CN105236429A - Ultrahighly-dispersed white carbon black preparation method - Google Patents
Ultrahighly-dispersed white carbon black preparation method Download PDFInfo
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- CN105236429A CN105236429A CN201510585843.7A CN201510585843A CN105236429A CN 105236429 A CN105236429 A CN 105236429A CN 201510585843 A CN201510585843 A CN 201510585843A CN 105236429 A CN105236429 A CN 105236429A
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Abstract
The present invention discloses an ultrahighly-dispersed white carbon black preparation method, which comprises: dissolving sodium silicate and diluting, preparing a 4.5% dilute sulfuric acid solution, and adjusting the temperature to 70 DEG C; taking the prepared diluted sodium silicate solution, adding sodium sulfate powder, stirring to obtain a 75-85 DEG C mixing liquid so as to form a bottom material, adding the prepared sulfuric acid solution to the bottom material, and carrying out a reaction until the sodium silicate completely reacts to form a suspension; and carrying out pressure filtration on the suspension to obtain a filter cake, carrying out pulp beating on the filter cake, adding a machine surfactant LA-02 during the pulp beating process so as to change into a liquid state, and finally drying to obtain the ultrahighly-dispersed white carbon black. According to the present invention, the reaction microenvironment is changed, and the product has lipophilicity during the post-treatment process, such that the formed silica particles are small; and during the pulp beating process, the surface hydroxyl is effectively removed, and the dispersion of the produced white carbon black is higher than the dispersion of the existing highly-dispersed white carbon black.
Description
Technical field:
The present invention relates to technical field prepared by white carbon black, particularly relate to a kind of preparation method of super high-dispersion white carbon black.
Background technology:
White carbon black is lightweight hydrated SiO 2 material, exists with the micropore powder of amorphous state, is a kind of purposes important Chemicals widely.White carbon black specific surface area is larger, usually 130m2/g is greater than, powder particle has a large amount of microvoid structures, rich surface hydroxyl, have the characteristics such as good absorption, fire-retardant, insulation, suspension, thixotropy, thixotroping, scattering of light, surface-area modification, its remarkable strengthening action obtains important application at rubber item manufacture field.
High-dispersion white carbon black is the indispensable raw material of green tire; The concept of green tire rises in European Union, and present European several tire fashion enterprise is proposed requirements at the higher level--super high-dispersity white carbon black.
Particle soil boy structure during difference mainly the synthesizing of high-dispersion white carbon black and traditional white carbon black is different; The size of fundamental particle determines dispersed quality.In the preparation process of white carbon black, the size of particles determining white carbon black product from the size of collecting process and the polymerization degree of silicic acid molecule, product cut size is more little is more easy to dispersion.
Existing high-dispersion white carbon black solves the problem of the polymerization degree, makes fundamental particle much smaller than traditional white carbon black; But, also have two aspect Resolving probiems thorough not: a silicic acid fiercer from collecting process; B surface hydroxyl is abundanter; Cause manufacturing processed slightly to fluctuate, dispersiveness is just difficult to the requirement meeting high-end green tire.
Summary of the invention:
In order to make up prior art problem, the object of this invention is to provide a kind of preparation method of super high-dispersion white carbon black, on high-dispersion white carbon black basis, breakthrough change reaction microenvironment, makes the silicon-dioxide basis particle miniaturization more of formation; More effectively remove surface hydroxyl in pulping process, its dispersiveness has considerable raising.
Technical scheme of the present invention is as follows:
The preparation method of super high-dispersion white carbon black, is characterized in that, comprises the steps:
1), water glass dissolves: by sodium silicate solid Na
2o.nSiO2 and water 1:(1.5 ~ 2.5 in mass ratio) join in static pressure kettle, the steam passing into 0.4 ~ 0.6Mpa dissolves 2 ~ 2.5h, filters out liquid sodium silicate;
2), the dilution of water glass: the concentration of the rearrange liquids that adds water water glass, simultaneously according to specific surface area adjustment steam heating to 75 ~ 85 DEG C, the concentration of the liquid sodium silicate after adjustment is 14 ~ 18%;
3), the dilution of acid: preparation 4.0 ~ 5% dilution heat of sulfuric acid, adjust the temperature to 68 ~ 72 DEG C;
4), reaction: get and prepare rare sodium silicate solution 90 ~ 110 weight part, add the sodium sulfate powder of 10 ~ 15 weight parts and stir and obtain mixed solution in rare sodium silicate solution, this is bed material; According to specific surface area adjustment, be heated to temperature 75 ~ 85 DEG C; In the mixed solution obtained, add the sulphuric acid soln reaction prepared, and to stir, complete to water glass reaction, now reaction system is suspension;
5), press filtration: the suspension obtained is carried out press filtration, and the by products such as sodium sulfate are removed in washing, obtain filter cake;
6), making beating: filter cake is evenly delivered in hollander through belt and auger, adds organic surface active agent LA-0 according to the ratio of 0.08 ~ 0.25% simultaneously
2, filter cake becomes liquid under high velocity agitation;
7), dry: liquid white carbon black cake slurry through high-pressure spray-drying, and is collected with sack cleaner and obtains super high-dispersion white carbon black.
2, the preparation method of high-dispersion white carbon black according to claim 1, is characterized in that, comprises the steps:
1), water glass dissolves: by sodium silicate solid Na
2o.nSiO2 and water 1:(1.8 ~ 2 in mass ratio) join in static pressure kettle, the steam passing into 0.4 ~ 0.6Mpa dissolves 2 ~ 2.3h, filters out liquid sodium silicate;
2), the dilution of water glass: the concentration of the rearrange liquids that adds water water glass, simultaneously according to specific surface area adjustment steam heating to 75 ~ 85 DEG C, the concentration of the liquid sodium silicate after adjustment is 16 ~ 17%;
3), the dilution of acid: prepare 4.5% dilution heat of sulfuric acid, adjust the temperature to 70 DEG C;
4), react: get and prepare rare sodium silicate solution 100 weight part, in rare sodium silicate solution, add the sodium sulfate of 12 weight parts, stir and obtain mixed solution; According to specific surface area adjustment, be heated to temperature 75 ~ 85 DEG C; In the mixed solution obtained, add the sulphuric acid soln reaction prepared, and to stir, complete to water glass reaction during reaction soln PH=5.5, now reaction system is suspension;
5), press filtration: the suspension obtained is carried out press filtration, and the by products such as sodium sulfate are removed in washing, obtain filter cake;
6), making beating: filter cake is evenly delivered in hollander through belt and auger, adds organic surface active agent LA-0 according to the ratio of 0.1 ~ 0.2% simultaneously
2, filter cake becomes liquid under high velocity agitation;
7), dry: liquid white carbon black cake slurry through high-pressure spray-drying, and is collected with sack cleaner and obtains super high-dispersion white carbon black.
Advantage of the present invention is:
The present invention's breakthrough change reaction microenvironment, better makes product more have lipophilicity to make the silicon-dioxide basis particle miniaturization more of formation in aftertreatment; More effectively remove surface hydroxyl in pulping process, the white carbon black of output is dispersed higher than existing high-dispersion white carbon black.
Embodiment:
A preparation method for super high-dispersion white carbon black, comprises the steps:
1), water glass dissolves: by sodium silicate solid Na
2o.nSiO2 and water 1:(1.5 ~ 2.5 in mass ratio) join in static pressure kettle, the steam passing into 0.4 ~ 0.6Mpa dissolves 2 ~ 2.5h, filters out liquid sodium silicate;
2), the dilution of water glass: the concentration of the rearrange liquids that adds water water glass, simultaneously according to specific surface area adjustment steam heating to 75 ~ 85 DEG C, the concentration of the liquid sodium silicate after adjustment is 14 ~ 18%;
3), the dilution of acid: preparation 4.0 ~ 5% dilution heat of sulfuric acid, adjust the temperature to 68 ~ 72 DEG C;
4), reaction: get and prepare rare sodium silicate solution 90 ~ 110 weight part, add the sodium sulfate powder of 10 ~ 15 weight parts and stir and obtain mixed solution in rare sodium silicate solution, this is bed material; According to specific surface area adjustment, be heated to temperature 75 ~ 85 DEG C; In the mixed solution obtained, add the sulphuric acid soln reaction prepared, and to stir, complete to water glass reaction, now reaction system is suspension;
5), press filtration: the suspension obtained is carried out press filtration, and the by products such as sodium sulfate are removed in washing, obtain filter cake;
6), making beating: filter cake is evenly delivered in hollander through belt and auger, adds organic surface active agent LA-0 according to the ratio of 0.08 ~ 0.25% simultaneously
2, filter cake becomes liquid under high velocity agitation;
7), dry: liquid white carbon black cake slurry through high-pressure spray-drying, and is collected with sack cleaner and obtains super high-dispersion white carbon black.
The preparation method of high-dispersion white carbon black, comprises the steps:
1), water glass dissolves: by sodium silicate solid Na
2o.nSiO2 and water 1:(1.8 ~ 2 in mass ratio) join in static pressure kettle, the steam passing into 0.4 ~ 0.6Mpa dissolves 2 ~ 2.3h, filters out liquid sodium silicate;
2), the dilution of water glass: the concentration of the rearrange liquids that adds water water glass, simultaneously according to specific surface area adjustment steam heating to 75 ~ 85 DEG C, the concentration of the liquid sodium silicate after adjustment is 16 ~ 17%;
3), the dilution of acid: prepare 4.5% dilution heat of sulfuric acid, adjust the temperature to 70 DEG C;
4), reaction: get and prepare rare sodium silicate solution 100 weight part, add the sodium sulfate powder of 12 weight parts and stir and obtain mixed solution in rare sodium silicate solution, this is bed material; According to specific surface area adjustment, be heated to temperature 75 ~ 85 DEG C; In the mixed solution obtained, add the sulphuric acid soln reaction prepared, and to stir, complete to water glass reaction during reaction soln PH=5.5, now reaction system is suspension;
5), press filtration: the suspension obtained is carried out press filtration, and the by products such as sodium sulfate are removed in washing, obtain filter cake;
6), making beating: filter cake is evenly delivered in hollander through belt and auger, adds organic surface active agent LA-0 according to the ratio of 0.1 ~ 0.2% simultaneously
2, filter cake becomes liquid under high velocity agitation;
7), dry: liquid white carbon black cake slurry through high-pressure spray-drying, and is collected with sack cleaner and obtains super high-dispersion white carbon black.
As follows in the actual course of processing:
1), water glass dissolves: by sodium silicate solid Na
2o.nSiO2 and water 1:(1.8 ~ 2 in mass ratio) join in static pressure kettle, the size specification of static pressure kettle on product without impact, the steam passing into 0.4 ~ 0.6Mpa dissolves 2 ~ 2.3h, obtain liquid sodium silicate to need to remove impurity through precipitation and filtration, liquid silicic acid sodium content is not less than 30%;
2), the dilution of water glass: dilution adopts continuous mode, thinning tank is furnished with steam heater, temperature and proportion are by on-line monitoring device control, the concentration of the rearrange liquids that adds water in thinning tank water glass, adjust steam heating to 75 ~ 85 DEG C according to specific surface area, the concentration of the liquid sodium silicate after adjustment is 16 ~ 17% simultaneously; The suitable rare water glass of preparation is selected to pump into header tank, stand-by;
3), the dilution of acid: hot water and the vitriol oil fully mix in special mixing tank, its concentration regulates the additional proportion of water and acid to realize by on-line computing model, prepare 4.5% dilution heat of sulfuric acid, and temperature needs to be controlled by adjustment hot water temperature, and adjust the temperature to 70 DEG C;
4), react: reactor volume is 53m
3, prepare rare sodium silicate solution and add 30 tons from header tank, add 3.6 tons of sodium sulfate powders and stir and obtain mixed solution, this is bed material; Bed material is heated to need temperature (according to specific surface area adjustment), is generally heated to temperature 75 ~ 85 DEG C; Open acidifying, dilute sulphuric acid flow velocity is for ensureing that whole acidificatoin time is 65 ± 2min, and to stir, complete to water glass reaction during reaction soln PH=5.5, now reaction system is suspension;
It is all the factor affecting final white carbon black dispersiveness that rare sodium silicate silicate and temperature, dilute sulphuric acid concentration and temperature, the content of initial sodium sulfate, dilute sulphuric acid add speed, mixing speed and temperature of reaction, so the core of the reaction process whole technique that is the present invention;
5), press filtration: the suspension obtained is carried out press filtration, and the object of press filtration removes the moisture that can remove, and then removes sodium sulfate byproduct with clear water washing; Finally squeeze and again remove moisture;
6), making beating: filter cake is evenly delivered in making beating tank through belt and auger and passes through the mechanical force given by stirring, and adds organic surface active agent LA-0 according to the ratio of 0.1 ~ 0.2% simultaneously
2, portion of water is separated out, and pie becomes for dense fluids under high velocity agitation; The add-on of tensio-active agent is determined by the viscosity of underflow; The selection of tensio-active agent is another key point of the present invention;
7), dry: liquid white carbon black cake slurry is through high-pressure spray-drying, the pore size of spray gun, the pressure of high-pressure pump determine microballon size distribution, determine drying temperature and time of drying the weight loss on heating (free water content) of the finished product.
The precipitated silica obtained by above technological process, its physicals is as following table (with high-dispersion white carbon black HD165 as a comparison):
Project | Unit elongation % | 300% pulling force MPa | Tensile strength MPa | Dispersity (Alpha) |
HD165 | 452 | 13.66 | 20.4 | 98.1% |
Product innovation (the present invention) | 473 | 14.09 | 20.6 | 99.8% |
Remarks: HD165 is the high-dispersion white carbon black product of our company, and this result is the rubber testing data obtained under identical tire formulation, can find out: product innovation has more polymolecularity.
Claims (2)
1. a preparation method for super high-dispersion white carbon black, is characterized in that, comprises the steps:
1), water glass dissolves: by sodium silicate solid Na
2o.nSiO2 and water 1:(1.5 ~ 2.5 in mass ratio) join in static pressure kettle, the steam passing into 0.4 ~ 0.6Mpa dissolves 2 ~ 2.5h, filters out liquid sodium silicate;
2), the dilution of water glass: the concentration of the rearrange liquids that adds water water glass, simultaneously according to specific surface area adjustment steam heating to 75 ~ 85 DEG C, the concentration of the liquid sodium silicate after adjustment is 14 ~ 18%;
3), the dilution of acid: preparation 4.0 ~ 5% dilution heat of sulfuric acid, adjust the temperature to 68 ~ 72 DEG C;
4), reaction: get and prepare rare sodium silicate solution 90 ~ 110 weight part, add the sodium sulfate powder of 10 ~ 15 weight parts and stir and obtain mixed solution in rare sodium silicate solution, this is bed material; According to specific surface area adjustment, be heated to temperature 75 ~ 85 DEG C; In the mixed solution obtained, add the sulphuric acid soln reaction prepared, and to stir, complete to water glass reaction, now reaction system is suspension;
5), press filtration: the suspension obtained is carried out press filtration, and the by products such as sodium sulfate are removed in washing, obtain filter cake;
6), making beating: filter cake is evenly delivered in hollander through belt and auger, adds organic surface active agent LA-0 according to the ratio of 0.08 ~ 0.25% simultaneously
2, filter cake becomes liquid under high velocity agitation;
7), dry: liquid white carbon black cake slurry through high-pressure spray-drying, and is collected with sack cleaner and obtains super high-dispersion white carbon black.
2. the preparation method of high-dispersion white carbon black according to claim 1, is characterized in that, comprises the steps:
1), water glass dissolves: by sodium silicate solid Na
2o.nSiO2 and water 1:(1.8 ~ 2 in mass ratio) join in static pressure kettle, the steam passing into 0.4 ~ 0.6Mpa dissolves 2 ~ 2.3h, filters out liquid sodium silicate;
2), the dilution of water glass: the concentration of the rearrange liquids that adds water water glass, simultaneously according to specific surface area adjustment steam heating to 75 ~ 85 DEG C, the concentration of the liquid sodium silicate after adjustment is 16 ~ 17%;
3), the dilution of acid: prepare 4.5% dilution heat of sulfuric acid, adjust the temperature to 70 DEG C;
4), react: get and prepare rare sodium silicate solution 100 weight part, in rare sodium silicate solution, add the sodium sulfate of 12 weight parts, stir and obtain mixed solution; According to specific surface area adjustment, be heated to temperature 75 ~ 85 DEG C; In the mixed solution obtained, add the sulphuric acid soln reaction prepared, and to stir, complete to water glass reaction during reaction soln PH=5.5, now reaction system is suspension;
5), press filtration: the suspension obtained is carried out press filtration, and the by products such as sodium sulfate are removed in washing, obtain filter cake;
6), making beating: filter cake is evenly delivered in hollander through belt and auger, adds organic surface active agent LA-0 according to the ratio of 0.1 ~ 0.2% simultaneously
2, filter cake becomes liquid under high velocity agitation;
7), dry: liquid white carbon black cake slurry through high-pressure spray-drying, and is collected with sack cleaner and obtains super high-dispersion white carbon black.
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CN106829975A (en) * | 2017-03-08 | 2017-06-13 | 福建正盛无机材料股份有限公司 | A kind of preparation method of green tire high-dispersion white carbon black |
CN107324343A (en) * | 2017-06-15 | 2017-11-07 | 确成硅化学股份有限公司 | A kind of high preparation method for stretching high dispersive hydrated SiO 2 surely |
CN107603281A (en) * | 2017-09-14 | 2018-01-19 | 枣庄矿业(集团)有限责任公司蒋庄煤矿 | A kind of fast preparation method with white carbon black modified by silane coupling agent |
CN107720763A (en) * | 2017-11-21 | 2018-02-23 | 广州市飞雪材料科技有限公司 | A kind of preparation method of high dispersive silica |
CN108584967A (en) * | 2018-06-25 | 2018-09-28 | 蚌埠市万科硅材料科技有限公司 | A kind of preparation method of white carbon |
CN108928827A (en) * | 2018-06-22 | 2018-12-04 | 确成硅化学股份有限公司 | A method of improving white carbon black specific surface area and Kong Rong |
CN110150272A (en) * | 2019-06-05 | 2019-08-23 | 确成硅化学股份有限公司 | A kind of dedicated white carbon black of farm chemical carrier and preparation method thereof |
CN111153412A (en) * | 2020-01-15 | 2020-05-15 | 河南省睿博环境工程技术有限公司 | White carbon black production flow based on filtering washing liquid and sodium sulfate cyclic utilization |
CN113336235A (en) * | 2021-06-30 | 2021-09-03 | 确成硅化学股份有限公司 | Preparation method of high-dispersion white carbon black special for high-controllability tire |
CN113401914A (en) * | 2021-07-01 | 2021-09-17 | 确成硅化学股份有限公司 | Preparation method of high-dispersion white carbon black special for high-fatigue-resistance tire |
CN114873597A (en) * | 2022-05-23 | 2022-08-09 | 福建远翔新材料股份有限公司 | Preparation method of high-dispersion hydrated silicon dioxide for silicone rubber |
CN114956094A (en) * | 2021-02-24 | 2022-08-30 | 中国石油化工股份有限公司 | White carbon black nano dispersion liquid and preparation method and application thereof |
CN115321548A (en) * | 2022-08-15 | 2022-11-11 | 确成硅化学股份有限公司 | Preparation method of special high-dispersion white carbon black for new energy automobile tire |
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CN111153412A (en) * | 2020-01-15 | 2020-05-15 | 河南省睿博环境工程技术有限公司 | White carbon black production flow based on filtering washing liquid and sodium sulfate cyclic utilization |
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CN113336235A (en) * | 2021-06-30 | 2021-09-03 | 确成硅化学股份有限公司 | Preparation method of high-dispersion white carbon black special for high-controllability tire |
CN113401914A (en) * | 2021-07-01 | 2021-09-17 | 确成硅化学股份有限公司 | Preparation method of high-dispersion white carbon black special for high-fatigue-resistance tire |
CN114873597A (en) * | 2022-05-23 | 2022-08-09 | 福建远翔新材料股份有限公司 | Preparation method of high-dispersion hydrated silicon dioxide for silicone rubber |
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Application publication date: 20160113 |