A kind of white carbon black production equipment and production method
Technical field
The present invention relates to white carbon black production technical field, is a kind of white carbon black production equipment and production method specifically.
Background technology
Precipitated silica normally soluble silicate (generally using water glass) and mineral acid (most cases is with sulfuric acid) under certain temperature and pH value, carry out and flow chemosynthesis reaction generate hydrated SiO 2 precipitation, reaction formula is as follows:
Na
2O·mSiO
2+H
2SO
4→mSiO
2·nH
2O+Na
2SO
4
mSiO
2·nH
2O→mSiO
2·n'H
2O+(n-n')H
2O↑
According to reaction kinetics principle, precipitated silica reacts existence two reaction process: the generation and the propagation process that one, are precipitated silica nucleus; Two, the accumulation process of precipitated silica.At present, the general single shaft of precipitated silica reaction unit stirs, intensity and the effect of stirring are undesirable, according to precipitated silica reaction principle, when water glass and sulfuric acid reaction, first generate nucleus, the formation speed of nucleus, the solubleness of nucleus, solution degree of supersaturation produces precipitated silica key control technology, the intensity stirred due to current single shaft reaction unit and effect undesirable, cause during precipitated silica Reactive Synthesis and occur some problem following: one, sulfuric acid and water glass fail to mix in time, local pH is on the low side, the silicic acid causing reaction to produce fails fully to be hydrolyzed in time, produce gel.Two, reaction paste mixing is uneven, and the silicon dioxide granule precursor size causing reaction to generate is uneven, and offspring aggregation extent is different, and the spacial framework of white carbon black is complicated, in rubber dispersing property difference and physics reinforcement inadequate.Three, fail the gel produced when solving reaction process and acidifying well, cause white carbon black in use in poor, the rubber compounding of dispersing property physicals poor.
Summary of the invention
In order to overcome the defect of above-mentioned prior art, technical problem to be solved by this invention is to provide a kind of white carbon black production equipment and the production method white carbon black that gel is few to prepare, performance is good.
In order to solve the problems of the technologies described above, the technical scheme of white carbon black production equipment provided by the invention is:
A kind of white carbon black production equipment, comprise reaction vessel, the top of described reaction vessel is provided with more than one first agitator, and the side of described reaction vessel is provided with more than one second agitator, forms many main shafts and many side shafts stirring system;
Described first agitator comprises the first drive-motor, first stir shaft and the first stirring rake, the drive end of described first drive-motor connects described first stir shaft, described first stir shaft vertically stretches in described reaction vessel, described first stir shaft is longitudinally connected to form by the sub-stir shaft of more than two, every sub-stir shaft is provided with more than one described first stirring rake vertically, coupling piece is provided with between adjacent two sub-stir shafts, described coupling piece comprises cone gear, middle cone gear and lower cone gear, described upper cone gear is horizontally disposed with and is connected with the sub-stir shaft of the top in adjacent two sub-stir shafts, described lower cone gear is horizontally disposed with and is connected with the sub-stir shaft of the below in adjacent two sub-stir shafts, described middle cone gear vertically arranges and is meshed with upper cone gear and lower cone gear respectively,
Described second agitator comprises the second drive-motor, the second stir shaft and the second stirring rake, the drive end of described second drive-motor connects described second stir shaft, described second stir shaft level stretches in described reaction vessel, described second stir shaft is provided with vertically more than one described second stirring rake.
White carbon black production equipment provided by the present invention, there is following beneficial effect: stirring intensity is high, mixing effect is good, adopt white carbon black production equipment of the present invention effectively can reduce the number of gels of white carbon black, improve the dispersing property of white carbon black, thus produce and obtain the rational white carbon black of spacial framework, ordinary precipitation process white carbon black compared by gained white carbon black, has the advantage such as number of gels is few, dispersing property good, effectively can improve rubber physicals and comprehensive use properties.
In order to solve the problems of the technologies described above, the technical scheme of white carbon black production method provided by the invention is:
A kind of white carbon black production method, adopts white carbon black production equipment as above, comprises the following steps:
Step 1, add in reaction vessel 40 ~ 50 parts by volume deionized water and be heated to 90 ~ 95 DEG C;
Step 2, open the first agitator and the second agitator, add the sodium lauryl sulphate of 10 ~ 15 weight parts and the water glass of 1.8 ~ 2.5 parts by volume in reaction vessel, the pH value controlling solution is 7 ± 0.2;
Step 3, maintenance whipped state, add the vitriol oil and water glass reacts in reaction vessel simultaneously, the speed that adds of the vitriol oil is that 0.685 ~ 0.85 parts by volume is per hour, the speed that adds of water glass is that 12 ~ 15 parts by volume are per hour, the pH value controlling solution during reaction is 7 ± 0.2, and the reaction times is 90 ~ 120min;
Step 4, reacted after, keep whipped state, the sodium sulfate adding 15 ~ 25 weight parts in reaction vessel stirs 10 ~ 20min, then continues to add the vitriol oil and carries out acidifying, the speed that adds of the vitriol oil is that 0.40 ~ 0.45 parts by volume is per hour, and the pH value being acidified to solution is 4 ~ 5;
After step 5, acidifying complete, stop stirring, by the solution left standstill ageing 30 ~ 60min in reaction vessel, then successively by press filtration, washing, slurrying, spraying dry, obtain white carbon black;
Wherein, described parts by volume: weight part=m
3: kg.
White carbon black production method provided by the present invention, there is following beneficial effect: adopt white carbon black production method of the present invention, can produce and obtain the rational white carbon black of spacial framework, ordinary precipitation process white carbon black compared by gained white carbon black, has the advantage such as number of gels is few, dispersing property good, effectively can improve rubber physicals and comprehensive use properties.
Accompanying drawing explanation
Figure 1 shows that the structural representation of the white carbon black production equipment of the embodiment of the present invention.
Label declaration:
1-reaction vessel; 2-first agitator; 3-second agitator; 4-motor erecting stage; 20-first drive-motor; 21-first stir shaft; 22-first stirring rake; 30-second drive-motor; 31-second stir shaft; 32-second stirring rake.
Embodiment
By describing technology contents of the present invention, structural attitude in detail, realized object and effect, accompanying drawing is coordinated to be explained in detail below in conjunction with embodiment.
The design of most critical of the present invention is: change the single shaft alr mode that existing white carbon black production adopts, use vertical stirring instead and side direction stirs the multiple alr mode combined, thus improve the mixing uniformity of stirring intensity and reaction mass, improve the horizontal intensity with longitudinally mixing, reach each several part solution mixing uniformity, the silicic acid that reaction is generated can fully be hydrolyzed generation silicon-dioxide in time, reduce the generation of gel, the silicon dioxide granule that hydrolysis generates is little and even, offspring aggregate also easily opens dispersion, the rational white carbon black of spacial framework is obtained therefore, it is possible to produce, ordinary precipitation process white carbon black compared by gained white carbon black, there is number of gels few, dispersing property is good, effectively can improve the advantages such as the physicals of rubber and comprehensive use properties.
Refer to shown in Fig. 1, the white carbon black production equipment of the present embodiment, comprise reaction vessel 1, the top of described reaction vessel 1 is provided with more than one first agitator 2, and the side of described reaction vessel 1 is provided with more than one second agitator 3;
Described first agitator 2 comprises the first drive-motor 20, first stir shaft 21 and the first stirring rake 22, the drive end of described first drive-motor 20 connects described first stir shaft 21, described first stir shaft 21 vertically stretches in described reaction vessel 1, described first stir shaft 21 is longitudinally connected to form by the sub-stir shaft of more than two, every sub-stir shaft is provided with more than one described first stirring rake 22 vertically, coupling piece is provided with between adjacent two sub-stir shafts, described coupling piece comprises cone gear, middle cone gear and lower cone gear, described upper cone gear is horizontally disposed with and is connected with the sub-stir shaft of the top in adjacent two sub-stir shafts, described lower cone gear is horizontally disposed with and is connected with the sub-stir shaft of the below in adjacent two sub-stir shafts, described middle cone gear vertically arranges and is meshed with upper cone gear and lower cone gear respectively,
Described second agitator 3 comprises the second drive-motor 30, second stir shaft 31 and the second stirring rake 32, the drive end of described second drive-motor 30 connects described second stir shaft 31, described second stir shaft 31 level stretches in described reaction vessel 1, described second stir shaft 31 is provided with vertically more than one described second stirring rake 32.
The principle of work of white carbon black production equipment of the present invention is as follows:
During work, open the first agitator 2 and the second agitator 3 simultaneously, the solution of the first agitator 2 pairs of reaction vessels 1 is made to carry out vertical stirring, the solution of the second agitator 3 pairs of reaction vessels 1 carries out side direction stirring, the mode combined is stirred by vertical stirring and side direction, solution in reaction vessel is carried out to the mix and blend in each orientation of multiaxis, thus greatly improve the mixing uniformity of stirring intensity and reaction mass.In addition, because the sub-stir shaft of the first stir shaft 21 by more than two longitudinally connects to form, adjacent two sub-stir shafts are connected by coupling piece, described coupling piece utilizes the cone gear of three mutual Vertical Meshing, not only can transmitting torque but also can change turn to, adjacent two sub-stir shafts are rotated backward relatively, therefore the first stir shaft 21 can carry out more complicated vertical stirring to the solution in reaction vessel, further increase the mixing uniformity of stirring intensity and reaction mass, the pH value of each several part in reaction vessel is reached unanimity, avoid the phenomenon that local pH is on the low side, the silicic acid that reaction generates can fully be hydrolyzed generation silicon-dioxide in time, generate less and uniform precursor, offspring aggregate also easily opens dispersion, therefore the number of gels of white carbon black is effectively reduced, improve the dispersing property of white carbon black.
From foregoing description, the beneficial effect of white carbon black production equipment provided by the present invention is: stirring intensity is high, mixing effect is good, adopt white carbon black production equipment of the present invention effectively can reduce the number of gels of white carbon black, improve the dispersing property of white carbon black, thus produce and obtain the rational white carbon black of spacial framework, ordinary precipitation process white carbon black compared by gained white carbon black, has the advantage such as number of gels is few, dispersing property good, effectively can improve rubber physicals and comprehensive use properties.
Further, in the above-described embodiments, described first agitator 2 has two or more, described plural first agitator 2 is evenly distributed on a concentric(al) circles of described reaction vessel 1, described second agitator 3 is at least provided with two along the short transverse of described reaction vessel 1, and the second agitator 3 be positioned on sustained height has two at least and circumference along described reaction vessel 1 is uniformly distributed.By above-mentioned improvement, can to the solution in reaction vessel carry out more multi-faceted evenly mix and blend, thus improve the mixing uniformity of stirring intensity and reaction mass further, reach the number of gels reducing white carbon black, improve the object of the product performance of white carbon black.Further, the second agitator 3 on adjacent two height staggers setting.The second agitator 3 on different heights so both can have been avoided to cause damage because easily making oar, space can be made full use of again to arrange the second more agitator 3, thus improve the mixing uniformity of stirring intensity and reaction mass further, reach the number of gels reducing white carbon black, improve the object of the product performance of white carbon black.
Further, in the above-described embodiments, described first stirring rake and the second stirring rake are cruciform.Criss-cross structure design both can ensure that the structural strength of stirring rake was not fragile, can provide higher stirring intensity again, reach better mixing effect.
Further, in the above-described embodiments, described first stirring rake is uniformly distributed along the axis of the first stir shaft, and described second stirring rake is uniformly distributed along the axis of the second stir shaft.Such stir shaft rotates more steady, and mixing effect is also more even.
Further, in the above-described embodiments, also comprise motor erecting stage 4, described second drive-motor 30 is fixed on described motor erecting stage 4.
In sum, white carbon black production equipment provided by the invention, stirring intensity is high, and mixing effect is good, and structural strength is high, stable and reliable operation, effectively can reduce the number of gels of white carbon black, improve the dispersing property of white carbon black, adopt white carbon black production equipment of the present invention to produce and obtain the rational white carbon black of spacial framework, ordinary precipitation process white carbon black compared by gained white carbon black, has the advantage such as number of gels is few, dispersing property good, effectively can improve rubber physicals and comprehensive use properties.
Shown in Fig. 1, white carbon black production method provided by the invention, comprises the following steps:
Step 1, add in reaction vessel 1 40 ~ 50 parts by volume deionized water and be heated to 90 ~ 95 DEG C;
Step 2, open the first agitator 2 and the second agitator 3, add the sodium lauryl sulphate of 10 ~ 15 weight parts and the water glass of 1.8 ~ 2.5 parts by volume in reaction vessel 1, the pH value controlling solution is 7 ± 0.2;
Step 3, maintenance whipped state, add the vitriol oil and water glass reacts in reaction vessel 1 simultaneously, the speed that adds of the vitriol oil is that 0.685 ~ 0.85 parts by volume is per hour, the speed that adds of water glass is that 12 ~ 15 parts by volume are per hour, the pH value controlling solution during reaction is 7 ± 0.2, and the reaction times is 90 ~ 120min;
Step 4, reacted after, keep whipped state, the sodium sulfate adding 15 ~ 25 weight parts in reaction vessel 1 stirs 10 ~ 20min, then continues to add the vitriol oil and carries out acidifying, the speed that adds of the vitriol oil is that 0.40 ~ 0.45 parts by volume is per hour, and the pH value being acidified to solution is 4 ~ 5;
After step 5, acidifying complete, stop stirring, by the solution left standstill ageing 30 ~ 60min in reaction vessel 1, then successively by press filtration, washing, slurrying, spraying dry, obtain white carbon black;
Wherein, described parts by volume: weight part=m
3: kg.
The technological principle of white carbon black production method of the present invention is as follows:
1, by carrying out vertical stirring and side direction stirring to the solution in reaction vessel simultaneously, greatly improve the mixing uniformity of stirring intensity and reaction mass, the pH value of each several part in reaction vessel is reached unanimity, avoid the phenomenon that local pH is on the low side, the silicic acid that reaction generates can fully be hydrolyzed generation silicon-dioxide in time, and generate less and uniform precursor, offspring aggregate also easily opens dispersion, therefore effectively reduce the number of gels of white carbon black, improve the dispersing property of white carbon black;
2, by adding anion surfactant-sodium lauryl sulphate in reaction end water, anion surfactant particle is utilized to wrap up silica dioxide granule, wetting action is carried out with the hydrogen bonded of silica dioxide granule, the silicon dioxide granule that hydrolysis is generated is little and even, bonding force between silicon dioxide granule declines, easily open under the effect of external force, thus improve the dispersing property of white carbon black;
3, sodium salt-sodium sulfate is added by suitable before acidifying, the pH value of reaction paste during acidifying is avoided sharply to decline, thus produce a large amount of silicic acid when preventing acidifying, and silicic acid fully can be hydrolyzed in time and generates little and uniform silicon dioxide granule, greatly reduces the generation of gel.
From foregoing description, white carbon black production method provided by the present invention, there is following beneficial effect: adopt white carbon black production method of the present invention, can produce and obtain the rational white carbon black of spacial framework, ordinary precipitation process white carbon black compared by gained white carbon black, has the advantage such as number of gels is few, dispersing property good, effectively can improve rubber physicals and comprehensive use properties.
Further, in order to obtain better product performance, the modulus of described water glass is 3.3 ~ 3.4, SiO
2content is 21 ~ 22wt%, and transparency is greater than 150mm.
Further, in order to make reaction more abundant, in step 3, the described vitriol oil and water glass stream join in reaction vessel and react.
Further, in order to more convenient control reaction time solution pH value, in step 3, keep water glass to add speed constant, by regulate the vitriol oil add speed to control reaction time solution pH value be 7 ± 0.2.What increase the vitriol oil when pH value is higher adds speed, and that reduces the vitriol oil when pH value is on the low side adds speed.
Embodiment 1
(1) water glass is prepared: the modulus of water glass is 3.30, SiO
2content is 21wt%, transparency > 150mm.
(2) first toward 90m
340m is added in reaction vessel 1
3water, pass into saturated vapor, to reaction the end water heat up; Be warming up to 95 DEG C, open the first agitator 2 and the second agitator 3 and start to stir, then add 10kg sodium lauryl sulphate, then add 1.8m
3water glass, the pH value measuring solution is 7 ± 0.2; And stream adds vitriol oil 0.85m
3/ h and water glass 15m
3/ h reacts, and solution pH value when controlling reaction is 7 ± 0.2, and keep the flow of water glass constant, increase the flow of the vitriol oil when pH value is higher, lower the flow of the vitriol oil when pH value is on the low side, the reaction times is 90min; Reaction terminates, and add 20kg sodium sulfate and stir 10min continuation enriching sulfuric acid acidation, the flow control of the vitriol oil is at 0.45m
3/ h, the pH value being acidified to solution is 4 ~ 5, continues ageing 30min.
(3) sheet frame material feeding washing, slurrying, spraying dry, packaging.
Embodiment 2
(1) water glass is prepared: the modulus of water glass is 3.35, SiO
2content is 21.5wt%, transparency > 150mm.
(2) first toward 90m
340m is added in reaction vessel 1
3water, pass into saturated vapor, to reaction the end water heat up; Be warming up to 95 DEG C, open the first agitator 2 and the second agitator 3 and start to stir, then add 10kg sodium lauryl sulphate, then add 1.8m
3water glass, the pH value measuring solution is 7 ± 0.2; And stream adds vitriol oil 0.685m
3/ h and water glass 12m
3/ h reacts, and solution pH value when controlling reaction is 7 ± 0.2, and keep the flow of water glass constant, increase the flow of the vitriol oil when pH value is higher, lower the flow of the vitriol oil when pH value is on the low side, the reaction times is 120min; Reaction terminates, and add 20kg sodium sulfate and stir 10min continuation enriching sulfuric acid acidation, the flow control of the vitriol oil is at 0.40m
3/ h, the pH value being acidified to solution is 4 ~ 5, continues ageing 45min.
(3) sheet frame material feeding washing, slurrying, spraying dry, packaging.
Embodiment 3
(1) water glass is prepared: the modulus of water glass is 3.4, SiO
2content is 22.0wt%, transparency > 150mm.
(2) first toward 90m
340m is added in reaction vessel 1
3water, pass into saturated vapor, to reaction the end water heat up; Be warming up to 94 DEG C, open the first agitator 2 and the second agitator 3 and start to stir, then add 10kg sodium lauryl sulphate, then add 1.8m
3water glass, the pH value measuring solution is 7 ± 0.2; And stream adds vitriol oil 0.715m
3/ h and water glass 12.5m
3/ h reacts, and solution pH value when controlling reaction is 7 ± 0.2, and keep the flow of water glass constant, increase the flow of the vitriol oil when pH value is higher, lower the flow of the vitriol oil when pH value is on the low side, the reaction times is 90min; Reaction terminates, and add 20kg sodium sulfate and stir 10min continuation enriching sulfuric acid acidation, the flow control of the vitriol oil is at 0.45m
3/ h, the pH value being acidified to solution is 4 ~ 5, continues ageing 60min.
(3) sheet frame material feeding washing, slurrying, spraying dry, packaging.
Above-described embodiment 1 ~ 3 is produced the white carbon black obtained carry out Performance Detection respectively and contrast with the performance of other white carbon blacks, comparing result is as shown in table 1 below:
Table 1 chemical index contrasts
Above-described embodiment 1 ~ 3 is produced the white carbon black obtained to join respectively in rubber compounding and carry out detecting and contrast with the rubber compounding performance of other white carbon blacks, comparing result is as shown in table 2 below:
From table 1 and table 2, the present invention produces the number of gels of the product obtained close to the sub-product in French sieve ground, and be obviously less than the quantity of ordinary precipitation process white carbon black, tensile strength and Akron abrasion are all greatly improved than ordinary precipitation process white carbon black.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize specification sheets of the present invention and accompanying drawing content to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.