A kind of high-dispersion white carbon black production equipment and production method
This case is the Application No. 201410279370.3 using the applying date as 2014-06-20, a kind of entitled " white carbon life
The divisional application that the patent of invention of production equipment and production method " is carried out for female case.
Technical field
The present invention relates to white carbon black production technical field, specifically a kind of high-dispersion white carbon black production equipment and producer
Method.
Background technology
Precipitated silica is typically that (most cases are to use sulphur for soluble silicate (typically using waterglass) and inorganic acid
Acid) under certain temperature and pH value, the hydrated SiO 2 precipitation of cocurrent chemosynthesis reaction generation is carried out, reaction equation is as follows:
Na2O·mSiO2+H2SO4→mSiO2·nH2O+Na2SO4
mSiO2·nH2O→mSiO2N ' H2O+ (n-n ') H2O↑
According to kinetics principle, there are two courses of reaction in precipitated silica reaction:First, it is that precipitated silica is brilliant
The generation of core and propagation process;2nd, the accumulation process of precipitated silica.At present, the general single shaft of precipitated silica reaction unit
Stirring, the intensity and effect of stirring is undesirable, according to precipitated silica reaction principle, when waterglass is with sulfuric acid reaction, sir
Into nucleus, the formation speed of nucleus, the solubility of nucleus, solution degree of supersaturation are production precipitated silica key control skills
Art, the intensity and effect stirred due to current single shaft reaction unit is undesirable, causes to occur during precipitated silica reaction synthesis
Some problem below:One, sulfuric acid and waterglass fail to be well mixed in time, and local pH is relatively low, the silicic acid for causing reaction to produce
Fail to be fully hydrolyzed in time, produce gel.Two, reaction paste mixing is uneven, and the silicon dioxide granule for causing reaction to generate is former
Level particle size is uneven, and offspring aggregation extent is different, and the spacial framework of white carbon is complicated, dispersed in rubber
Can be poor inadequate with physics reinforcement.Three, fail the gel for solving to produce when course of reaction and acidifying well, cause white carbon to make
Used time dispersive property is poor, physical property is poor in rubber compounding.
The content of the invention
In order to overcome the defect of above-mentioned prior art, it is white that the technical problems to be solved by the invention are to provide a kind of high dispersive
Carbon black production equipment and production method are to prepare the white carbon that gel is few, performance is good.
In order to solve the above-mentioned technical problem, the technical scheme for the high-dispersion white carbon black production equipment that the present invention is provided is:
Be provided with the top of a kind of high-dispersion white carbon black production equipment, including reaction vessel, the reaction vessel one with
On the first agitator, the side of the reaction vessel is provided with more than one second agitator, forms many main shafts and many sides
Axle stirring system;
First agitator includes the first motor, the first agitating shaft and the first agitating paddle, the first driving electricity
The drive end of machine connects first agitating shaft, and first agitating shaft is extended vertically into the reaction vessel, and described first stirs
Axle is mixed to be made up of along longitudinally connected the sub- agitating shaft of more than two, it is axially disposed on every sub- agitating shaft to have more than one institute
State and coupling piece is provided between the first agitating paddle, adjacent two sub- agitating shafts, the coupling piece includes upper bevel gear, middle bevel gear
With lower bevel gear, the upper bevel gear is horizontally disposed and is connected with the sub- agitating shaft of the top in adjacent two sub- agitating shafts, institute
State lower bevel gear to be horizontally disposed with and be connected with the sub- agitating shaft of the lower section in adjacent two sub- agitating shafts, the middle bevel gear is vertical
Set and be meshed respectively with upper bevel gear and lower bevel gear;
Second agitator includes the second motor, the second agitating shaft and the second agitating paddle, the second driving electricity
The drive end of machine connects second agitating shaft, and second agitating shaft is horizontally extended into the reaction vessel, and described second stirs
Mixing axially disposed on axle has more than one second agitating paddle;
Short transverse of second agitator along the reaction vessel is at least provided with two, on sustained height
At least two, second agitator and it is uniformly distributed along the circumference of the reaction vessel;The second agitator in two neighboring height
Stagger setting.
High-dispersion white carbon black production equipment provided by the present invention, has the advantages that:Stirring intensity is high, stirring effect
It is really good, the number of gels of white carbon can effectively be reduced using the high-dispersion white carbon black production equipment of the present invention, white carbon is improved
Dispersive property, obtain the rational white carbon of spacial framework so as to produce, gained white carbon compare ordinary precipitation process hard charcoal
It is black, have the advantages that number of gels is few, dispersive property is good, the physical property of rubber can be effectively improved and comprehensive performance.
In order to solve the above-mentioned technical problem, the technical scheme for the high-dispersion white carbon black production method that the present invention is provided is:
A kind of high-dispersion white carbon black production method, using high-dispersion white carbon black production equipment as described above, including it is following
Step:
Step 1, the deionized water for adding into reaction vessel 40~50 parts by volume are simultaneously heated to 90~95 DEG C;
Step 2, the first agitator of unlatching and the second agitator, the dodecane of 10~15 parts by weight is added into reaction vessel
The waterglass of base sodium sulphate and 1.8~2.5 parts by volume, the pH value for controlling solution is 7 ± 0.2;
Step 3, state is kept stirring for, adds the concentrated sulfuric acid simultaneously into reaction vessel and waterglass is reacted, the concentrated sulfuric acid
Addition speed for 0.685~0.85 parts by volume per hour, the addition speed of waterglass for 12~15 parts by volume per hour, reaction
When control solution pH value be 7 ± 0.2, the reaction time be 90~120min;
After the completion of step 4, reaction, state is kept stirring for, the sodium sulphate that 15~25 parts by weight are added into reaction vessel is stirred
10~20min is mixed, the addition concentrated sulfuric acid is then proceeded to and is acidified, the addition speed of the concentrated sulfuric acid is every small for 0.40~0.45 parts by volume
When, the pH value for being acidified to solution is 4~5;
After the completion of step 5, acidifying, stop stirring, the solution left standstill in reaction vessel is aged 30~60min, Ran Houyi
It is secondary by press filtration, washing, slurrying, spray drying, obtain white carbon;
Wherein, the parts by volume: parts by weight=m3∶kg。
High-dispersion white carbon black production method provided by the present invention, has the advantages that:Using the high score of the present invention
White carbon black production method is dissipated, can produce and obtain the rational white carbon of spacial framework, gained white carbon compares conventional precipitation
Method white carbon, with number of gels is few, dispersive property is good, can effectively improve the physical property of rubber and comprehensive performance etc. is excellent
Point.
Brief description of the drawings
Fig. 1 show the structural representation of the high-dispersion white carbon black production equipment of the embodiment of the present invention.
Label declaration:
1- reaction vessels;The agitators of 2- first;The agitators of 3- second;4- motor mounting platforms;The motors of 20- first;
The agitating shafts of 21- first;The agitating paddles of 22- first;The motors of 30- second;The agitating shafts of 31- second;The agitating paddles of 32- second.
Embodiment
To describe the technology contents of the present invention in detail, feature, the objects and the effects being constructed, below in conjunction with embodiment
And coordinate accompanying drawing to be explained in detail.
The design of most critical of the present invention is:Change the single shaft agitating mode that existing white carbon black production is used, use instead vertical
Stir and laterally stir the multiple agitating mode being combined, so as to improve the mixing uniformity of stirring intensity and reaction mass, carry
The intensity that laterally and longitudinally mixes of height, reaches each several part solution mixing uniformity, enables silicic acid that reaction generates abundant water in time
Solution generation silica, reduces the generation of gel, the silicon dioxide granule for hydrolyzing generation is small and uniform, offspring aggregation
It is easily opened scattered, the rational white carbon of spacial framework is obtained therefore, it is possible to produce, gained white carbon compares conventional precipitation
Method white carbon, with number of gels is few, dispersive property is good, can effectively improve the physical property of rubber and comprehensive performance etc. is excellent
Point.
Refer to shown in Fig. 1, the high-dispersion white carbon black production equipment of the present embodiment, including reaction vessel 1, the reaction appearance
The top of device 1 is provided with more than one first agitator 2, and the side of the reaction vessel 1 is provided with more than one second
Agitator 3;
First agitator 2 includes the first motor 20, the first agitating shaft 21 and the first agitating paddle 22, described first
The drive end of motor 20 connects first agitating shaft 21, and first agitating shaft 21 extends vertically into the reaction vessel 1
Interior, first agitating shaft 21 is made up of the sub- agitating shaft of more than two along longitudinally connected, is set vertically on every sub- agitating shaft
It is equipped between more than one first agitating paddle 22, adjacent two sub- agitating shafts and is provided with coupling piece, the coupling piece bag
Include bevel gear, middle bevel gear and lower bevel gear, the upper bevel gear it is horizontally disposed and with it is upper in adjacent two sub- agitating shafts
The sub- agitating shaft connection of side, the lower bevel gear is horizontally disposed with and connected with the sub- agitating shaft of the lower section in adjacent two sub- agitating shafts
Connect, the middle bevel gear is vertically arranged and is meshed respectively with upper bevel gear and lower bevel gear;
Second agitator 3 includes the second motor 30, the second agitating shaft 31 and the second agitating paddle 32, described second
The drive end of motor 30 connects second agitating shaft 31, and second agitating shaft 31 horizontally extends into the reaction vessel 1
It is interior, it is axially disposed on second agitating shaft 31 to have more than one second agitating paddle 32.
The operation principle of the high-dispersion white carbon black production equipment of the present invention is as follows:
During work, while opening the first agitator 2 and the second agitator 3, make the first agitator 2 to the molten of reaction vessel 1
Liquid carries out vertical stirring, and the second agitator 3 is laterally stirred to the solution of reaction vessel 1, stirs by vertical stirring and laterally
The mode being combined is mixed, the mixing in each orientation of multiaxis is carried out to the solution in reaction vessel, so that it is strong to greatly improve stirring
The mixing uniformity of degree and reaction mass.Further, since the first agitating shaft 21 by the sub- agitating shaft of more than two along longitudinally connected
Composition, adjacent two sub- agitating shafts are connected by coupling piece, and the coupling piece is using three bevel gears for being mutually perpendicular to engagement, both
Moment of torsion can be transmitted can change steering again, make adjacent two sub- agitating shafts are relative to rotate backward, therefore the first agitating shaft 21 can
To carry out increasingly complex vertical stirring to the solution in reaction vessel, the mixed of stirring intensity and reaction mass is further increased
Uniformity is closed, the pH value of each several part in reaction vessel is reached unanimity, it is to avoid local pH relatively low phenomenon, reaction generation
Silicic acid can be fully hydrolyzed generation silica in time, generate smaller and uniform precursor, and offspring aggregation is also easy
Open scattered, therefore effectively reduce the number of gels of white carbon, improve the dispersive property of white carbon.
It was found from foregoing description, the beneficial effect of high-dispersion white carbon black production equipment provided by the present invention is:Stirring
Intensity is high, and mixing effect is good, and the composite gel count of white carbon can be effectively reduced using the high-dispersion white carbon black production equipment of the present invention
Amount, improves the dispersive property of white carbon, the rational white carbon of spacial framework is obtained so as to produce, and gained white carbon is compared to general
Logical precipitated silica, with number of gels is few, dispersive property is good, can effectively improve the physical property of rubber and comprehensive usability
The advantages of energy.
Further, in the above-described embodiments, first agitator 2 has two or more, the first of described two above
Agitator 2 is evenly distributed on a concentric circles of the reaction vessel 1, and second agitator 3 is along the reaction vessel 1
Short transverse is at least provided with two, at least two, the second agitator 3 on sustained height and along the reaction vessel 1
Circumference be uniformly distributed.By above-mentioned improvement, mixing more multi-faceted, evenly can be carried out to the solution in reaction vessel and stirred
Mix, so as to further improve the mixing uniformity of stirring intensity and reaction mass, reach the number of gels for reducing white carbon, improve
The purpose of the properties of product of white carbon.Further, the second agitator 3 in two neighboring height staggers setting.So both
Can avoid the second agitator 3 on different height because easily beat oar and caused by damage, space can be made full use of to arrange again
The second more agitator 3, so as to further improve the mixing uniformity of stirring intensity and reaction mass, reaches that reduction is white
The number of gels of carbon black, improves the purpose of the properties of product of white carbon.
Further, in the above-described embodiments, first agitating paddle and the second agitating paddle are in cross.Criss-cross knot
Structure design can both ensure that the structural strength of agitating paddle is hardly damaged, and can provide higher stirring intensity again, reach preferably
Mixing effect.
Further, in the above-described embodiments, axial direction of first agitating paddle along the first agitating shaft is uniformly distributed, described
Axial direction of second agitating paddle along the second agitating shaft is uniformly distributed.So agitating shaft rotates more steady, and mixing effect is also more equal
It is even.
Further, in the above-described embodiments, in addition to motor mounting platform 4, second motor 30 is fixed on
On the motor mounting platform 4.
In summary, the high-dispersion white carbon black production equipment that the present invention is provided, stirring intensity is high, and mixing effect is good, structure
Intensity is high, stable and reliable operation, can effectively reduce the number of gels of white carbon, the dispersive property of white carbon is improved, using this hair
Bright white carbon black production equipment, which can be produced, obtains the rational white carbon of spacial framework, and gained white carbon compares conventional precipitation
Method white carbon, with number of gels is few, dispersive property is good, can effectively improve the physical property of rubber and comprehensive performance etc. is excellent
Point.
Please continue to refer to shown in Fig. 1, the high-dispersion white carbon black production method that the present invention is provided comprises the following steps:
Step 1, the deionized water for adding into reaction vessel 1 40~50 parts by volume are simultaneously heated to 90~95 DEG C;
Step 2, the first agitator 2 of unlatching and the second agitator 3, the ten of 10~15 parts by weight are added into reaction vessel 1
The waterglass of sodium dialkyl sulfate and 1.8~2.5 parts by volume, the pH value for controlling solution is 7 ± 0.2;
Step 3, state is kept stirring for, adds the concentrated sulfuric acid simultaneously into reaction vessel 1 and waterglass is reacted, the concentrated sulfuric acid
Addition speed for 0.685~0.85 parts by volume per hour, the addition speed of waterglass for 12~15 parts by volume per hour, reaction
When control solution pH value be 7 ± 0.2, the reaction time be 90~120min;
After the completion of step 4, reaction, state is kept stirring for, the sodium sulphate that 15~25 parts by weight are added into reaction vessel 1 is stirred
10~20min is mixed, the addition concentrated sulfuric acid is then proceeded to and is acidified, the addition speed of the concentrated sulfuric acid is every small for 0.40~0.45 parts by volume
When, the pH value for being acidified to solution is 4~5;
After the completion of step 5, acidifying, stop stirring, the solution left standstill in reaction vessel 1 is aged 30~60min, Ran Houyi
It is secondary by press filtration, washing, slurrying, spray drying, obtain white carbon;
Wherein, the parts by volume: parts by weight=m3∶kg。
The technological principle of the high-dispersion white carbon black production method of the present invention is as follows:
1st, by carrying out vertical stirring and lateral stirring simultaneously to the solution in reaction vessel, greatly improve stirring intensity and
The mixing uniformity of reaction mass, makes the pH value of each several part in reaction vessel reach unanimity, it is to avoid local pH is relatively low to be showed
As the silicic acid of reaction generation can be fully hydrolyzed generation silica in time, generate smaller and uniform precursor, offspring
Aggregation is also easily opened scattered, therefore effectively reduces the number of gels of white carbon, improves the dispersive property of white carbon;
2nd, by adding anion surfactant-lauryl sodium sulfate in reaction bottom water, anionic surface is utilized
Activating agent particle wraps up silica dioxide granule, and wetting action is carried out with the Hydrogenbond of silica dioxide granule, makes what hydrolysis was generated
Silicon dioxide granule is small and uniform, and the adhesion between silicon dioxide granule declines, and is easily opened in the presence of external force, so as to carry
The dispersive property of high white carbon;
3rd, addition sodium salt-sodium sulphate appropriate before acidifying is passed through, it is to avoid the pH value of reaction paste drastically declines during acidifying,
So as to prevent from producing substantial amounts of silicic acid during acidifying, and silicic acid can in time be fully hydrolyzed and generate small and uniform silicon dioxide granule,
Greatly reduce the generation of gel.
It was found from foregoing description, high-dispersion white carbon black production method provided by the present invention has the advantages that:Adopt
With the high-dispersion white carbon black production method of the present invention, it can produce and obtain the rational white carbon of spacial framework, gained hard charcoal
It is black to compare ordinary precipitation process white carbon, with number of gels is few, dispersive property is good, can effectively improve the physical property of rubber and comprehensive
The advantages of closing performance.
Further, in order to obtain more preferable properties of product, the modulus of the waterglass is 3.3~3.4, SiO2Content is
21~22wt%, transparency is more than 150mm.
Further, in order that reaction is more abundant, in step 3, the concentrated sulfuric acid and the waterglass cocurrent is added to reaction
Reacted in container.
The pH value of solution when further, in order to be more convenient to control to react, in step 3, keeps the addition speed of waterglass
Rate is constant, and the pH value that solution during reaction is controlled by adjusting the addition speed of the concentrated sulfuric acid is 7 ± 0.2.Increase when pH value is higher
The addition speed of the big concentrated sulfuric acid, the addition speed of the concentrated sulfuric acid is reduced when pH value is relatively low.
Embodiment 1
(1) waterglass is prepared:The modulus of waterglass is 3.30, SiO2Content is 21wt%, transparency > 150mm.
(2) first toward 90m340m is added in reaction vessel 13Water, be passed through saturated vapor, to reaction bottom water heat up;
95 DEG C are warming up to, the first agitator 2 is opened and the second agitator 3 starts stirring, then add 10kg lauryl sodium sulfate, then
Plus 1.8m3Waterglass, the pH value for determining solution is 7 ± 0.2;Cocurrent adds concentrated sulfuric acid 0.85m3/ h and waterglass 15m3/ h is carried out
Reaction, it is 7 ± 0.2 to control solution pH value during reaction, keeps the flow of waterglass constant, the concentrated sulfuric acid is increased when pH value is higher
Flow, when pH value is relatively low lower the concentrated sulfuric acid flow, the reaction time is 90min;Reaction terminates, and adds 20kg sodium sulphate and stirs
Mix 10min and continue the acidifying of enriching sulfuric acid, the flow of the concentrated sulfuric acid is controlled in 0.45m3/ h, the pH value for being acidified to solution is 4~5, after
Continuous ageing 30min.
(3) sheet frame material feeding washing, slurrying, spray drying, packaging.
Embodiment 2
(1) waterglass is prepared:The modulus of waterglass is 3.35, SiO2Content is 21.5wt%, transparency > 150mm.
(2) first toward 90m340m is added in reaction vessel 13Water, be passed through saturated vapor, to reaction bottom water heat up;
95 DEG C are warming up to, the first agitator 2 is opened and the second agitator 3 starts stirring, then add 10kg lauryl sodium sulfate, then
Plus 1.8m3Waterglass, the pH value for determining solution is 7 ± 0.2;Cocurrent adds concentrated sulfuric acid 0.685m3/ h and waterglass 12m3/ h is carried out
Reaction, it is 7 ± 0.2 to control solution pH value during reaction, keeps the flow of waterglass constant, the concentrated sulfuric acid is increased when pH value is higher
Flow, when pH value is relatively low lower the concentrated sulfuric acid flow, the reaction time is 120min;Reaction terminates, and adds 20kg sodium sulphate
Stir 10min and continue the acidifying of enriching sulfuric acid, the flow of the concentrated sulfuric acid is controlled in 0.40m3/ h, the pH value for being acidified to solution is 4~5,
Continue to be aged 45min.
(3) sheet frame material feeding washing, slurrying, spray drying, packaging.
Embodiment 3
(1) waterglass is prepared:The modulus of waterglass is 3.4, SiO2Content is 22.0wt%, transparency > 150mm.
(2) first toward 90m340m is added in reaction vessel 13Water, be passed through saturated vapor, to reaction bottom water heat up;
94 DEG C are warming up to, the first agitator 2 is opened and the second agitator 3 starts stirring, then add 10kg lauryl sodium sulfate, then
Plus 1.8m3Waterglass, the pH value for determining solution is 7 ± 0.2;Cocurrent adds concentrated sulfuric acid 0.715m3/ h and waterglass 12.5m3/ h enters
Row reaction, it is 7 ± 0.2 to control solution pH value during reaction, keeps the flow of waterglass constant, increases dense sulphur when pH value is higher
The flow of acid, lowers the flow of the concentrated sulfuric acid when pH value is relatively low, the reaction time is 90min;Reaction terminates, and adds 20kg sodium sulphate
Stir 10min and continue the acidifying of enriching sulfuric acid, the flow of the concentrated sulfuric acid is controlled in 0.45m3/ h, the pH value for being acidified to solution is 4~5,
Continue to be aged 60min.
(3) sheet frame material feeding washing, slurrying, spray drying, packaging.
By above-described embodiment 1~3 produce obtained white carbon carry out respectively performance detection and with the performance of other white carbons
Contrasted, comparing result is as shown in table 1 below:
The chemical index of table 1 is contrasted
By above-described embodiment 1~3 produce obtained white carbon be added separately to carry out detecting in rubber compounding and and other
The rubber compounding performance of white carbon is contrasted, and comparing result is as shown in table 2 below:
It was found from Tables 1 and 2, the number of gels of product that present invention production is obtained is close to the sub- product in French sieve ground, hence it is evident that
Less than the quantity of ordinary precipitation process white carbon, tensile strength and Akron abrasion all have very big than ordinary precipitation process white carbon
Lifting.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
Equivalent structure or equivalent flow conversion that bright specification and accompanying drawing content are made, or directly or indirectly it is used in other related skills
Art field, is included within the scope of the present invention.