CN109054084B - Modified zinc oxide-carbon fiber composite fiber for rubber and preparation method thereof - Google Patents
Modified zinc oxide-carbon fiber composite fiber for rubber and preparation method thereof Download PDFInfo
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- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses a modified zinc oxide-carbon fiber composite fiber for rubber and a preparation method thereof, the prepared modified zinc oxide-carbon fiber composite fiber has higher dispersibility and stronger interface bonding force with a rubber substrate, and when the fiber is applied to a rubber sealing ring, the rubber sealing ring has higher tensile strength and elongation at break and better mechanical property, and meanwhile, the fatigue resistance of the rubber sealing ring is greatly improved; the carbon fiber is activated, so that the surface activity of the carbon fiber is improved, the adhesion of zinc oxide on the surface of the carbon fiber is promoted, after the zinc oxide is adhered, the agglomeration phenomenon of the zinc oxide is improved, the dispersion degree of the zinc oxide is improved, the interface bonding force between the carbon fiber and a rubber substrate is improved, the acting point is provided for the carbon fiber, the interface bonding force between the carbon fiber and the rubber substrate is improved, the compatibility between the composite fiber and the rubber substrate is further promoted under the action of the fatty alcohol-polyoxyethylene ether, and the mechanical property and the fatigue resistance of rubber are improved.
Description
Technical Field
The invention belongs to the technical field, and particularly relates to a modified zinc oxide-carbon fiber composite fiber for rubber and a preparation method thereof.
Background
The rubber sealing leather ring is an annular cover composed of one or more parts, is fixed on one ferrule or gasket of the bearing and is in contact with the other ferrule or gasket or forms a narrow labyrinth gap to prevent lubricating oil from leaking and foreign objects from invading, and is made of rubber elastomers (nitrile butadiene, fluororubber, silica gel, natural rubber and other rubbers) as main materials, and a rubber reinforcement body as a framework, and different elastomers and frameworks can be selected according to customer requirements to be processed into rubber membranes with different thicknesses. Zinc oxide is used as a traditional rubber filler, mainly as an activator in rubber and secondly as a reinforcing agent and a coloring agent, and the property of zinc oxide influences the performance of zinc oxide in rubber. In practical application, the nano zinc oxide has hydrophilic and oleophobic properties and strong polarity, is easy to agglomerate in the mixing process and has poor dispersibility, so that the fatigue resistance of the rubber is poor and the comprehensive performance needs to be improved.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a modified zinc oxide-carbon fiber composite fiber for rubber, which has good dispersibility and can improve rubber fatigue resistance, and a preparation method thereof.
The invention is realized by the following technical scheme:
the modified zinc oxide-carbon fiber composite fiber for rubber is characterized by being prepared from the following raw materials in parts by weight:
5-10 parts of carbon fiber, 0.5-1 part of sodium pyrophosphate, 20-30 parts of fatty alcohol-polyoxyethylene ether, 2-4 parts of polyacrylamide and Zn2+40-50 parts of mixed liquid.
Further, the preparation method comprises the following steps:
(1) adding carbon fibers into a sulfuric acid solution with the volume of 30-50 times that of the carbon fibers, performing ultrasonic treatment for 40-60min at 50-60 ℃, filtering, transferring into a microwave device, performing ultrasonic treatment for 10-15s at 2200W of 2000-5 ℃, taking out, placing into a sodium hydroxide solution with the volume of 50-100 times that of the carbon fibers, performing ultrasonic treatment for 40-60min at 2-5 ℃, filtering, washing to be neutral by using distilled water, and then placing into a vacuum drying box with the temperature of 110-120 ℃ for drying to obtain activated carbon fibers;
(2) adding the carbon fiber obtained in the step (1) into an alcoholic solution with the volume 40-80 times of that of the carbon fiber, then adding sodium pyrophosphate, stirring for 30-40min at the temperature of 20-30 ℃ and the speed of 1000-2+Continuously stirring the mixed solution for 10-20min, treating the obtained substance for 40-50min by using 500-600W microwave, then transferring the treated substance into a reaction kettle, reacting for 10-12h at the temperature of 155-160 ℃, then filtering, washing and drying in vacuum at the temperature of 80-90 ℃;
(3) and (3) putting the product obtained in the step (2) and fatty alcohol-polyoxyethylene ether into a ball mill for ball milling for 5-10min, then adding polyacrylamide, continuing ball milling for 5-10min, then adding the obtained slurry into n-propanol with the volume of 50-100 times of that of the slurry, carrying out ultrasonic treatment for 3-5h at 35-45Hz, and carrying out spray drying on the obtained slurry to obtain the modified zinc oxide-carbon fiber composite fiber.
Further, the mass fraction of the sulfuric acid solution in the step (1) is 30-35%.
Further, the ultrasonic condition of the step (1) is 60-65 Hz.
Further, the mass fraction of the sodium hydroxide solution in the step (1) is 20-30%.
Further, the Zn is contained in the step (2)2+The preparation method of the mixed solution comprises the following steps: according to triethanolamine with Zn2+The mass ratio is 0.5-1.5:1, triethanolamine is slowly added into Zn under the stirring of 600 plus 800rpm2+In a salt solution, the Zn2+The salt solution is one of zinc acetate, zinc nitrate and zinc chloride solution with the concentration of 0.8-1.2 mol/L.
Further, the alcoholic solution in the step (2) is prepared from propylene glycol, polyethylene glycol and ethanol according to a mass ratio of 0.2-0.3: 0.05-0.1: 1.
Further, the linear speed of the ball mill in the step (3) is 1-2 m/s.
The invention has the beneficial effects that: the modified zinc oxide-carbon fiber composite fiber prepared by the invention has higher dispersibility and stronger interface bonding force with a rubber substrate, and when the modified zinc oxide-carbon fiber composite fiber is applied to a rubber sealing ring, the rubber sealing ring has higher tensile strength and elongation at break and better mechanical property, and meanwhile, the fatigue resistance of the rubber sealing ring is greatly improved; the carbon fiber is activated, so that the surface activity of the carbon fiber is improved, the adhesion of zinc oxide on the surface of the carbon fiber is promoted, after the zinc oxide is adhered, the agglomeration phenomenon of the zinc oxide is improved, the dispersion degree of the zinc oxide is improved, the interface bonding force between the carbon fiber and a rubber substrate is improved, the acting point is provided for the carbon fiber, the interface bonding force between the carbon fiber and the rubber substrate is improved, the compatibility between the composite fiber and the rubber substrate is further promoted under the action of the fatty alcohol-polyoxyethylene ether, and the mechanical property and the fatigue resistance of rubber are improved.
Detailed Description
The invention is illustrated by the following specific examples, which are not intended to be limiting.
Example 1
The modified zinc oxide-carbon fiber composite fiber for rubber is characterized by being prepared from the following raw materials in parts by weight:
5 carbon fibers, 0.5 sodium pyrophosphate, 20 fatty alcohol-polyoxyethylene ether, 2 polyacrylamide and Zn2+And (3) mixing the solution 40.
Further, the preparation method comprises the following steps:
(1) adding carbon fibers into a sulfuric acid solution with the volume 30 times that of the carbon fibers, performing ultrasonic treatment at 50 ℃ for 40min, filtering, transferring the carbon fibers into a microwave device, performing treatment at 2000W for 10s, taking out the carbon fibers, putting the carbon fibers into a sodium hydroxide solution with the volume 50 times that of the carbon fibers, performing ultrasonic treatment at 2 ℃ for 40min, filtering, washing the carbon fibers to be neutral by using distilled water, and drying the carbon fibers in a vacuum drying box at 110 ℃ to obtain activated carbon fibers;
(2) adding the carbon fiber obtained in the step (1) into an alcoholic solution with the volume 40 times of that of the carbon fiber, then adding sodium pyrophosphate, stirring at 20 ℃ and 1000rpm for 30min, and then adding Zn-containing solution2+Mixing the solution, stirring for 10min, treating the resultant with 500W microwave for 40min, transferring into a reaction kettle, reacting at 155 deg.C for 10h, filtering, washing, and vacuum drying at 80 deg.C;
(3) and (3) putting the product obtained in the step (2) and fatty alcohol-polyoxyethylene ether into a ball mill for ball milling for 5min, then adding polyacrylamide, continuing ball milling for 5min, then adding the obtained slurry into n-propanol with the volume 50 times of that of the slurry, carrying out ultrasonic treatment for 3h at 35Hz, and carrying out spray drying on the slurry to obtain the modified zinc oxide-carbon fiber composite fiber.
Further, the mass fraction of the sulfuric acid solution in the step (1) is 30%.
Further, the ultrasonic condition in the step (1) is 60 Hz.
Further, the mass fraction of the sodium hydroxide solution in the step (1) is 20%.
Further, the Zn is contained in the step (2)2+The preparation method of the mixed solution comprises the following steps: according to triethanolamine with Zn2+The weight ratio is 0.5:1, triethanolamine is slowly added into Zn under the stirring of 600rpm2+In a salt solution, the Zn2+The salt solution is one of zinc acetate, zinc nitrate and zinc chloride solution with the concentration of 0.8 mol/L.
Further, the alcoholic solution in the step (2) is prepared from propylene glycol, polyethylene glycol and ethanol according to a mass ratio of 0.2: 0.05: 1.
Further, the linear speed of the ball mill in the step (3) is 1 m/s.
Example 2
The modified zinc oxide-carbon fiber composite fiber for rubber is characterized by being prepared from the following raw materials in parts by weight:
carbon fiber 7, sodium pyrophosphate 0.8, fatty alcohol-polyoxyethylene ether 25, polyacrylamide 3 and Zn2+And (4) a mixed solution 45.
Further, the preparation method comprises the following steps:
(1) adding carbon fibers into a sulfuric acid solution with the volume 40 times that of the carbon fibers, carrying out ultrasonic treatment for 50min at 55 ℃, filtering, then transferring the carbon fibers into a microwave device, carrying out treatment for 12s at 2100W, taking out the carbon fibers, then putting the carbon fibers into a sodium hydroxide solution with the volume 70 times that of the carbon fibers, carrying out ultrasonic treatment for 50min at 3 ℃, filtering, washing the carbon fibers to be neutral by using distilled water, and then drying the carbon fibers in a vacuum drying box at 115 ℃ to obtain activated carbon fibers;
(2) adding the carbon fiber obtained in the step (1) into an alcoholic solution with the volume 60 times that of the carbon fiber, then adding sodium pyrophosphate, stirring at the temperature of 25 ℃ and the rpm of 1500 for 35min, and then adding Zn2+Mixing the solution, stirring for 15min, treating the resultant with 550W microwave for 45min, transferring into a reaction kettle, reacting at 158 deg.C for 11h, filtering, washing, and vacuum drying at 85 deg.C;
(3) and (3) putting the product obtained in the step (2) and fatty alcohol-polyoxyethylene ether into a ball mill for ball milling for 7min, then adding polyacrylamide, continuing ball milling for 8min, then adding the obtained slurry into n-propanol with the volume 60 times that of the slurry, carrying out ultrasonic treatment for 4h at 40Hz, and carrying out spray drying on the slurry to obtain the modified zinc oxide-carbon fiber composite fiber.
Further, the mass fraction of the sulfuric acid solution in the step (1) is 32%.
Further, the ultrasonic condition in the step (1) is 63 Hz.
Further, the mass fraction of the sodium hydroxide solution in the step (1) is 25%.
Further, the Zn is contained in the step (2)2+The preparation method of the mixed solution comprises the following steps: according to triethanolamine with Zn2+The mass ratio is 1:1, triethanolamine is slowly added into Zn under the stirring of 700rpm2+In a salt solution, the Zn2+The salt solution is one of zinc acetate, zinc nitrate and zinc chloride solution with the concentration of 1 mol/L.
Further, the alcoholic solution in the step (2) is prepared from propylene glycol, polyethylene glycol and ethanol according to a mass ratio of 0.3: 0.08: 1.
Further, the linear speed of the ball mill in the step (3) is 2 m/s.
Example 3
The modified zinc oxide-carbon fiber composite fiber for rubber is characterized by being prepared from the following raw materials in parts by weight:
10 carbon fibers, 1 sodium pyrophosphate, 30 fatty alcohol-polyoxyethylene ether, 4 polyacrylamide and Zn2+And (3) mixing the solution 50.
Further, the preparation method comprises the following steps:
(1) adding carbon fibers into a sulfuric acid solution with the volume 50 times that of the carbon fibers, carrying out ultrasonic treatment at 60 ℃ for 60min, filtering, transferring the carbon fibers into a microwave device, carrying out treatment at 2200W for 15s, taking out the carbon fibers, putting the carbon fibers into a sodium hydroxide solution with the volume 100 times that of the carbon fibers, carrying out ultrasonic treatment at 5 ℃ for 60min, filtering, washing the carbon fibers to be neutral by using distilled water, and then drying the carbon fibers in a vacuum drying box at 120 ℃ to obtain activated carbon fibers;
(2) adding the carbon fiber obtained in the step (1) into an alcoholic solution with the volume of 80 times of that of the carbon fiber, then adding sodium pyrophosphate, stirring at the temperature of 30 ℃ and the rpm of 1200 for 40min, and then adding Zn2+Continuously stirring the mixed solution for 20min, treating the obtained product with 600W microwave for 50min, transferring into a reaction kettle, reacting at 160 ℃ for 12h, filtering, washing and vacuum-drying at 90 ℃;
(3) and (3) putting the product obtained in the step (2) and fatty alcohol-polyoxyethylene ether into a ball mill for ball milling for 10min, then adding polyacrylamide, continuing ball milling for 10min, then adding the obtained slurry into n-propanol with the volume of 100 times that of the slurry, carrying out ultrasonic treatment for 5h at 45Hz, and carrying out spray drying on the slurry to obtain the modified zinc oxide-carbon fiber composite fiber.
Further, the mass fraction of the sulfuric acid solution in the step (1) is 35%.
Further, the ultrasonic condition in the step (1) is 65 Hz.
Further, the mass fraction of the sodium hydroxide solution in the step (1) is 30%.
Further, the Zn is contained in the step (2)2+The preparation method of the mixed solution comprises the following steps: according to triethanolamine with Zn2+The mass ratio is 1.5:1, triethanolamine is slowly added into Zn under the stirring of 800rpm2+In a salt solution, the Zn2+The salt solution is one of zinc acetate, zinc nitrate and zinc chloride solution with the concentration of 1.2 mol/L.
Further, the alcoholic solution in the step (2) is prepared from propylene glycol, polyethylene glycol and ethanol according to a mass ratio of 0.3: 0.1: 1.
Further, the linear speed of the ball mill in the step (3) is 2 m/s.
Comparative example 1
This comparative example is similar to example 2 except that the process step of step (1) is omitted.
Comparative example 2
This comparative example, compared with example 2, omits the operation of the microwave treatment in step (2), and the process steps are the same except for this.
Comparative example 3
Compared with the embodiment 2, the method of the comparative embodiment omits the addition of the fatty alcohol-polyoxyethylene ether, and has the same steps except the addition.
Experiment: 10 parts of the products obtained in the examples and the comparative examples, 80 parts of nitrile rubber, 2 parts of sulfur, 1.5 parts of antioxidant RD, 2 parts of stearic acid and 20 parts of carbon black are taken to prepare rubber sealing rings, and then the tensile strength, the elongation at break and the dynamic fatigue resistance of each group of the obtained rubber sealing rings are tested:
and (3) testing tensile strength: the test was carried out according to the national standard GB/T528-1998.
Elongation at break test: the detection is carried out according to the national standard GB/T528-1998.
And (3) testing the dynamic fatigue resistance: the test was carried out according to the national standard GB/T15584-1995, with a preload of 4900N, an amplitude of. + -. 3mm and a frequency of 3 Hz.
The results are shown in table 1:
TABLE 1
As can be seen from Table 1, when the modified zinc oxide-carbon fiber composite fiber prepared by the invention is used for a rubber sealing ring, the tensile strength and the elongation at break are higher, the mechanical property is better, and meanwhile, the fatigue resistance is also greatly improved.
Claims (7)
1. The modified zinc oxide-carbon fiber composite fiber for rubber is characterized by being prepared from the following raw materials in parts by weight: 5-10 parts of carbon fiber, 0.5-1 part of sodium pyrophosphate, 20-30 parts of fatty alcohol-polyoxyethylene ether, 2-4 parts of polyacrylamide and 40-50 parts of Zn-containing mixed solution, wherein the preparation method comprises the following steps: (1) adding carbon fibers into a sulfuric acid solution with the volume of 30-50 times that of the carbon fibers, carrying out ultrasonic treatment for 40-60min at 50-60 ℃, filtering, transferring into a microwave device, carrying out ultrasonic treatment for 10-15s at 2000-2200W, taking out, placing into a sodium hydroxide solution with the volume of 50-100 times that of the carbon fibers, carrying out ultrasonic treatment for 40-60min at 2-5 ℃, filtering, washing to be neutral by using distilled water, and then placing into a vacuum drying box with the temperature of 110-120 ℃ for drying to obtain activated carbon fibers; (2) adding the carbon fiber obtained in the step (1) into an alcohol solution with the volume 40-80 times of that of the carbon fiber, then adding sodium pyrophosphate, stirring at 20-30 ℃ and 1200rpm for 30-40min, then adding a Zn-containing mixed solution, continuing stirring for 10-20min, treating the obtained substance for 40-50min by using 500-600W microwave, then transferring the treated substance into a reaction kettle, reacting at 155-160 ℃ for 10-12h, then filtering, washing and vacuum drying at 80-90 ℃; and (3) putting the product obtained in the step (2) and fatty alcohol-polyoxyethylene ether into a ball mill for ball milling for 5-10min, adding polyacrylamide, continuing ball milling for 5-10min, adding the obtained slurry into n-propanol with the volume of 50-100 times of that of the slurry, performing ultrasonic treatment for 3-5h at 35-45Hz, and performing spray drying to obtain the modified zinc oxide-carbon fiber composite fiber.
2. The modified zinc oxide-carbon fiber composite fiber for rubber as claimed in claim 1, wherein the mass fraction of the sulfuric acid solution in the step (1) is 30-35%.
3. The modified zinc oxide-carbon fiber composite fiber for rubber as claimed in claim 1, wherein the ultrasonic condition in step (1) is 60-65 Hz.
4. The modified zinc oxide-carbon fiber composite fiber for rubber as claimed in claim 1, wherein the sodium hydroxide solution in step (1) has a mass fraction of 20-30%.
5. The modified zinc oxide-carbon fiber composite fiber for rubber according to claim 1, wherein the preparation method of the Zn-containing mixed solution in the step (2) comprises the following steps: according to the mass ratio of 0.5-1.5:1 of triethanolamine to Zn, under the stirring of 600-800rpm, slowly adding the triethanolamine into a Zn salt solution, wherein the Zn salt solution is one of zinc acetate, zinc nitrate and zinc chloride with the concentration of 0.8-1.2 mol/L.
6. The modified zinc oxide-carbon fiber composite fiber for rubber as claimed in claim 1, wherein the alcoholic solution in step (2) is prepared from propylene glycol, polyethylene glycol and ethanol in a mass ratio of 0.2-0.3: 0.05-0.1: 1.
7. The modified zinc oxide-carbon fiber composite fiber for rubber as claimed in claim 1, wherein the ball milling linear velocity in step (3) is 1-2 m/s.
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Denomination of invention: The invention relates to a modified zinc oxide carbon fiber composite fiber for rubber and a preparation method thereof Effective date of registration: 20210721 Granted publication date: 20200811 Pledgee: Hanshan County sub branch of Postal Savings Bank of China Limited Pledgor: ANHUI JINHUA ZINC OXIDE Co.,Ltd. Registration number: Y2021980006527 |