CN111825098B - High-dispersion large-pore-volume pore-diameter narrow-distribution hydrated silicon dioxide and preparation method thereof - Google Patents
High-dispersion large-pore-volume pore-diameter narrow-distribution hydrated silicon dioxide and preparation method thereof Download PDFInfo
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- CN111825098B CN111825098B CN202010684629.8A CN202010684629A CN111825098B CN 111825098 B CN111825098 B CN 111825098B CN 202010684629 A CN202010684629 A CN 202010684629A CN 111825098 B CN111825098 B CN 111825098B
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 25
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 24
- 239000006185 dispersion Substances 0.000 title claims abstract description 15
- 238000009826 distribution Methods 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 35
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 35
- 239000011148 porous material Substances 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000003792 electrolyte Substances 0.000 claims abstract description 8
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 8
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052753 mercury Inorganic materials 0.000 claims abstract description 4
- 230000035515 penetration Effects 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 229960001866 silicon dioxide Drugs 0.000 claims description 19
- 229960004029 silicic acid Drugs 0.000 claims description 14
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical group [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 13
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 claims description 13
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 13
- 235000011152 sodium sulphate Nutrition 0.000 claims description 13
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 12
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 5
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical group [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000012744 reinforcing agent Substances 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 description 37
- 230000001105 regulatory effect Effects 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 238000004537 pulping Methods 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 238000003825 pressing Methods 0.000 description 4
- 239000008213 purified water Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229920001971 elastomer Polymers 0.000 description 3
- 239000005060 rubber Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- FHKPLLOSJHHKNU-INIZCTEOSA-N [(3S)-3-[8-(1-ethyl-5-methylpyrazol-4-yl)-9-methylpurin-6-yl]oxypyrrolidin-1-yl]-(oxan-4-yl)methanone Chemical compound C(C)N1N=CC(=C1C)C=1N(C2=NC=NC(=C2N=1)O[C@@H]1CN(CC1)C(=O)C1CCOCC1)C FHKPLLOSJHHKNU-INIZCTEOSA-N 0.000 description 1
- JAWMENYCRQKKJY-UHFFFAOYSA-N [3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-ylmethyl)-1-oxa-2,8-diazaspiro[4.5]dec-2-en-8-yl]-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]methanone Chemical compound N1N=NC=2CN(CCC=21)CC1=NOC2(C1)CCN(CC2)C(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F JAWMENYCRQKKJY-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/06—Copolymers with styrene
-
- 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
- C01P2006/14—Pore volume
-
- 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
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
-
- 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
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
-
- 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
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Abstract
The invention discloses high-dispersion large-pore-volume pore-diameter narrow-distribution hydrated silicon dioxide, which has the following performance parameters: dispersion grade 10, mercury penetration pore volume not less than 1.7cm 3 The pore volume of the pores with the aperture of 25-50nm is more than or equal to 60 percent of the total pore volume. The preparation process comprises the following steps: preparing a sodium silicate solution containing an additional electrolyte and a surfactant; sulfuric acid and sodium silicate are alternately added into the prepared sodium silicate solution, so that the pH value of a reaction system swings back and forth for a plurality of times, the end point of the pH value swing is controlled to be 3-6, and the obtained hydrated silicon dioxide slurry is subjected to solid-liquid separation to obtain the hydrated silicon dioxide. The hydrated silicon dioxide has the characteristics of high dispersion grade, large pore volume and narrow pore size distribution, and is particularly suitable for serving as a reinforcing agent of a high-performance tire.
Description
Technical Field
The invention belongs to the field of hydrated silicon dioxide, and particularly relates to high-dispersion large-pore-volume pore-diameter narrow-distribution hydrated silicon dioxide and a preparation method thereof.
Background
The hydrated silicon dioxide is an amorphous light hydrated silicon dioxide material, the particles have a large number of micropore structures, the specific surface area is large, the surface is rich in hydroxyl groups, and the characteristics of good adsorption, flame retardance, insulation, suspension, vibration liquefaction, thixotropy and the like are achieved. The hydrated silicon dioxide used for the high-performance radial tire can reduce rolling resistance, save fuel consumption, improve wet skid resistance and improve vehicle safety performance. In order to meet the needs of the development of the tire industry, it is highly desirable to obtain hydrated silica having a high dispersion level, a large pore volume, and a narrow pore size distribution.
Disclosure of Invention
The invention aims to provide high-dispersion large-pore-volume pore-diameter narrow-distribution hydrated silicon dioxide.
Another object of the present invention is to provide a method for preparing the above-mentioned high-dispersion large-pore-volume pore-diameter narrow-distribution hydrated silica.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a highly dispersed, large pore volume, narrow pore size distribution hydrated silica having the following performance parameters: dispersion grade 10, mercury penetration pore volume not less than 1.7cm 3 The pore volume of the pores with the aperture of 25-50nm accounts for 60-85% of the total pore volume.
More preferably, the mercury penetration hole has a volume of 1.7 to 2.0cm 3 The pore volume of the pores with the aperture of 25-50nm is more than or equal to 60 percent of the total pore volume.
According to one of the preferred embodiments of the present invention, the hydrated silica is SiO 2 The content is more than or equal to 92 percent based on dry basis.
According to one of the preferred technical scheme of the invention, the total iron content of the hydrated silicon dioxide is less than or equal to 400mg/Kg, the total copper content is less than or equal to 5mg/Kg and the total manganese content is less than or equal to 20mg/Kg.
The preparation method of the hydrated silicon dioxide comprises the following steps:
(1) Preparing a sodium silicate solution containing an additional electrolyte and a surfactant;
(2) Alternately adding sulfuric acid and sodium silicate into the sodium silicate solution in the step (1) to enable the pH value of a reaction system to swing back and forth for a plurality of times, and controlling the end point of the pH value swing to be 3-6 to obtain hydrated silicon dioxide slurry;
(3) And (3) carrying out solid-liquid separation on the hydrated silicon dioxide slurry obtained in the step (2) to obtain the hydrated silicon dioxide.
According to one of the preferred technical schemes of the invention, the external electrolyte is sodium sulfate.
More preferably, the concentration of the additional electrolyte in step (1) is 20 to 200g/L.
In a preferred embodiment of the present invention, the surfactant is sodium dodecyl sulfonate and/or sodium dodecyl benzene sulfonate.
More preferably, the concentration of the surfactant in step (1) is 1 to 10g/L and/or the sodium silicate concentration is 10 to 30wt%.
In one of the preferred embodiments of the present invention, in the step (2), the pH of the reaction system swings back and forth between the alkaline and the acidic, and the difference in pH values of the back and forth swings gradually increases.
A rubber composition for a tire comprising a rubber and a reinforcing agent, wherein the reinforcing agent is the hydrated silica as described above.
The rubber composition for the tire has the following mechanical properties: the 300% stretching stress is more than or equal to 5.5MPa, the tensile strength is more than or equal to 19.0MPa, and the elongation at break is more than or equal to 550%.
The invention controls the speed of silicic acid polymerization reaction through the selection and the addition amount of the added electrolyte, improves the dispersibility of silicon dioxide through adding the surfactant, combines pH swing and controls the growth process of a silicon dioxide aggregate network, thereby obtaining the hydrated silicon dioxide with high dispersion and large pore volume and narrow pore diameter distribution, and is particularly suitable for being used as a reinforcing agent of a high-performance tire.
Detailed Description
The technical scheme of the present invention will be described in further detail with reference to the preferred embodiments.
Example 1
Dilute sulfuric acid was prepared at a concentration of 25 wt%. The liquid sodium silicate concentration was 30wt%, modulus n=3.
Adding a certain amount of liquid sodium silicate, purified water, sodium sulfate and sodium dodecyl benzene sulfonate into a reaction kettle in advance according to 25 weight percent of sodium silicate, 100g/L of sodium sulfate and 5g/L of sodium dodecyl benzene sulfonate, stirring uniformly, then adding dilute sulfuric acid under stirring, adjusting the pH value of the system to about 6.5 (+ -0.2), stirring for 5 minutes, adding the liquid sodium silicate, adjusting the pH value of the system to about 8, stirring for 5 minutes, adding the dilute sulfuric acid, adjusting the pH value of the system to about 5.5, stirring for 5 minutes, adding the liquid sodium silicate, adjusting the pH value of the system to about 9, stirring for 5 minutes, adding the dilute sulfuric acid, adjusting the pH value of the system to about 9.5, stirring for 5 minutes, adding the dilute sulfuric acid, adjusting the pH value of the system to about 4, stirring for 10 minutes, and performing filter pressing, washing, pulping and drying to obtain hydrated silica.
Example 2
Dilute sulfuric acid was prepared at a concentration of 25 wt%. The liquid sodium silicate concentration was 30wt%, modulus n=3.2.
Adding a certain amount of liquid sodium silicate, purified water, sodium sulfate and sodium dodecyl benzene sulfonate into a reaction kettle in advance according to 20 weight percent of sodium silicate, 30g/L of sodium sulfate and 2g/L of sodium dodecyl benzene sulfonate, uniformly stirring, adding dilute sulfuric acid under stirring, regulating the pH value of a system to about 6, stirring for 5 minutes, adding the liquid sodium silicate, regulating the pH value of the system to about 7.5, stirring for 5 minutes, adding the dilute sulfuric acid, regulating the pH value of the system to about 5, stirring for 5 minutes, adding the liquid sodium silicate, regulating the pH value of the system to about 8.5, stirring for 5 minutes, adding the dilute sulfuric acid, regulating the pH value of the system to about 4, stirring for 10 minutes, and performing filter pressing, washing, pulping and drying on the obtained hydrated silica thin slurry to obtain the hydrated silica.
Example 3
Dilute sulfuric acid was prepared at a concentration of 25 wt%. The liquid sodium silicate concentration was 30wt%, modulus n=3.
Adding a certain amount of liquid sodium silicate, sodium sulfate and sodium dodecyl benzene sulfonate into a reaction kettle in advance according to 30 weight percent of sodium silicate, 150g/L of sodium sulfate and 10g/L of sodium dodecyl benzene sulfonate, uniformly stirring, adding dilute sulfuric acid under stirring, regulating the pH value of the system to about 6.5, stirring for 5 minutes, adding the liquid sodium silicate, regulating the pH value of the system to about 8, stirring for 5 minutes, adding the dilute sulfuric acid, regulating the pH value of the system to about 5, stirring for 5 minutes, adding the liquid sodium silicate, regulating the pH value of the system to about 9.5, stirring for 5 minutes, adding the dilute sulfuric acid, regulating the pH value of the system to about 4, stirring for 5 minutes, regulating the pH value of the system to about 10, stirring for 5 minutes, adding the dilute sulfuric acid, regulating the pH value of the system to 3.5, stirring for 15 minutes, and obtaining hydrated silica slurry through further steps of washing, pulping and drying.
Example 4
Dilute sulfuric acid was prepared at a concentration of 25 wt%. The liquid sodium silicate concentration was 30wt%, modulus n=2.5.
Adding a certain amount of liquid sodium silicate, purified water, sodium sulfate and sodium dodecyl benzene sulfonate into a reaction kettle in advance according to 15wt% of sodium silicate, 100g/L of sodium sulfate and 3g/L of sodium dodecyl sulfate, stirring uniformly, adding dilute sulfuric acid under stirring, adjusting the pH value of the system to about 6.5, stirring for 5 minutes, adding the liquid sodium silicate, adjusting the pH value of the system to about 8, stirring for 5 minutes, adding the dilute sulfuric acid, adjusting the pH value of the system to about 5.5, stirring for 5 minutes, adding the liquid sodium silicate, adjusting the pH value of the system to about 9, stirring for 5 minutes, adding the dilute sulfuric acid, adjusting the pH value of the system to about 4.5, stirring for 5 minutes, adding the dilute sulfuric acid, adjusting the pH value of the system to about 4, stirring for 10 minutes, and performing filter pressing, washing, pulping and drying on the obtained hydrated silica slurry.
Comparative example 1
The difference compared to example 1 is that no sodium sulfate is added.
Comparative example 2
In comparison with example 1, the difference is that sodium dodecylbenzenesulfonate is not added.
Comparative example 3
Dilute sulfuric acid was prepared at a concentration of 25 wt%. The liquid sodium silicate concentration was 30wt%, modulus n=3.
Adding a certain amount of liquid sodium silicate, purified water, sodium sulfate and sodium dodecyl benzene sulfonate into a reaction kettle in advance according to 25 weight percent of sodium silicate and 100g/L of sodium sulfate and 5g/L of sodium dodecyl benzene sulfonate, stirring uniformly, adding dilute sulfuric acid under stirring, regulating the pH value of the system to about 4, stirring for 5 minutes, adding the liquid sodium silicate, regulating the pH value of the system to about 8, stirring for 5 minutes, adding the dilute sulfuric acid, regulating the pH value of the system to about 4, stirring and press-filtering for 10 minutes, and obtaining hydrated silica by washing, pulping and drying.
In the above examples, the "left and right" was controlled to.+ -. 0.2 when the pH was adjusted.
The conventional processes are adopted for filter pressing, washing, pulping and drying.
TABLE 1
TABLE 2
| Dispersion grade | 300% stress at definite elongation | Tensile Strength | Elongation at break | |
| Example 1 | 10 | 7.5MPa | 22MPa | 650％ |
| Example 2 | 10 | 5.8MPa | 19.5MPa | 550％ |
| Example 3 | 10 | 6.7MPa | 21MPa | 660％ |
| Example 4 | 10 | 6.4MPa | 20MPa | 600％ |
| Comparative example 1 | 8 | 4.5MPa | 18.1MPa | 510％ |
| Comparative example 2 | 8 | 4.1MPa | 17.5MPa | 500％ |
| Comparative example 3 | 9 | 5.2MPa | 18.7MPa | 550％ |
The dispersion grade was determined according to GB/T6030-2006 standard.
Pore volume and pore size distribution were determined according to GB/T21650.1-2008 standard.
The formula of the vulcanized rubber comprises the following steps: 1500 100 parts of Styrene Butadiene Rubber (SBR), 50 parts of white carbon black, 5 parts of zinc oxide, 1 part of stearic acid, 4000 3 parts of polyethylene glycol, 1.2 parts of accelerator DM, 0.7 part of accelerator M, 0.5 part of accelerator DPG and 2 parts of sulfur. Mixing and 300% elongation stress, tensile strength and elongation at break were tested according to HG/T2404-2008.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. A preparation method of high-dispersion large-pore-volume pore-diameter narrow-distribution hydrated silicon dioxide is characterized by comprising the following steps: the performance parameters of the hydrated silica are as follows: dispersion grade 10, mercury penetration pore volume not less than 1.7cm 3 The pore volume of the pores with the aperture of 25-50nm accounts for more than or equal to 60 percent of the total pore volume;
the method comprises the following steps:
(1) Preparing a sodium silicate solution containing an additional electrolyte and a surfactant;
(2) Alternately adding sulfuric acid and sodium silicate into the sodium silicate solution in the step (1) to enable the pH value of a reaction system to swing back and forth for a plurality of times, and controlling the end point of the pH value swing to be 3-6 to obtain hydrated silicon dioxide slurry;
(3) The hydrated silicon dioxide slurry in the step (2) is subjected to solid-liquid separation to obtain the hydrated silicon dioxide;
the concentration of the additional electrolyte in the step (1) is 20-200 g/L, and the additional electrolyte is sodium sulfate;
in the step (2), the pH value of the reaction system swings back and forth between alkalinity and acidity, and the pH value difference value of the back and forth swing gradually becomes larger.
2. The method of manufacturing according to claim 1, characterized in that: siO of the hydrated silica 2 The content is more than or equal to 92 percent based on dry basis.
3. The method of manufacturing according to claim 1, characterized in that: the surfactant is sodium dodecyl sulfonate and/or sodium dodecyl benzene sulfonate.
4. A method of preparation according to claim 1 or 3, characterized in that: the concentration of the surfactant in the step (1) is 1-10 g/L, and/or the concentration of the sodium silicate is 10-30 wt%.
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| CN113321217A (en) * | 2021-06-30 | 2021-08-31 | 确成硅化学股份有限公司 | Preparation method of special high-dispersion white carbon black for high-ice-surface-gripping tire |
| CN114560471A (en) * | 2022-03-25 | 2022-05-31 | 福建省三明同晟化工有限公司 | Silica for wear-resistant tire rubber and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005281012A (en) * | 2004-03-26 | 2005-10-13 | Tokuyama Corp | Method for manufacturing binary porous silica |
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