CN116514131A - Method for preparing surface hydrophobic superfine modified white carbon black by using hydroxyl silicone oil - Google Patents
Method for preparing surface hydrophobic superfine modified white carbon black by using hydroxyl silicone oil Download PDFInfo
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- CN116514131A CN116514131A CN202310094084.9A CN202310094084A CN116514131A CN 116514131 A CN116514131 A CN 116514131A CN 202310094084 A CN202310094084 A CN 202310094084A CN 116514131 A CN116514131 A CN 116514131A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 145
- 239000006229 carbon black Substances 0.000 title claims abstract description 139
- 125000002887 hydroxy group Chemical group [H]O* 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 53
- 229920002545 silicone oil Polymers 0.000 title claims abstract description 53
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 19
- 230000004048 modification Effects 0.000 claims abstract description 37
- 238000012986 modification Methods 0.000 claims abstract description 37
- 238000003756 stirring Methods 0.000 claims abstract description 34
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 20
- 238000012545 processing Methods 0.000 claims abstract description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims description 48
- 239000000047 product Substances 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 238000003825 pressing Methods 0.000 claims description 19
- 239000000428 dust Substances 0.000 claims description 17
- 239000012065 filter cake Substances 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 11
- 241000872198 Serjania polyphylla Species 0.000 claims description 9
- 238000007664 blowing Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000004537 pulping Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000001694 spray drying Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 22
- 238000004519 manufacturing process Methods 0.000 abstract description 16
- 238000010438 heat treatment Methods 0.000 abstract description 9
- 238000001556 precipitation Methods 0.000 abstract description 5
- 238000002715 modification method Methods 0.000 abstract description 4
- 239000003607 modifier Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 241000227425 Pieris rapae crucivora Species 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000005868 electrolysis reaction Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000004513 sizing Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000004115 Sodium Silicate Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000013040 rubber vulcanization Methods 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000010902 jet-milling Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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
- C01P2006/21—Attrition-index or crushing strength of granulates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Developing Agents For Electrophotography (AREA)
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Abstract
The invention discloses a modification method for preparing surface hydrophobic precipitation method superfine white carbon black by using hydroxyl silicone oil in a dry environment, which comprises the steps of firstly preparing common white carbon black by using water glass and concentrated sulfuric acid as raw materials under a precipitation method process, then processing the common white carbon black into superfine white carbon black by a pulverizer, and then mixing and stirring the superfine white carbon black and the hydroxyl silicone oil in a closed container and heating for a certain time to obtain the surface hydrophobic superfine white carbon black; the modification process only uses a small amount of hydroxyl silicone oil and is completed in a sealed environment, so that the production process is safer for operators and basically has no pollution to the environment; the preparation method has the advantages of higher production efficiency, easily available production raw materials and modifiers, energy conservation and environmental protection in the production process.
Description
Technical Field
The invention relates to the technical field of surface modified superfine white carbon black, in particular to a method for preparing surface hydrophobic modified superfine white carbon black by using hydroxyl silicone oil.
Background
White carbon black is a white, nontoxic and powdery compound obtained by taking solid sodium silicate and concentrated sulfuric acid as raw materials under specific conditions, and the chemical name is hydrated silicon dioxide. The polymer has excellent characteristics of porosity, high dispersibility, good chemical stability, high temperature resistance, no combustion, good electrical insulation and the like, and has wide application in the aspects of rubber, plastics, papermaking and the like. The superfine white carbon black is a white carbon black product with finer granularity, which is obtained by taking white carbon black as a master batch and carrying out jet milling or mechanical milling, and the granularity is generally more than or equal to 1200 meshes.
The white carbon black particles are easy to agglomerate due to abundant hydrogen bonds on the surfaces of the white carbon black particles, and are difficult to infiltrate and disperse in an organic phase. When used as a reinforcing agent in rubber, the rubber has poor compatibility with hydrocarbon rubber, a large amount of filling rubber has large viscosity, and the processability is deteriorated with the extension of storage time. After storage, the sizing material is hard to harden, difficult to extrude and poor in molding viscosity, and static electricity accumulation is easy to generate when the sizing material is filled, so that the application effect of the sizing material is influenced. Therefore, the white carbon black products are mostly subjected to surface modification treatment before industrial application, so as to improve the industrial application performance.
Chinese patent CN 115159534A discloses a surface modification method of white carbon black by precipitation method, comprising the following steps of (1) placing a prepared sodium silicate solution in a reaction kettle, heating the reaction kettle to a certain temperature, then slowly adding a dilute sulfuric acid solution under continuous stirring to react until the reaction is finished, obtaining a white carbon black crude product (2), adding a certain amount of surface modifier into the obtained white carbon black crude product, and stirring for a period of time; (3) And (3) filtering and pulping the product in the step (2), and then drying and crushing to obtain a white carbon black finished product. Chinese patent CN 114014326A discloses a method for modifying white carbon black. The method comprises the following steps: performing heat treatment on white carbon black, and then modifying; the temperature of the heat treatment is more than 120 ℃ and less than or equal to 800 ℃. According to the technical scheme, the surface hydrophobicity of the white carbon black is improved to a certain extent, the mechanical properties of the white carbon black are improved, but the problems are also solved, such as the processes of subsequent filtering, pulping, drying, crushing and the like are carried out after modification, so that the direct connection between the process and the modification degree of the final product is difficult to establish in the modification process, the modification process is difficult to control and optimize, the subsequent operation is carried out after modification, and the specific surface area of the white carbon black is inevitably changed after filtration and crushing, so that the previous modification effect is also influenced. And adding additional heat treatment will necessarily increase the process complexity and increase the production cost.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a modification method for preparing the surface hydrophobic precipitation method superfine white carbon black by using hydroxyl silicone oil in a dry environment, which can solve the technical problems by simple and energy-saving production process on the premise of ensuring the surface hydrophobic modification of the superfine white carbon black and using the hydroxyl silicone oil as an additive for being easily dispersed in organic substances (such as rubber, paint and the like).
The complete technical scheme of the invention comprises the following steps:
a method for preparing surface hydrophobic modified superfine white carbon black by using hydroxyl silicone oil comprises the following steps:
s1: preparing white carbon black by using water glass and concentrated sulfuric acid; the method specifically comprises the following steps:
s1.1, material conversion: dissolving water glass in hot water; the water glass is water-solubleThe density of the liquid is 1.2-1.4 g/cm 3 ；
S1.2 pretreatment: precipitating and filtering the water glass solution obtained in the step S1.1, and transferring the water glass solution into a high-level tank;
s1.3, white carbon black synthesis: simultaneously injecting concentrated sulfuric acid and the water glass solution obtained in the step S1.2 into a reaction kettle, wherein the flow ratio of the concentrated sulfuric acid to the water glass solution is 1:12-18;
s1.4, white carbon black filter pressing and washing: performing filter pressing washing on the mixture obtained in the step S1.3, monitoring the conductivity of washing water in the washing process until the conductivity of the washing water is less than 3.5 ms/cm, and blowing high-pressure air to a filter cake for 10-20 min; and the filter cake is dehydrated in the modes of central blowing, water squeezing and central blowing.
S1.5, pulping a filter cake: conveying the filter cake obtained after filter pressing and washing in the step S1.4 into a pulping tank by using a belt, and adding water for pulping, wherein the mass ratio of the filter cake to the water is 3.8-1.3:1;
s1.6, drying the product: and (3) conveying the slurry obtained in the step (S1.5) to a spray drying tower by a screw pump, and separating by a bag type dust collector after spray drying to obtain white carbon black.
S2: crushing the white carbon black obtained in the step S1; specifically, the finished product obtained in the step S1.6 is conveyed to a pulverizer through a pipeline by an air blower, subjected to superfine processing and separated by a bag type dust collector, and the superfine white carbon black is obtained.
S3: mixing and stirring the white carbon black crushed in the step S2 with hydroxyl silicone oil to obtain surface hydrophobic superfine white carbon black modified by the hydroxyl silicone oil; and (3) conveying the finished product obtained in the step (S2) to a modification stirrer through an air blower and a pipeline, mixing and stirring with hydroxyl silicone oil, and separating through a bag type dust collector to obtain the surface hydrophobic superfine white carbon black.
As a further scheme of the invention, in the step S2, the superfine white carbon black meeting the preset particle size is obtained by carrying out superfine processing on the white carbon black by a pulverizer, and preferably, the mesh number of the white carbon black subjected to superfine processing by the pulverizer is more than or equal to 1200 meshes.
In step S3, the present invention further provides a method of mixing and modifying the superfine silica and the hydroxy silicone oil under the conditions of the specified mass ratio of the superfine silica to the hydroxy silicone oil, the mixing and stirring temperature, the stirring time and the stirring speed. Preferably, the mass ratio of the superfine white carbon black to the hydroxyl silicone oil is 1 (0.1-0.07), the mixing and stirring temperature is 120-180 ℃, the stirring time is 30-60 min, and the stirring speed is 1200-1500 r/min.
As a further proposal of the invention, in the step S3, the superfine white carbon black is heated by an external heater.
As a further scheme of the invention, in the step S3, the superfine white carbon black and the hydroxyl silicone oil are directly mixed and stirred in a dry environment without adding other solvents.
The surface hydrophobic superfine white carbon black modified by the hydroxyl silicone oil prepared by the method.
Aiming at the problems in the prior art, the invention firstly improves the filter-pressing washing process in the white carbon black production system and improves the filter-pressing washing efficiency; and secondly, the method extends on the basis of the processing technology of the superfine white carbon black, and improves the industrial usability of the superfine white carbon black product. The method comprises the following steps: in the step S1.4, the filter pressing washing efficiency is improved by controlling the temperature and pressure of the washing water, the squeezing pressure and the blowing mode; in the step S3, the good surface hydrophobic modification rate of the superfine white carbon black is realized by controlling the mass ratio of the product to the modifier, the modification temperature, the modification time and the stirring rate. When the surface modification of the superfine white carbon black is performed by using a dry modification process, the surface hydrophobic modification of the superfine white carbon black can be realized only under the conditions of a certain proportion, temperature and time; the method is implemented at the tail end of the superfine white carbon black product, the modification of the existing superfine white carbon black production system is not needed, and the investment is low; the modification process can not generate waste gas, waste water and waste, and has no harm to the health of operators and the ecological environment.
The beneficial effects of the invention are as follows: after the common white carbon black is processed into the superfine white carbon black finished product, the surface modification and reprocessing are carried out, which is a continuation of the white carbon black deep processing industry chain, and the modification of a front production system is not needed, so that the production process is simpler, the investment is less, and the method can be used as an independent white carbon black product deep processing industry; the modification process only uses a small amount of hydroxyl silicone oil and is completed in a sealed environment, so that the production process is safer for operators and basically has no pollution to the environment; and the optimized mixed preparation process parameters are obtained through the defined process parameter relation, the production efficiency of the preparation by adopting the process parameters is higher, the production raw materials and the modifier are easy to obtain, and the production process is energy-saving and environment-friendly.
Drawings
FIG. 1 is a schematic flow chart of the method of the present invention.
FIG. 2 is a diagram of a modified white carbon black product prepared by the method of the invention.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the examples of the present application, and it is obvious that the described embodiments are merely examples and are not intended to limit the present application.
As shown in figure 1, the modification method for preparing the surface hydrophobic precipitation method superfine white carbon black by using hydroxyl silicone oil in a dry environment comprises the following steps:
s1: preparing white carbon black by using water glass and concentrated sulfuric acid; the method specifically comprises the following steps:
s1.1, material conversion: dissolving water glass in hot water, wherein the density of the water solution of the water glass is 1.2-1.4 g/cm 3 ；
S1.2 pretreatment: precipitating and filtering the water glass solution obtained in the step S1, and transferring the water glass solution into a high-level tank;
s1.3, synthesizing white carbon black, and simultaneously injecting concentrated sulfuric acid and the water glass solution obtained in the step S2 into a reaction kettle, wherein the flow ratio of the concentrated sulfuric acid to the water glass solution is 1:12-18;
s1.4, white carbon black filter pressing and washing: performing filter pressing washing on the mixture obtained in the step S3, monitoring the conductivity of washing water in the washing process until the conductivity of the washing water is less than 3.5 ms/cm, and blowing high-pressure air to a filter cake for 10-20 min; in the step, the filter cake is dehydrated in the modes of central blowing, water squeezing, central blowing and side blowing, so that the water content in the filter cake can be further reduced, the washing efficiency is improved, the production period is shortened, and quick washing is realized.
S1.5, pulping a filter cake: conveying the filter cake obtained in the step S4 to a pulping tank by using a belt, and adding water to pulp, wherein the mass ratio of the filter cake to the water is 3.8-1.3:1;
s1.6, drying a product: and (3) conveying the slurry obtained in the step (S5) to a spray drying tower by a screw pump, and separating by a bag type dust collector after spray drying to obtain white carbon black.
S2, superfine white carbon black: and (3) conveying the finished product obtained in the step (S6) to a pulverizer through a pipeline by using an air blower, and separating by using a bag type dust collector after superfine processing to obtain superfine white carbon black. In the step, the white carbon black is subjected to superfine processing by a pulverizer, so that the granularity of the white carbon black can be thinned, the granularity is more than or equal to 1200 meshes, and the white carbon black is more uniformly mixed when being used as an additive.
S3, modifying superfine white carbon black: and (3) conveying the finished product obtained in the step (S7) to a modification stirrer through an air blower and a pipeline, mixing and stirring with hydroxyl silicone oil, and separating through a bag type dust collector to obtain the surface hydrophobic superfine white carbon black. In the step, the external heater is used for heating the superfine white carbon black, so that the uneven heating of the superfine white carbon black is avoided, and the modification effect is influenced. In the actual process of stirring, mixing and modifying the white carbon black and the hydroxyl silicone oil, the particle size of the white carbon black, the consumption of the hydroxyl silicone oil and the comprehensive influence among stirring parameters are comprehensively considered, and because the particle size of the white carbon black is generally related to the actual demands of customers, the specific surface area is increased due to the excessively fine particle size of the white carbon black, and agglomeration or poor modification effect are easily caused; the excessively coarse particle size also causes poor performance of the white carbon black in the subsequent use process. Meanwhile, under different particle sizes, the requirements on the dosage of the hydroxyl silicone oil, namely the mass ratio of the superfine white carbon black to the hydroxyl silicone oil, are different in order to obtain a better modification effect and avoid the excessive use of the hydroxyl silicone oil so as to cause cost improvement due to different specific surface areas. However, under different usage amounts of the hydroxyl silicone oil, parameters affecting the stirring and mixing effects such as viscosity of the mixture are changed, so that corresponding mixing and stirring parameters such as modification temperature, stirring speed, time and the like are designed. Experiments show that in the mixing and stirring modification process, the parameters are complex and are not in a simple linear relationship. Thus in order to do so,according to the data of white carbon black particle size, hydroxyl silicone oil consumption, modification temperature, stirring parameters and the like obtained in the actual treatment process of mixing and stirring modification in a large amount, the relation among the parameter data is analyzed, fitting analysis is carried out, and the following use relation is set:wherein D is the particle size of superfine white carbon black, and the unit is mu M s Is the mass of hydroxyl silicone oil, M c The quality of the superfine white carbon black is that k is a coefficient, and the value range is 1.8-2.2. The influence of the use amount of different hydroxyl silicone oils adopted under the superfine white carbon black with different particle sizes is considered. In the most preferred mode, the adopted superfine white carbon black is sieved by a 1340 mesh sieve, namely the particle size is 10 mu m, and the mass ratio of the superfine white carbon black to the hydroxyl silicone oil is about 1: (0.098-0.12), taking into account the loss in the process of adding the hydroxyl silicone oil, setting the mass ratio of the superfine white carbon black to the hydroxyl silicone oil to be 1:0.1. in terms of stirring parameters, the mixing and stirring rate is limited to 1200-1500 r/min due to equipment limitation, and the heating temperature range is limited to 120-180 ℃ in consideration of the relation between the hydroxyl content, viscosity and temperature of different hydroxyl silicone oils. The stirring time is 30-60 min. Preferably, for hydroxyl silicone oil with hydroxyl content of 6-8%, heating temperature is 140 ℃ and stirring time is 40min.
Example 1
S1.4, white carbon black filter pressing and washing: performing filter pressing washing on the mixture obtained in the step S1.3, wherein the temperature of the adopted washing water is 45-55 o C, the washing pressure is 0.7-0.75MPa, the squeezing pressure is 0.7-0.8MPa, and the washing water electrolysis rate is monitored in the washing process until the washing water electrolysis rate is less than 3.5 mS/cm;
s2, superfine white carbon black: conveying the finished product obtained in the step S1.6 to a jet mill with the set feeding pressure of 0.7MPa and the crushing pressure of 0.4MPa through an air blower, carrying out superfine processing, separating through a bag type dust collector, and passing through a screen with the specified mesh number to obtain superfine white carbon black;
s3, modifying superfine white carbon black: conveying the superfine white carbon black obtained in the step S2 into a modification stirrer through a pipeline by an air blower, wherein the mass ratio of the superfine white carbon black to the hydroxyl silicone oil is 1:0.1, mixing and stirring at 140 ℃, and separating by a bag type dust collector to obtain a product 1#, wherein the actual product is shown in figure 2.
Other processes and parameters are the same as those described above, and will not be described again here.
Example 2
S1.4, white carbon black filter pressing and washing: performing filter pressing washing on the mixture obtained in the step S1.3, wherein the temperature of the adopted washing water is 45-55 o C, the washing pressure is 0.7-0.75MPa, the squeezing pressure is 0.7-0.8MPa, and the washing water electrolysis rate is monitored in the washing process until the washing water electrolysis rate is less than 3.5 mS/cm;
s2, superfine white carbon black: conveying the finished product obtained in the step S1.6 to a jet mill with the set feeding pressure of 0.7MPa and the crushing pressure of 0.4MPa through an air blower, carrying out superfine processing, separating through a bag type dust collector, and passing through a screen with the specified mesh number to obtain superfine white carbon black;
s3, modifying superfine white carbon black: conveying the superfine white carbon black obtained in the step S2 into a modification stirrer through a pipeline by an air blower, wherein the mass ratio of the superfine white carbon black to the hydroxyl silicone oil is 1:0.09, mixing and stirring at 140 ℃, and separating by a bag type dust collector to obtain the product named as No. 2.
Other processes and parameters are the same as those described above, and will not be described again here.
Example 3
S1.4, white carbon black filter pressing and washing: performing filter pressing washing on the mixture obtained in the step S1.3, wherein the temperature of the adopted washing water is 45-55 o C, the washing pressure is 0.7-0.75MPa, the squeezing pressure is 0.7-0.8MPa, and the washing water electrolysis rate is monitored in the washing process until the washing water electrolysis rate is less than 3.5 mS/cm;
s2, superfine white carbon black: conveying the finished product obtained in the step S1.6 to a jet mill with the set feeding pressure of 0.7MPa and the crushing pressure of 0.4MPa through an air blower, carrying out superfine processing, separating through a bag type dust collector, and passing through a screen with the specified mesh number to obtain superfine white carbon black;
s3, modifying superfine white carbon black: conveying the superfine white carbon black obtained in the step S2 into a modification stirrer through a pipeline by an air blower, wherein the mass ratio of the superfine white carbon black to the hydroxyl silicone oil is 1:0.08, mixing and stirring at 140 ℃, and separating by a bag type dust collector to obtain the product which is marked as No. 3.
Other processes and parameters are the same as those described above, and will not be described again here.
Example 4
S1.4, white carbon black filter pressing and washing: performing filter pressing washing on the mixture obtained in the step S1.3, wherein the temperature of the adopted washing water is 45-55 o C, the washing pressure is 0.7-0.75MPa, the squeezing pressure is 0.7-0.8MPa, and the washing water electrolysis rate is monitored in the washing process until the washing water electrolysis rate is less than 3.5 mS/cm;
s2, superfine white carbon black: conveying the finished product obtained in the step S1.6 to a jet mill with the set feeding pressure of 0.7MPa and the crushing pressure of 0.4MPa through an air blower, carrying out superfine processing, separating through a bag type dust collector, and passing through a screen with the specified mesh number to obtain superfine white carbon black;
s3, modifying superfine white carbon black: conveying the superfine white carbon black obtained in the step S2 into a modification stirrer through a pipeline by an air blower, wherein the mass ratio of the superfine white carbon black to the hydroxyl silicone oil is 1:0.07, mixing and stirring at 140 ℃, and separating by a bag type dust collector to obtain the product named as No. 4.
Other processes and parameters are the same as those described above, and will not be described again here.
The modified superfine white carbon black products of No. 1, no. 2, no. 3 and No. 4 are obtained by the four examples, and the surface hydrophobicity of the modified superfine white carbon black is tested according to industry standards, and the measured performance results are shown in the following table:
TABLE 1 comparison of surface hydrophobicity Properties
The influence of the superfine white carbon black before and after modification on the rubber properties is tested according to industry standards, and the physical properties of the rubber are measured, and the results are shown in the following table:
TABLE 2 comparison of physical Properties index of modified white carbon Black
As can be seen from the data in the table, the modified superfine white carbon black is applied to rubber as an additive, and has certain optimization on indexes of rubber products. Meanwhile, as can be seen from the data calculation in the table, the modified superfine white carbon black is beneficial to improving the vulcanization rate of rubber, and the crosslinking degree during vulcanization is better, and the improvement of the two indexes is helpful to reducing the energy consumption of the rubber vulcanization process and improving the production efficiency of the rubber vulcanization operation.
The above applications are only some of the embodiments of the present application. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit of the inventive concept.
Claims (10)
1. The method for preparing the surface hydrophobic modified superfine white carbon black by using the hydroxyl silicone oil is characterized by comprising the following steps of:
s1: preparing white carbon black by using water glass and concentrated sulfuric acid;
s2: crushing the white carbon black obtained in the step S1;
s3: and (3) mixing and stirring the white carbon black after the S2 is crushed with the hydroxyl silicone oil to obtain the surface hydrophobic superfine white carbon black modified by the hydroxyl silicone oil.
2. The method for preparing surface-hydrophobically modified ultrafine white carbon black with hydroxyl silicone oil as set forth in claim 1, wherein the step S1 comprises:
s1.1, material conversion: dissolving water glass in hot water;
s1.2 pretreatment: precipitating and filtering the water glass solution obtained in the step S1.1, and transferring the water glass solution into a high-level tank;
s1.3, white carbon black synthesis: simultaneously injecting concentrated sulfuric acid and the water glass solution obtained in the step S1.2 into the reaction kettle;
s1.4, white carbon black filter pressing and washing: carrying out filter pressing washing on the mixture obtained in the step S1.3;
s1.5, pulping a filter cake: conveying the filter cake obtained after filter pressing and washing in the step S1.4 to a pulping tank by using a belt, and adding water to pulp;
s1.6, drying the product: and (3) conveying the slurry obtained in the step (S1.5) to a spray drying tower by a screw pump, and separating by a bag type dust collector after spray drying to obtain white carbon black.
3. The method for preparing surface-hydrophobically modified ultrafine white carbon black with hydroxyl silicone oil as set forth in claim 2, wherein the step S2 comprises: and (3) conveying the finished product obtained in the step (S1.6) to a pulverizer through a pipeline by using an air blower, and separating by using a bag type dust collector after superfine processing to obtain the superfine white carbon black.
4. A method for preparing surface-hydrophobically modified ultrafine white carbon black with hydroxyl silicone oil as set forth in claim 3, wherein said step S3 comprises: and (3) conveying the finished product obtained in the step (S2) to a modification stirrer through an air blower and a pipeline, mixing and stirring with hydroxyl silicone oil, and separating through a bag type dust collector to obtain the surface hydrophobic superfine white carbon black.
5. The method for preparing surface-hydrophobically modified ultrafine white carbon black with hydroxyl silicone oil as set forth in claim 4, wherein the filter cake is dehydrated in step S1.4 by means of central blowing-water pressing-central blowing.
6. The method for preparing surface-hydrophobically modified ultrafine white carbon black with hydroxyl silicone oil as set forth in claim 5, wherein in step S2, the ultrafine white carbon black is subjected to ultrafine processing by a pulverizer to obtain ultrafine white carbon black conforming to a predetermined particle diameter.
7. The method for preparing surface-hydrophobically modified ultrafine white carbon black with a hydroxyl silicone oil as set forth in claim 6, wherein in step S3, the mixing modification is performed under the conditions of the specified mass ratio of ultrafine white carbon black to hydroxyl silicone oil, mixing and stirring temperature, stirring time, stirring speed.
8. The method for preparing surface-hydrophobically modified ultrafine white carbon black with hydroxyl silicone oil as set forth in claim 7, wherein in step S3, the ultrafine white carbon black is heated by an external heater.
9. The method for preparing surface-hydrophobically modified ultrafine white carbon black with hydroxy silicone oil as set forth in claim 8, wherein in step S3, the ultrafine white carbon black and the hydroxy silicone oil are directly mixed and stirred in a dry environment without adding other solvents.
10. The surface-modified hydrophobic ultrafine white carbon black modified by hydroxyl silicone oil prepared by the method according to any one of claims 1 to 9.
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