature is 30~32
DEG C when be mixed, until the pH value of solution in reaction kettle, which when reaching 6.0~7.5, stands progress aging in 1~3 hour, simultaneously generates crystalline substance
Kind, then stirring forms mixed solution；
S3：High-temperature water vapor is passed through in the mixed solution of step S2 and is heated, when solution temperature is heated to 70 in reaction kettle
At~80 DEG C, stopping is passed through high-temperature water vapor, and addition specific gravity is 1.36~1.38g/cm3Dilute sodium metasilicate, when in reaction kettle
When pH value of solution is 11.0~11.5, stop that dilute sodium metasilicate is added；
S4：High-temperature water vapor is passed through in the solution after step S3 reaction again and is heated, when solution temperature heats in reaction kettle
When to 88~94 DEG C, stopping is passed through high-temperature water vapor, and by 98% sulfuric acid with 0.52~0.7m3Solution is added in the flow rate of/h
In, when the pH value of solution in reaction kettle is 3.0~5.0, synthesis terminates, and has sediment precipitation in reaction kettle；
S5：By sediment through filtering, mashing, the primary white carbon black of dry formation；
S6：The primary white carbon black normal hexane prepared in step S5 is fully dispersed, couplingization reagent is then added, in no water bar
Under part, it is stirred to react 6~48 hours with 20~80 DEG C；Reaction was completed, is successively washed with normal hexane, ethyl alcohol, dry with 30~200 DEG C
It is dry；The molar ratio of primary white carbon black and couplingization reagent is 1:(0.01~0.1).
2. modified white carbon black preparation method according to claim 1, which is characterized in that the sediment mistake in the step S5
Filtering step includes：Suspension after reacting in step S4 is filtered out into mother liquor with filter and recycles sodium sulphate, then plus is washed
Filter cake is washed, until with until saturation barium hydroxide solution detection filtrate is without precipitating, dries up filter cake blanking with compressed air.
3. modified white carbon black preparation method according to claim 1, which is characterized in that further include to the waste water after washing into
Row recycles, and including the waste water for filtering generation in step S5 to be delivered in sedimentation basin, and quick lime is added and carries out at neutralization
It manages, the supernatant on sedimentation basin upper layer is delivered in step S5 after precipitating and is recycled, and periodically will precipitate shape in sedimentation basin
At calcium sulfate dehydration outer sell.
4. modified white carbon black preparation method according to claim 1, which is characterized in that the couplingization reagent is hexamethyl
Disilazane.
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| CN109678165A (en) * | 2019-01-03 | 2019-04-26 | 山东联科科技股份有限公司 | A kind of preparation method of lutein carrier high adsorption silica |
| CN110003415A (en) * | 2019-04-18 | 2019-07-12 | 华北电力大学（保定） | A kind of inner core packing material and preparation method thereof for composite insulation cross arm |
| CN110294480A (en) * | 2019-07-19 | 2019-10-01 | 四川微松新材料有限公司 | A kind of liquid phase method white carbon black and preparation method thereof |
| CN115626649A (en) * | 2022-08-26 | 2023-01-20 | 三明市丰润化工有限公司 | Preparation method of feed white carbon black |
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