CN111423622A - Silicon dioxide nano composite reinforcing agent for hydrogenated nitrile rubber and preparation method thereof - Google Patents
Silicon dioxide nano composite reinforcing agent for hydrogenated nitrile rubber and preparation method thereof Download PDFInfo
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Abstract
The invention provides a silicon dioxide nano composite reinforcing agent for hydrogenated nitrile rubber and a preparation method thereof, belonging to the technical field of chemical industry, wherein sodium silicate is used as a silicon dioxide precursor, sulfuric acid is used as a precipitator, and a molybdenum disulfide/silicon dioxide nano reinforcing agent is prepared by an in-situ precipitation method; the layered molybdenum disulfide is added in the preparation process, so that silicon dioxide nano particles can directly grow on the surface of the molybdenum disulfide, the agglomeration phenomenon of nano fillers in rubber is reduced, the nano fillers with double components of molybdenum disulfide and silicon dioxide can play a synergistic reinforcement role, the reinforcement efficiency of the fillers is enhanced, and the reinforcing agent is more stable and efficient. The prepared double-component nano reinforcing agent has the advantages of stability, high efficiency, environmental protection, remarkable effect and the like, and can promote the further development of a hydrogenated nitrile butadiene rubber reinforcing system.
Description
Technical Field
The invention relates to a silicon dioxide nano composite reinforcing agent and a preparation method thereof, in particular to a silicon dioxide nano composite reinforcing agentSilicon dioxide nano composite reinforcing agent (MoS) for hydrogenated nitrile rubber2/SiO2) And a preparation method thereof, belonging to the technical field of chemical industry.
Technical Field
Hydrogenated nitrile as a highly saturated synthetic rubber has been highly regarded by governments. When the hydrogenated nitrile rubber is used as an elastomer material widely used in the fields of aviation, oil fields and sealing, a rubber reinforcing system of the hydrogenated nitrile rubber has the advantages of high efficiency, functionality and the like, and is considered to be the first choice for the elastomer material used under extreme conditions.
The Chinese patent application CN201611130069 describes a hydrogenated nitrile-butadiene rubber composite material and a preparation method thereof, wherein natural gas reinforcing carbon black N774 is used as a rubber reinforcing agent in an amount of 35-40 parts, and silica micropowder is used as a reinforcing auxiliary agent in an amount of 15-20 parts. The natural gas reinforced carbon black N774 has the defects of environmental pollution and serious dependence on fossil energy such as natural gas and the like. In the hydrogenated nitrile rubber composite material, the consumption of natural gas reinforcing carbon black N774 is large, the consumption of the silicon micropowder is combined, the consumption of the reinforcing agent in the hydrogenated nitrile rubber composite material is too large, the mass ratio of the reinforcing agent to the hydrogenated nitrile rubber masterbatch is 50-60: 100, the use efficiency of the filler in the rubber composite material is too low, and certain resource waste is generated.
The Chinese invention patent application CN201410391897 introduces a hydrogenated nitrile rubber vulcanized rubber with high strength, high pressure resistance and hydrogen sulfide corrosion resistance. The mass ratio of the reinforcing agent to the hydrogenated butyronitrile master batch in the rubber composite material is 60-120: 100, and the composite material uses excessive reinforcing agent, so that the reinforcing agent efficiency is extremely low, and serious resource waste is generated.
The silica nanoparticles have the characteristics of no environmental pollution, low price and excellent reinforcing performance, and are considered to be a new generation of green filler capable of replacing carbon black. The surface of the silicon dioxide is rich in hydrophilic hydroxyl groups and is easy to modify, but the silicon dioxide is easy to agglomerate in rubber in a nanoparticle state, the formation of the agglomerates limits the exertion of the reinforcing effect of the silicon dioxide on the rubber, and the silicon dioxide is not beneficial to obtaining a high-performance hydrogenated nitrile butadiene rubber composite material, so that the large-scale application of the hydrogenated nitrile butadiene rubber is not facilitated.
The silicon dioxide nano composite filler with high efficiency, high dispersibility and strong stability is developed, is applied to a hydrogenated nitrile-butadiene rubber reinforcing system, and has very important theoretical value and practical significance for the application of high-performance hydrogenated nitrile-butadiene rubber composite materials.
Therefore, the molybdenum disulfide/silicon dioxide nano reinforcing agent (MoS) which is used for a hydrogenated nitrile rubber reinforcing system, has high efficiency and high stability and keeps high dispersity in rubber2/SiO2) And the preparation method thereof become a technical problem which needs to be solved urgently in the technical field.
Disclosure of Invention
The invention aims to provide a molybdenum disulfide/silicon dioxide reinforcing agent for hydrogenated nitrile rubber, which has the characteristics of high dispersibility, high efficiency and good stability.
The above object of the present invention is achieved by the following technical solutions:
the silicon dioxide nano composite reinforcing agent for hydrogenated nitrile rubber uses molybdenum disulfide as a carrier of nano silicon dioxide, simultaneously the molybdenum disulfide is a reinforcing additive, the nano silicon dioxide is a main reinforcing component, and the mass ratio of the reinforcing additive to the nano silicon dioxide is as follows: molybdenum disulfide: nano silica is 0.3: 30-1.2: 30.
preferably, the molybdenum disulfide is layered molybdenum disulfide prepared by a solvent sonication method.
Preferably, the nano-silica is loaded on the surface of the layered molybdenum disulfide in a highly dispersed manner to form a stress dissipation center.
Preferably, the stress dissipation center is a nano material consisting of nano silicon dioxide and molybdenum disulfide, the particle size of the nano silicon dioxide is 10-20 nm, and the side length of the molybdenum disulfide is 400-1000 nm.
The invention also aims to provide a preparation method of the silica nano reinforcing agent for the hydrogenated nitrile rubber.
The above object of the present invention is achieved by the following technical solutions:
a preparation method of a silicon dioxide nano composite reinforcing agent for hydrogenated nitrile rubber comprises the following steps:
(1) adding molybdenum disulfide into a reaction device, then adding an aqueous solution of hexadecyl trimethyl ammonium bromide, and performing ultrasonic dispersion to obtain dispersed layered molybdenum disulfide;
(2) adding an aqueous solution of soluble silicate into the dispersed layered molybdenum disulfide obtained in the step (1) to enable the mass ratio of molybdenum disulfide to silicate in the mixed solution to be 1: 200-5: 200, and stirring to obtain the mixed solution;
(3) heating the mixed solution obtained in the step (2) to 75-90 ℃ under the condition of stirring, adjusting the pH of the mixed solution to 5-6 by using dilute sulfuric acid, adding absolute ethyl alcohol after stabilization, and reacting to obtain molybdenum disulfide/silicon dioxide slurry;
(4) and (4) sequentially using deionized water and ethanol as detergents to carry out centrifugal separation washing on the molybdenum disulfide/silicon dioxide slurry obtained in the step (3) until the slurry is neutral to obtain molybdenum disulfide/silicon dioxide nano particles, and drying the molybdenum disulfide/silicon dioxide nano particles in an oven to obtain the target reinforcing agent molybdenum disulfide/silicon dioxide nano reinforcing agent (MoS)2/SiO2) (i.e., silica nanocomposite reinforcement).
Preferably, the molybdenum disulfide in the step (1) is lamellar molybdenum disulfide prepared by a solvent ultrasonic method.
Preferably, the mass of the layered molybdenum disulfide in the step (1) is 0.3-1.2 g.
Preferably, the concentration of the aqueous solution of cetyltrimethylammonium bromide in the step (1) is 0.03 mol/l.
Preferably, the soluble silicate in the step (2) is sodium silicate.
Preferably, in the aqueous solution of the silicate in the step (2), the concentration of silicate ions is 2.5 mol/l.
Preferably, the ultrasonic dispersion time in the step (1) is 2-3 hours.
Preferably, the stirring in the step (2) is magnetic stirring or mechanical stirring, and the stirring time is 0.5-1 hour.
Preferably, the concentration of the dilute sulfuric acid solution in the step (3) is 1-1.2 mol/L.
Preferably, the heating temperature in the step (3) is 85 ℃.
Preferably, the volume ratio of the absolute ethyl alcohol added in the step (3) to the mixed solution obtained in the step (2) is 1: 1-1: 2.
Preferably, the reaction time after the addition of the absolute ethanol in the step (3) is 0.5 to 1.5 hours, preferably 1 hour.
Preferably, the drying temperature of the oven in the step (4) is 60 ℃, and the drying time is 22-26 hours.
Has the advantages that:
the invention relates to a molybdenum disulfide/silicon dioxide nano reinforcing agent (MoS) for hydrogenated nitrile rubber2/SiO2) The hydrogenated nitrile rubber can be efficiently reinforced, the silicon dioxide in the reinforcing agent is in a high-dispersity nanoparticle form and is dispersed on the surface of the molybdenum disulfide, the silicon dioxide and the molybdenum disulfide have a synergistic effect, and the reinforcing effect is remarkable.
The method adopts sodium silicate as a silicon dioxide precursor and sulfuric acid as a precipitator, and prepares the molybdenum disulfide/silicon dioxide nano reinforcing agent (MoS) by an in-situ precipitation method2/SiO2). In addition, the layered molybdenum disulfide is added in the preparation process, so that silicon dioxide nano particles can directly grow on the surface of the molybdenum disulfide, the agglomeration phenomenon of nano fillers in rubber is reduced, the nano fillers with double components of molybdenum disulfide and silicon dioxide can play a role in synergistic reinforcement, the reinforcement efficiency of the fillers is enhanced, and the reinforcing agent is more stable and efficient. The prepared double-component nano reinforcing agent has the advantages of stability, high efficiency, environmental protection, remarkable effect and the like, and can promote the further development of a hydrogenated nitrile butadiene rubber reinforcing system.
The invention can greatly improve the reinforcing efficiency of the reinforcing agent and the utilization rate of molybdenum disulfide, promote the development of a hydrogenated nitrile-butadiene rubber reinforcing system and promote the development of special elastomers.
The invention is further illustrated by the following figures and specific examples, which are not meant to limit the scope of the invention.
Drawings
FIG. 1 shows a molybdenum disulfide/silica nano reinforcing agent (MoS) according to example 1 of the present invention2/SiO2) An infrared spectrum of (1).
FIG. 2 shows a molybdenum disulfide/silica nano reinforcing agent (MoS) according to example 1 of the present invention2/SiO2) Transmission electron micrograph (D).
FIG. 3 shows a molybdenum disulfide/silica nano reinforcing agent (MoS) according to example 1 of the present invention2/SiO2) The reinforcing performance diagram of the mechanical property of the hydrogenated nitrile-butadiene rubber.
Detailed Description
Example 1
(1) 0.3g of commercially available layered molybdenum disulfide (either growth or exfoliation) was weighed out, the growth starting material included ammonium tetrathiomolybdate ((NH)4)2MoS4) Molybdenum (Mo) and molybdenum trioxide (MoO)3) The stripping preparation comprises micro-mechanical stripping, liquid phase ultrasonic method, namely solvent ultrasonic method, lithium ion intercalation method, electrochemical lithium ion intercalation method and the like, and the lamellar molybdenum disulfide prepared by the solvent ultrasonic method is preferably selected) is put into a 2000ml three-necked bottle, and 500ml of commercial hexadecyl trimethyl ammonium bromide aqueous solution (6g CTAB,12 g/L CTAB/H) is added2O), performing ultrasonic treatment at room temperature for 2-3 hours to fully disperse the molybdenum disulfide in the hexadecyl trimethyl ammonium bromide aqueous solution;
(2) 200ml of a commercially available aqueous sodium silicate solution (30g of SiO) were added to a three-necked flask with mechanical stirring2150 g/L of Na2SiO3/H2O), wherein the sodium silicate is a precursor of silicon dioxide, and can help to generate small and uniform silicon dioxide nanoparticles due to the large concentration of the aqueous solution, and the small and uniform silicon dioxide nanoparticles are fully stirred to obtain a mixed solution;
(3) heating the mixed solution in the step (2) to 85 ℃ under mechanical stirring, continuing stirring, and using a commercial dilute sulfuric acid solution (H)2SO4/H2O) adjusting the pH of the mixed solution obtained in step (2) to 5.5 and maintaining the pH for 0.5 hour, then adding 300ml of commercially available absolute ethanol while stirring, and reacting for 1 hour to obtain a molybdenum disulfide/silica slurry；
(4) Cooling to room temperature after reaction, respectively using commercially available ethanol and water, centrifugally washing, detecting whether the solution is neutral by using pH test paper, after washing, putting the obtained solid into an oven, drying at 60 ℃ for 12 hours to obtain the target reinforcing agent (MoS)2/SiO2)1。
Example 2
(1) 0.6g of commercially available layered molybdenum disulfide was weighed into a 2000ml three-necked flask, and 500ml of commercially available aqueous cetyltrimethylammonium bromide (6g CTAB,12 g/L CTAB/H) was added2O), performing ultrasonic treatment at room temperature for 2-3 hours to fully disperse the molybdenum disulfide in the hexadecyl trimethyl ammonium bromide aqueous solution;
(2) 200ml of a commercially available aqueous sodium silicate solution (30g of SiO) were added to a three-necked flask with mechanical stirring2，150g/L Na2SiO3/H2O), wherein the sodium silicate is a precursor of silicon dioxide, and can help to generate small and uniform silicon dioxide nanoparticles due to the large concentration of the aqueous solution, and the mixed solution is obtained by fully stirring;
(3) heating the mixed solution in the step (2) to 85 ℃ under mechanical stirring, continuing stirring, and using a commercial dilute sulfuric acid solution (H)2SO4/H2O) adjusting the pH of the mixed solution obtained in step (2) to 5.5, maintaining the pH for 0.5 hour, adding 300ml of commercially available absolute ethanol under stirring, and reacting for 1 hour to obtain a molybdenum disulfide/silica slurry;
(4) cooling to room temperature after reaction, respectively using commercially available ethanol and water, centrifugally washing, detecting whether the solution is neutral by using pH test paper, after washing, putting the obtained solid into an oven, drying at 60 ℃ for 12 hours to obtain the target reinforcing agent (MoS)2/SiO2)2。
Example 3
(1) 0.9g of commercially available layered molybdenum disulfide was weighed into a 2000ml three-necked flask, and 500ml of commercially available cetyltrimethylammonium bromide aqueous solution (6g CTAB,12 g/L CTAB/H) was added2O), performing ultrasonic treatment at room temperature for 2-3 hours to fully disperse the molybdenum disulfide in the hexadecyl trimethyl ammonium bromide aqueous solution;
(2) machine with a movable working part200ml of a commercially available aqueous sodium silicate solution (30g of SiO) was added to a three-necked flask with stirring2，150g/LNa2SiO3/H2O), wherein the sodium silicate is a precursor of silicon dioxide, the concentration of the aqueous solution is high, which can help to generate small and uniform silicon dioxide nano-particles, and the mixed solution is obtained by fully stirring;
(3) heating the mixed solution in the step (2) to 85 ℃ under mechanical stirring, continuing stirring, and using a commercial dilute sulfuric acid solution (H)2SO4/H2O) adjusting the pH value of the mixed solution obtained in the step (2) to 5.5, maintaining the pH value for 0.5 hour, adding 300ml of commercial absolute ethyl alcohol under stirring, and reacting for 1 hour to obtain molybdenum disulfide/silicon dioxide slurry;
(4) cooling to room temperature after reaction, respectively using commercially available ethanol and water, centrifugally washing, detecting whether the solution is neutral by using pH test paper, after washing, putting the obtained solid into an oven, drying at 60 ℃ for 12 hours to obtain the target reinforcing agent (MoS)2/SiO2)3。
Example 4
(1) Weighing 1.2g of commercially available layered molybdenum disulfide into a 2000ml three-necked flask, and adding 500ml of commercially available cetyltrimethylammonium bromide aqueous solution (6g CTAB,12 g/L CTAB/H)2O), performing ultrasonic treatment at room temperature for 2-3 hours to fully disperse the molybdenum disulfide in the hexadecyl trimethyl ammonium bromide aqueous solution;
(2) 200ml of a commercially available aqueous sodium silicate solution (30g SiO) was added to a three-necked flask with mechanical stirring2，150g/LNa2SiO3/H2O), wherein the sodium silicate is a precursor of silicon dioxide, the concentration of the aqueous solution of the sodium silicate is high, and the sodium silicate can help to generate small and uniform silicon dioxide nano-particles, and the small and uniform silicon dioxide nano-particles are fully stirred to obtain a mixed solution;
(3) heating the mixed solution in the step (2) to 85 ℃ under mechanical stirring, continuing stirring, and using a commercial dilute sulfuric acid solution (H)2SO4/H2O) adjusting the pH value of the mixed solution obtained in the step (2) to 5.5, maintaining the pH value for 0.5 hour, adding 300ml of commercial absolute ethyl alcohol under stirring, and reacting for 1 hour to obtain molybdenum disulfide/silicon dioxide slurry;
(4) cooling to room temperature after reaction, respectively using commercially available ethanol and water, centrifugally washing, detecting whether the solution is neutral by using pH test paper, after washing, putting the obtained solid into an oven, and drying at 60 ℃ for 12 hours to obtain the target reinforcing agent (MoS)2/SiO2)4。
Comparative example 1
(1) 0.3g of commercial molybdenum disulfide was weighed into a 2000ml three-necked flask and 500ml of commercial aqueous cetyltrimethylammonium bromide (6g CTAB,12 g/L CTAB/H) was added2O), performing ultrasonic treatment at room temperature for 2-3 hours to fully disperse the reduced molybdenum disulfide oxide in the hexadecyl trimethyl ammonium bromide aqueous solution;
(2) 30g of commercial silicon dioxide dispersion (30g/200ml SiO) were added to a three-necked flask with mechanical stirring2/H2O) fully stirring to obtain a mixed solution;
(3) under the mechanical stirring, adding 300ml of commercial absolute ethyl alcohol, and reacting for 1 hour to obtain molybdenum disulfide/silicon dioxide slurry;
(4) after the reaction is finished, respectively using commercially available ethanol and water, centrifugally washing, using pH test paper to detect whether the reaction is neutral, after the reaction is finished, placing the obtained solid into an oven, drying at 60 ℃ for 12 hours to obtain the target reinforcing agent (MoS)2/SiO2)5。
The structural characterization of the products prepared in examples 1 to 4 proves that the products are prepared by using layered molybdenum disulfide as a carrier, and silica nanoparticles are loaded on the surface of the molybdenum disulfide, wherein a mechanical dissipation center (stress dissipation center) is a nano material consisting of nano silica and molybdenum disulfide, the particle size of the nano silica is 10-20 nm, the side length of the molybdenum disulfide is 400-1000 nm, and the observation of an electron microscope shows that the silica nanoparticles are uniformly distributed on the surface of the molybdenum disulfide.
Molybdenum disulfide/silica reinforcing agent (MoS) prepared in example 1 of the present invention2/SiO2)1, infrared spectrum detection is carried out, and the spectrum is shown in figure 1.
Samples of molybdenum disulfide/silica at wave number 3400cm-1The broad peak at the position (A) is a stretching vibration absorption peak of-O-H on the surface of silica, and the wave number is 1100-1The strong peak appearing at the position of (a) is a characteristic absorption peak of the Si-O-Si chemical bond of silica.
Molybdenum disulfide/silica reinforcing agent (MoS) prepared in example 1 of the present invention was subjected to a 120KV transmission electron microscope of HT7700 type by Hitachi, Japan2/SiO2) The amplification of 1 was 20000 times, and the results are shown in FIG. 2. By adding molybdenum disulfide/silicon dioxide reinforcing agent (MoS)2/SiO2)1, the silicon dioxide is loaded on the layered molybdenum disulfide in a nano particle form and is uniformly distributed, and the particle size of the silicon dioxide nano particles is 10-20 nanometers.
Molybdenum disulfide/silica reinforcing agent (MoS) prepared in example 1 of the present invention2/SiO2)1, detecting the mechanical property of the reinforced hydrogenated nitrile-butadiene rubber. Preparing molybdenum disulfide/silicon dioxide reinforced hydrogenated nitrile rubber compound by a mechanical blending method, and vulcanizing at 170 ℃ for 5 minutes by a flat vulcanizing instrument to obtain molybdenum disulfide/silicon dioxide reinforced hydrogenated nitrile rubber vulcanizate, wherein the mass ratio of the reinforcing agent to the hydrogenated nitrile rubber is 30: 100. the static mechanical properties of the vulcanized rubber are tested by using a CMT4203 type electronic tensile machine of SANS, the testing method conforms to the standard sample preparation and measurement of GB/T528-.
As can be seen in FIG. 3, the molybdenum disulfide/silica reinforcement (MoS) prepared in example 1 of the present invention2/SiO2)1 has better mechanical property reinforcing property, and 30 parts of prepared molybdenum disulfide/silicon dioxide reinforcing agent (MoS) is added into an HNBR rubber system2/SiO2)1, the mechanical property of the rubber can be greatly improved. The test was carried out by first preparing a molybdenum disulfide/silica-hydrogenated nitrile rubber material (MoS)2/SiO2HNBR) and hydrogenated nitrile rubber material without filler (HNBR), the addition of molybdenum disulfide/silica reinforcement (MoS) being then measured separately2/SiO2)1 and the mechanical properties of the rubber material without the reinforcing agent, and stretching the rubber material in a rubber stretching mode.
According to the method, hexadecyl trimethyl ammonium bromide aqueous solution is utilized to carry out intercalation dispersion on layered molybdenum disulfide under the ultrasonic action, sodium silicate is used as a silicon dioxide precursor, silicic acid and ions are firstly adsorbed on the surface of the layered molybdenum disulfide, the pH value is adjusted by using sulfuric acid, and silicon dioxide nano particles grow in situ on the surface of the molybdenum disulfide through an in-situ precipitation method. The loading effect of the molybdenum disulfide can effectively disperse the silicon dioxide nano particles. In addition, the molybdenum disulfide/silicon dioxide nano composite material is added into rubber, and the molybdenum disulfide can effectively prevent the silicon dioxide from agglomerating in the rubber. According to the invention, the layered molybdenum disulfide is added in the preparation process, so that nano silicon dioxide particles can be highly dispersed on the molybdenum disulfide, the agglomeration phenomenon of nano fillers in rubber is reduced, the nano fillers with double components of molybdenum disulfide and silicon dioxide can play a role in synergistic reinforcement, the reinforcement efficiency of the fillers is enhanced, and the reinforcing agent is more stable and efficient.
The prepared double-component nano reinforcing agent has the advantages of stability, high efficiency, environmental protection, remarkable effect and the like, and can promote the further development of a hydrogenated nitrile butadiene rubber reinforcing system.
Claims (10)
1. The silicon dioxide nano composite reinforcing agent for hydrogenated nitrile rubber uses molybdenum disulfide as a carrier of nano silicon dioxide, simultaneously the molybdenum disulfide is a reinforcing additive, the nano silicon dioxide is a main reinforcing component, and the mass ratio of the reinforcing additive to the nano silicon dioxide is as follows: molybdenum disulfide: nano silica is 0.3: 30-1.2: 30.
2. the silica nanocomposite reinforcement for hydrogenated nitrile rubber according to claim 1, wherein: the molybdenum disulfide is lamellar molybdenum disulfide prepared by a solvent ultrasonic method.
3. The silica nanocomposite reinforcement for hydrogenated nitrile rubber according to claim 2, wherein: the nano silicon dioxide is loaded on the surface of the layered molybdenum disulfide to form a stress dissipation center.
4. The silica nanocomposite reinforcement for hydrogenated nitrile rubber according to claim 3, wherein: the stress dissipation center is made of a nano material consisting of nano silicon dioxide and molybdenum disulfide, the particle size of the nano silicon dioxide is 10-20 nm, and the side length of the molybdenum disulfide is 400-1000 nm.
5. A process for the preparation of silica nanocomposite reinforcement for hydrogenated nitrile rubber according to any of claims 1 to 4, comprising the steps of:
(1) adding layered molybdenum disulfide into a reaction device, then adding hexadecyl trimethyl ammonium bromide aqueous solution, and performing ultrasonic dispersion to obtain dispersed molybdenum disulfide;
(2) respectively adding soluble silicate solution into the dispersed molybdenum disulfide obtained in the step (1), so that the mass ratio of molybdenum disulfide to silicate in the mixed solution is 1: 200-5: 200, stirring to obtain a mixed solution;
(3) heating the mixed solution obtained in the step (2) to 75-95 ℃ under the condition of stirring, adjusting the pH of the mixed solution to 5-6 by using dilute sulfuric acid, adding absolute ethyl alcohol after stabilization, and reacting to obtain molybdenum disulfide/silicon dioxide slurry;
(4) and (4) taking the deionized water and ethanol as detergents in sequence, carrying out centrifugal separation washing on the molybdenum disulfide/silicon dioxide slurry obtained in the step (3) until the slurry is neutral to obtain molybdenum disulfide/silicon dioxide nano particles, and drying to obtain the target reinforcing agent molybdenum disulfide/silicon dioxide nano reinforcing agent.
6. The method for preparing silica nano composite reinforcing agent for hydrogenated nitrile rubber according to claim 5, wherein: the molybdenum disulfide in the step (1) is lamellar molybdenum disulfide prepared by a solvent ultrasonic method.
7. The method for preparing silica nano composite reinforcing agent for hydrogenated nitrile rubber according to claim 6, wherein: the soluble silicate in the step (2) is sodium silicate.
8. The method for preparing silica nano composite reinforcing agent for hydrogenated nitrile rubber according to claim 7, wherein: the concentration of silicate ions in the aqueous solution of silicate in the step (2) is 2.5 mol/l.
9. The method for preparing silica nanocomposite reinforcing agent for hydrogenated nitrile rubber according to claim 8, wherein: and (2) in the step (1), the ultrasonic dispersion time is 2-3 hours.
10. The method for preparing silica nanocomposite reinforcing agent for hydrogenated nitrile rubber according to claim 9, wherein: the stirring in the step (2) is mechanical stirring or ultrasonic stirring, and the stirring time is 0.5-1 hour; the concentration of the dilute sulfuric acid solution in the step (3) is 1-1.2 mol/L; the volume ratio of the absolute ethyl alcohol added in the step (3) to the mixed solution obtained in the step (2) is 1: 1-1: 2; the reaction time after adding the absolute ethyl alcohol in the step (3) is 1 hour; and (4) drying in an oven at 60 ℃ for 22-26 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113480789A (en) * | 2021-06-29 | 2021-10-08 | 北京化工大学 | Double-component composite reinforcing agent for rubber and preparation method thereof |
| CN113527776A (en) * | 2021-08-06 | 2021-10-22 | 中铁工程装备集团有限公司 | Rubber composite material, preparation method and application in shield machine main driving system sealing |
| CN114716743A (en) * | 2022-03-25 | 2022-07-08 | 成都飞机工业（集团）有限责任公司 | Hydrogenated nitrile rubber reinforcing agent and preparation method and application thereof |
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| CN113480789A (en) * | 2021-06-29 | 2021-10-08 | 北京化工大学 | Double-component composite reinforcing agent for rubber and preparation method thereof |
| CN113527776A (en) * | 2021-08-06 | 2021-10-22 | 中铁工程装备集团有限公司 | Rubber composite material, preparation method and application in shield machine main driving system sealing |
| CN114716743A (en) * | 2022-03-25 | 2022-07-08 | 成都飞机工业（集团）有限责任公司 | Hydrogenated nitrile rubber reinforcing agent and preparation method and application thereof |
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| CN111423622B (en) | 2021-05-25 |
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