CN111099595A - Preparation method of high-performance silicon dioxide - Google Patents
Preparation method of high-performance silicon dioxide Download PDFInfo
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- CN111099595A CN111099595A CN202010034664.5A CN202010034664A CN111099595A CN 111099595 A CN111099595 A CN 111099595A CN 202010034664 A CN202010034664 A CN 202010034664A CN 111099595 A CN111099595 A CN 111099595A
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- silicon dioxide
- sodium silicate
- reaction kettle
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 42
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 42
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 30
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 30
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 6
- 230000032683 aging Effects 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 150000004965 peroxy acids Chemical class 0.000 claims abstract description 5
- 238000004537 pulping Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 12
- 239000007822 coupling agent Substances 0.000 claims description 9
- 238000005374 membrane filtration Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 239000012065 filter cake Substances 0.000 claims description 3
- 239000012452 mother liquor Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 239000012744 reinforcing agent Substances 0.000 abstract description 6
- 230000003014 reinforcing effect Effects 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 230000002431 foraging effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 25
- 239000002245 particle Substances 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
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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
Abstract
The invention discloses a preparation method of high-performance silicon dioxide in the technical field of silicon dioxide, which comprises the steps of preparing raw materials, adding a base solution, carrying out synthetic reaction, then acidifying, aging, filtering, washing, pulping and drying, wherein the synthetic reaction is carried out by firstly adding sulfuric acid and then dropwise adding a sodium silicate solution, the dropwise adding flow rate is reduced in the latter half section of the reaction, the reaction process is continuously stirred and is heated by introducing steam, after rapidly peracid with higher acid flow rate is used in the later acidifying process, stirring is continuously carried out until the solution forms sticky gel, the materials are kept stand in a reaction kettle for aging, then filtering, washing, pulping and drying are carried out to obtain a silicon dioxide product, the preparation method of the high-performance silicon dioxide provided by the invention has the advantages that the high-performance silicon dioxide with large specific surface area and good dispersibility is prepared in the whole process, the rubber reinforcing agent has high reinforcing property in rubber products, and can obviously improve the mechanical property of rubber when used as a rubber reinforcing agent.
Description
Technical Field
The invention relates to the technical field of silicon dioxide, in particular to a preparation method of high-performance silicon dioxide.
Background
Silica is widely used in many fields such as rubber, paint, feed and the like due to its special surface structure and unique physicochemical characteristics. Because of the characteristics of low price, good reinforcing performance, large filling amount and the like, the silicon dioxide is the second largest rubber reinforcing agent second to carbon black. Compared with carbon black tread rubber, the friction resistance of the silica tread rubber is reduced by about 20%, so that the silica tread rubber is beneficial to energy conservation and environmental protection, and has important practical significance and industrial value for the development of the tire rubber industry.
Therefore, with the increasing awareness of environmental protection and energy conservation of modern people, tire rubber manufacturers are gradually using silica instead of carbon black. The problems of large particle size, low dispersity and specific surface area and the like of the silicon dioxide commonly existing in the preparation process of the silicon dioxide by the existing precipitation method affect that the reinforcing property of the silicon dioxide in rubber is low, and the properties of the rubber product such as tensile strength, tearing strength and the like can be reduced when the silicon dioxide is used in the rubber.
Based on the above, the invention designs a preparation method of high-performance silicon dioxide to solve the above problems.
Disclosure of Invention
The invention aims to provide a preparation method of high-performance silicon dioxide to solve the problems.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of high-performance silicon dioxide comprises the following steps:
s1, preparation of raw materials: adding a certain amount of solid sodium silicate and water into a dissolving device, sealing the dissolving device, setting a certain pressure in the dissolving device, keeping the temperature at 150-200 ℃, and preparing to obtain a sodium silicate solution with the concentration of 1.0-1.1 mol/L after the sodium silicate is completely dissolved;
s2, base solution: after the complete cleanness in the reaction kettle and the correct states of all valves are confirmed, the reaction kettle is rotated to 35m3Process hot water and 4.0m3Adding the sodium silicate solution into a reaction kettle, stirring at a certain rotating speed, continuously introducing steam to raise the temperature, and controlling the temperature to be 60 ℃;
s3, synthesis reaction: firstly, respectively adding 0.5-0.6 m of sulfuric acid and diluting water3The sum of the sums of the sum of the sums3The flow rate of the mixture is simultaneously injected into the reaction kettle, after stirring for 30min, steam is introduced under continuous stirring to heat to 80-90 ℃, and then the mixture is heated to 0.5-1.0 m3Adding the sodium silicate solution into the reaction kettle at a dropping speed of/h until the pH value of the reaction system is 8.0-8.5, and reducing the dropping speed of the sodium silicate solution by 0.05-0.08 m3Continuing to add the solution dropwise until the pH value is 9.5 and the addition end point is reached, and stopping adding the sodium silicate solution;
s4, post-acidification: stirring continuously until the sulfuric acid is 1.5m3The flow rate of the solution/h is introduced into the reaction kettle for rapid peracid, and the flow rate is 7.5m3Water/h dilution until pH 5.05.5, finishing post-acidification;
s5, aging: after the post-acidification is finished, continuously stirring until the solution forms viscous gel, finely adjusting the pH value of the system to 5.0-5.5, and standing the material in a reaction kettle for 3-10 hours;
and S6, filtering the materials, performing filter pressing and washing through a plate-and-frame filter press, pulping the washed filter cake up to the standard, and drying to obtain the silicon dioxide product.
Preferably, the stirring speed of 40 rpm is kept during the reactions of S2, S3, S4 and S5.
Preferably, a coupling agent (Si 75) is dropwise added into the reaction kettle in the stirring process of adding the sulfuric acid into the S3, the adding amount of the coupling agent is 0.15-0.20% of the weight of the solid sodium silicate in the S1, and the dropwise addition of the coupling agent is stopped when the pH value of the reaction system is greater than 9.0.
Preferably, the step of filtering the material in S6 is to dehydrate the material in a membrane filtration manner to obtain sodium sulfate aqueous phase mother liquor and silica slurry.
Preferably, the flow velocity of the material is controlled to be 13-20 m during membrane filtration3/h。
Compared with the prior art, the invention has the beneficial effects that: the synthesis reaction is carried out in a mode of dropwise adding the sodium silicate solution into the sulfuric acid, the sodium silicate solution is firstly dropwise added into the sulfuric acid at a certain lower flow rate, and the dropwise adding flow rate is reduced in the latter half section of the reaction, so that the reaction end point pH value can be accurately controlled, the reaction time can be effectively prolonged, the synthesis reaction of the sulfuric acid and the sodium silicate solution can be completely carried out, the nucleated particles can be fully grown, the pore volume is larger, and the specific surface area of the silicon dioxide is further increased; the reaction pH is continuously adjusted in the reaction process, so that the pore size distribution of the silicon dioxide is adjusted in the particle generation process; in addition, in the post-acidification process, a larger acid flow rate is used for rapidly preparing peracid, the time of the material in neutral is reduced from alkalinity to acidity as much as possible, the product dispersibility is better, the product has high reinforcement in rubber products, and high-performance silicon dioxide with large specific surface area and good dispersibility is prepared in the whole process and used as a rubber reinforcing agent, so that the mechanical property of rubber can be obviously improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a table showing the comparison of the comprehensive indexes of the products of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme that: the embodiment of the preparation method of high-performance silicon dioxide comprises the following specific operation steps:
s1, preparation of raw materials: respectively adding a certain amount of solid sodium silicate and water into a dissolving device, sealing the dissolving device, dissolving the sodium silicate at a required pressure and high temperature in the dissolving device, keeping the temperature at 150-200 ℃, preparing the sodium silicate solution with the concentration of 1.0-1.1 mol/L after the sodium silicate is completely dissolved, and introducing steam to accelerate the heating of the solid sodium silicate, improve the molecular activity and shorten the dissolving period;
s2, base solution: after the complete cleanness in the reaction kettle and the correct states of all valves are confirmed, the reaction kettle is rotated to 35m3Process hot water and 4.0m3Adding the sodium silicate solution into a reaction kettle, stirring at the rotating speed of 40 rpm, continuously introducing steam to raise the temperature, and controlling the temperature to be 60 ℃;
s3, synthesis reaction: firstly, respectively adding 0.5-0.6 m of sulfuric acid and diluting water3The sum of the sums of the sum of the sums3The flow rate of the solution/h is simultaneously injected into a reaction kettle, the solution is stirred for 30min at the rotating speed of 40 r/min, and the coupling solution is dropwise added into the reaction kettleAn agent (Si 75), wherein the addition amount of the coupling agent is 0.15-0.20% of the weight of the solid sodium silicate, and the pH value of the coupling agent in a reaction system>Stopping adding the raw materials at 9.0, reducing the viscosity of rubber materials, reducing the number of mixing stages, improving the processing performance of the rubber materials, promoting the dispersion of reinforcing agents and improving the dynamic mechanical property of the rubber materials by using the silica filled with the coupling agents, stirring at the rotating speed of 40 revolutions per minute, introducing steam, raising the temperature to 80-90 ℃, and then adding the steam at the rotating speed of 0.5-1.0 m3Adding the sodium silicate solution into the reaction kettle at a dropping speed of/h until the pH value of the reaction system is 8.0-8.5, and reducing the dropping speed of the sodium silicate solution by 0.05-0.08 m3The dripping is continued until the pH value reaches the dripping end point of 9.5, the method not only can accurately control the pH value of the reaction end point, but also can effectively prolong the reaction time, ensure that the synthesis reaction of the sulfuric acid and the sodium silicate solution can be completely carried out, ensure that the nucleated particles can fully grow up and have larger pore volume, and further increase the specific surface area of the silicon dioxide;
s4, post-acidification: stirring was carried out at a rotational speed of 40 rpm, and the sulfuric acid was set at 1.5m3The flow rate of the solution/h is introduced into the reaction kettle for rapid peracid, and the flow rate is 7.5m3Diluting water for h until the pH value reaches 5.0-5.5, and then acidifying to finish;
s5, aging: after the post-acidification is finished, continuously stirring until the solution forms viscous gel, finely adjusting the pH value of the system to 5.0-5.5, standing the material in a reaction kettle for 3-10 hours, and aging to generate seed crystals;
s6, firstly dehydrating the obtained material by membrane filtration to obtain sodium sulfate water phase mother liquor and silicon dioxide slurry, wherein the membrane filtration also comprises a natural sedimentation process, and the flow rate of the material is controlled to be 13-20 m during the membrane filtration3And h, performing filter pressing washing on the silicon dioxide slurry through a plate-and-frame filter press, pulping the washed filter cake up to the standard, and drying through a complete set of drying tower to obtain the silicon dioxide product.
The properties of the silica product obtained in the above examples were tested against a rubber product obtained from a conventional 1165MP silica product, and comparative analysis is shown in FIG. 1.
As can be seen from FIG. 1, the specific surface area, tensile strength, elongation, tear strength and other aspects of the examples are better than those of the 1165MP silica product, which shows that the high-performance silica obtained in the examples has larger specific surface area and good dispersibility, and can obviously improve the mechanical properties of rubber when used as a rubber reinforcing agent.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (5)
1. A preparation method of high-performance silicon dioxide is characterized by comprising the following steps:
s1, preparation of raw materials: adding a certain amount of solid sodium silicate and water into a dissolving device, sealing the dissolving device, setting a certain pressure in the dissolving device, keeping the temperature at 150-200 ℃, and preparing to obtain a sodium silicate solution with the concentration of 1.0-1.1 mol/L after the sodium silicate is completely dissolved;
s2, base solution: after the complete cleanness in the reaction kettle and the correct states of all valves are confirmed, the reaction kettle is rotated to 35m3Process hot water and 4.0m3Adding sodium silicate solution into the reaction kettle, stirring at a certain rotation speed, continuously introducing steam to raise the temperature, and makingControlling the temperature at 60 ℃;
s3, synthesis reaction: firstly, respectively adding 0.5-0.6 m of sulfuric acid and diluting water3The sum of the sums of the sum of the sums3The flow rate of the mixture is simultaneously injected into the reaction kettle, after stirring for 30min, steam is introduced under continuous stirring to heat to 80-90 ℃, and then the mixture is heated to 0.5-1.0 m3Adding the sodium silicate solution into the reaction kettle at a dropping speed of/h until the pH value of the reaction system is 8.0-8.5, and reducing the dropping speed of the sodium silicate solution by 0.05-0.08 m3Continuing to add the solution dropwise until the pH value is 9.5 and the addition end point is reached, and stopping adding the sodium silicate solution;
s4, post-acidification: stirring continuously until the sulfuric acid is 1.5m3The flow rate of the solution/h is introduced into the reaction kettle for rapid peracid, and the flow rate is 7.5m3Diluting water for h until the pH value reaches 5.0-5.5, and then acidifying to finish;
s5, aging: after the post-acidification is finished, continuously stirring until the solution forms viscous gel, finely adjusting the pH value of the system to 5.0-5.5, and standing the material in a reaction kettle for 3-10 hours;
and S6, filtering the materials, performing filter pressing and washing through a plate-and-frame filter press, pulping the washed filter cake up to the standard, and drying to obtain the silicon dioxide product.
2. The method for preparing high-performance silica according to claim 1, wherein: stirring at 40 rpm is maintained during the reactions of S2, S3, S4 and S5.
3. The method for preparing high-performance silica according to claim 1, wherein: and in the stirring process of adding sulfuric acid into the S3, dropwise adding a coupling agent (Si 75) into the reaction kettle, wherein the addition amount of the coupling agent is 0.15-0.20% of the weight of the solid sodium silicate in the S1, and the dropwise adding of the coupling agent is stopped when the pH value of the reaction system is greater than 9.0.
4. The method for preparing high-performance silica according to claim 1, wherein: and in the S6, the material is filtered in a membrane filtration mode, and the material is dehydrated to obtain sodium sulfate water-phase mother liquor and silicon dioxide slurry.
5. The method for preparing high-performance silica according to claim 4, wherein: the flow velocity of the materials is controlled to be 13-20 m during membrane filtration3/h。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112678831A (en) * | 2021-02-02 | 2021-04-20 | 福建省三明正元化工有限公司 | Method for preparing silicon dioxide by using graphene oxide waste liquid |
| CN113651332A (en) * | 2021-08-11 | 2021-11-16 | 常州大学 | Preparation method of high-performance white carbon black based on styrene butadiene rubber reinforcement |
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| CN112678831A (en) * | 2021-02-02 | 2021-04-20 | 福建省三明正元化工有限公司 | Method for preparing silicon dioxide by using graphene oxide waste liquid |
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| CN113651332B (en) * | 2021-08-11 | 2023-10-27 | 常州大学 | Preparation method of high-performance white carbon black based on styrene-butadiene rubber reinforcement |
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Application publication date: 20200505 |