CN108794938B - One-time low-temperature vulcanized fluororubber, preparation method and fluororubber rubber roll - Google Patents
One-time low-temperature vulcanized fluororubber, preparation method and fluororubber rubber roll Download PDFInfo
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- CN108794938B CN108794938B CN201810500952.8A CN201810500952A CN108794938B CN 108794938 B CN108794938 B CN 108794938B CN 201810500952 A CN201810500952 A CN 201810500952A CN 108794938 B CN108794938 B CN 108794938B
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- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
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- C08K3/22—Oxides; Hydroxides of metals
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Abstract
The invention aims to solve the problems of energy consumption and time consumption of a fluororubber process in the prior art, provides a fluororubber vulcanized at low temperature once, a preparation method and a fluororubber roller, and belongs to the field of high polymer materials. The fluororubber provided by the invention comprises the following components in parts by mass: 100 parts of crude fluororubber, 12-18 parts of magnesium oxide, 6-10 parts of 1, 4-butanediol, 35-45 parts of spray carbon black, 8-12 parts of ethyl acetate, 0.8-1.2 parts of anti-aging agent RD and 1.5-2.5 parts of bisphenol A. The fluororubber formula provided by the invention can realize one-time low-temperature vulcanization of the fluororubber, and simultaneously still maintain the performances of the fluororubber. The preparation method reduces the energy consumption of the conventional fluororubber vulcanization process and saves the cost. All performance indexes of the fluororubber roll product prepared by the formula are superior to those of a product of a universal vulcanization system.
Description
Technical Field
The invention belongs to the field of high polymer materials, and particularly relates to one-time low-temperature vulcanized fluororubber, a preparation method and a rubber roller prepared from the fluororubber.
Background
Fluororubbers (fluororubers) are synthetic polymer elastomers containing fluorine atoms in carbon atoms in the main chain or side chains. Due to the introduction of fluorine atoms, the rubber has excellent heat resistance, oxidation resistance, oil resistance, corrosion resistance and atmospheric aging resistance, is widely applied in the fields of aerospace, aviation, automobiles, petroleum, household appliances and the like, and is a key material which cannot be replaced in national defense advanced industry.
The rubber vulcanization process is mainly a cross-linking process formed by chemical reaction of macromolecular chains. At present, all common fluororubber formulations need secondary vulcanization. Secondary vulcanization is an essential step in the production of its articles. The main purposes of carrying out the secondary vulcanization are: 1) completing the reaction of the unreacted crosslinking groups remaining after the primary vulcanization; 2) the crosslinking reaction residue generated in the primary vulcanization is removed, mainly water and carbon dioxide remaining in the fluororubber formed product, and a small amount of fluoride or fragments generated by the vulcanizing agent, etc. The secondary vulcanization can improve the mechanical property and the compression set property of the product, reduce the gas generated in the using process of the product and reduce the shrinkage rate of the product. Therefore, secondary vulcanization plays an important role in the vulcanization of fluororubbers.
The primary vulcanization is generally carried out at 160-180 ℃, and the vulcanization at 150 ℃ can also be adopted, and the secondary vulcanization is the vulcanization by raising the temperature to 250 ℃ in sections or the constant-temperature vulcanization at 230 ℃. Therefore, the production process of fluororubbers consumes much energy and time.
Disclosure of Invention
The invention aims to solve the problems of energy consumption and time consumption of a fluororubber process in the prior art, and provides a fluororubber vulcanized at low temperature once, a preparation method and a fluororubber roller. The fluororubber formula provided by the invention can realize one-time low-temperature vulcanization of the fluororubber, and simultaneously still maintain the performances of the fluororubber. The preparation method reduces the energy consumption of the conventional fluororubber vulcanization process and saves the cost. All performance indexes of the fluororubber roll product prepared by the formula are superior to those of a product of a universal vulcanization system.
One of the technical schemes of the invention is that the once-used low-temperature vulcanized fluororubber comprises the following components in parts by mass:
100 portions of crude fluororubber
12-18 parts of magnesium oxide
6-10 parts of 1, 4-butanediol
35-45 parts of spray carbon black
8-12 parts of ethyl acetate
0.8-1.2 parts of anti-aging agent RD
1.5 to 2.5 parts of bisphenol A,
wherein the Mooney viscosity of the raw fluororubber is 50-60.
The ethyl acetate in the formula plays a plasticizing role in the rubber material and replaces a softening agent. The semi-finished rubber material product using ethyl acetate is soft in colloid, good in processability, smooth in extruded rubber strip, and capable of being recycled after secondary processing, so that the yield of the product is improved. And the ethyl acetate can also play a role of an operation aid in the rubber material, so that the rubber compound is convenient to process, and the vulcanized rubber roll product has higher elasticity.
The 1, 4-butanediol in the formula plays a role of a temporary plasticizer in the processing process and participates in the vulcanization effect in the vulcanization process, so that the vulcanized rubber can be endowed with higher crosslinking density. Therefore, the application of 1, 4-butanediol not only improves the processability of the fluororubber and the quality of the product, but also reduces or replaces other materials, such as: the amount of the softening agent, the accelerator and the carbon black used, which reduces the cost in the use of the raw material.
The second technical scheme of the invention is that the preparation method of the disposable low-temperature vulcanized fluororubber comprises the following steps:
1) crushing the blocky part in each component of the once low-temperature vulcanized fluororubber into powder;
2) heating an internal mixer to 110-130 ℃, adding fluororubber raw rubber, magnesium oxide, 1, 4-butanediol and 1/2 formula parts of spray carbon black, and mixing for 5-10 minutes; then, adding the rest materials into an internal mixer to be mixed for 4-6 minutes to obtain a sizing material;
3) putting the rubber material into a vulcanizing tank, pressurizing the vulcanizing tank to 0.4-0.6 MPa, and then starting a vulcanization reaction;
the vulcanization reaction comprises the following steps:
raising the temperature of the vulcanizing tank to 100-110 ℃ within 2-2.5 hours, preserving heat and vulcanizing for 1-1.5 hours, then raising the temperature of the vulcanizing tank to 120-135 ℃, preserving heat and vulcanizing for 1.5-2 hours, then raising the temperature of the vulcanizing tank to 140-155 ℃, preserving heat and vulcanizing for 8-10 hours, and then stopping heating; and (4) recovering the vulcanizing tank to normal pressure, and naturally cooling to 50 ℃ or below to obtain the product.
After inspection, the tensile strength and the tearing strength of the fluororubber vulcanized by the method are 16-18MPa35-45KN/M, elongation at break of 300-3/1.6km。
The third technical scheme of the invention is that the fluororubber roll consists of a steel roll body and the disposable low-temperature vulcanized fluororubber outer skin positioned outside the roll body.
The preparation method of the fluororubber roll comprises the following steps:
1) crushing the blocky part in each component of the once low-temperature vulcanized fluororubber into powder;
2) heating an internal mixer to 110-130 ℃, adding fluororubber raw rubber, magnesium oxide, 1, 4-butanediol and 1/2 formula parts of spray carbon black, and mixing for 5-10 minutes; then, adding the rest materials into an internal mixer to be mixed for 4-6 minutes to obtain a sizing material;
3) performing thin-pass treatment on the rubber material, pressing the rubber material into a sheet with the thickness of 0.3-0.7 mm, then beating the sheet into a triangular bag, repeating the process for 3-5 times, then pressing the sheet into a rubber sheet with the thickness of 5-6 mm on an open mill, and ventilating and reducing the temperature to the normal temperature to obtain a fluororubber rubber sheet;
4) coating an adhesive on the surface of a steel roller body, processing a film into an adhesive tape, and lining the adhesive tape on the surface of the roller body in an extrusion or surface mounting mode; the lined roller body is wound and wrapped by a soaked nylon cloth strip;
5) putting the wrapped rubber roller into a vulcanizing tank, and starting a vulcanization reaction after the vulcanizing tank is pressurized to 0.4-0.6 MPa;
the vulcanization reaction comprises the following steps:
raising the temperature of the vulcanizing tank to 100-110 ℃ within 2-2.5 hours, preserving heat and vulcanizing for 1-1.5 hours, then raising the temperature of the vulcanizing tank to 120-135 ℃, preserving heat and vulcanizing for 1.5-2 hours, then raising the temperature of the vulcanizing tank to 140-150 ℃, preserving heat and vulcanizing for 8-10 hours, and then stopping heating; and (4) recovering the vulcanizing tank to normal pressure, and naturally cooling to 50 ℃ to obtain the fluororubber roller.
Through inspection, the fluororubber roll prepared by the method HAs the tensile strength of 16-18MPa, the tearing strength of 35-45KN/M, the elongation at break of 300-400 percent, the Shore hardness of 70-75HA and the abrasion of 0.200-0.260 cm3/1.6km。
Compared with the prior art, the invention has the advantages that:
1. the fluororubber formula disclosed by the invention can enable linear molecular chains to form three-dimensional reticular molecular chains at a lower temperature in a short time in the vulcanization process, and the crosslinking density of the product is increased after vulcanization, so that various performance indexes of the product are superior to those of a product of a universal vulcanization system.
2. The 1, 4-butanediol in the formula of the fluororubber improves the processability of the fluororubber and the quality of products, and reduces or replaces other materials, such as: the amount of the softening agent, the accelerator and the carbon black used, which reduces the cost in the use of the raw material.
Detailed Description
Example 1
The preparation method of the disposable low-temperature vulcanized fluororubber comprises the following formula:
fluororubber raw rubber FE 2603100 parts
15 portions of magnesium oxide
8 parts of 1, 4-butanediol
Spray carbon black 40 parts
10 portions of ethyl acetate
1 part of antioxidant RD
2 parts of bisphenol A;
1) crushing the blocky part in each component of the once low-temperature vulcanized fluororubber into powder;
2) heating an internal mixer to 120 ℃, adding 100 parts of fluororubber, 15 parts of magnesium oxide, 8 parts of 1, 4-butanediol and 20 parts of spray carbon black, and mixing for 8 minutes; then, adding the rest materials into an internal mixer to be mixed for 5-6 minutes to obtain a sizing material;
3) putting the rubber material into a vulcanizing tank, pressurizing the vulcanizing tank to 0.5MP, and then starting a vulcanization reaction;
the vulcanization reaction comprises the following steps:
raising the temperature of the vulcanizing tank to 110 ℃ within 2 hours, preserving heat and vulcanizing for 1 hour, then raising the temperature of the vulcanizing tank to 130 ℃, preserving heat and vulcanizing for 2 hours, then raising the temperature of the vulcanizing tank to 145 ℃, preserving heat and vulcanizing for 9 hours, and then stopping heating; and (5) recovering the vulcanizing tank to normal pressure, and naturally cooling to 50 ℃ to obtain the product.
The test shows that the fluororubber vulcanized by the method HAs the tensile strength of 17.8MPa, the tearing strength of 41KN/M, the elongation at break of 315 percent, the Shore hardness of 74HA and the abrasion of 0.231cm31.6km, compression set (23 ℃ C. 72 h) 17%.
Comparative example 1
The preparation method of the disposable low-temperature vulcanized fluororubber comprises the following formula:
fluororubber FE 2603100 parts
15 portions of magnesium oxide
8 parts of 1, 3-propylene glycol
Spray carbon black 40 parts
Ethyl acetate 12 parts
1 part of antioxidant RD
2 parts of bisphenol A;
the preparation method is the same as example 1.
After inspection, the tensile strength of the fluororubber vulcanized by the method is 14.25 MPa, the tearing strength is 34KN/M, the elongation at break is 346 percent, the Shore hardness is 65HA, and the abrasion is 0.294cm31.6 km; the compression set was 18.4% higher than that of example 1, and the total impurity content was 48.6% higher than that of the secondary vulcanization.
Comparative example 2
The preparation method of the disposable low-temperature vulcanized fluororubber comprises the following formula:
fluororubber FE 2603100 parts
15 portions of magnesium oxide
8 parts of 1, 4-butanediol
Spray carbon black 40 parts
10 portions of ethyl formate
1 part of antioxidant RD
2 parts of bisphenol A;
the preparation method is the same as example 1.
Upon inspection, the above methodThe vulcanized fluororubber HAs the tensile strength of 13.16 MPa, the tearing strength of 35KN/M, the elongation at break of 304 percent, the Shore hardness of 62HA and the abrasion of 0.296cm31.6 km; the compression set was 22.7% higher than that of example 1, and the total impurity content was 61.3% higher than that of the secondary vulcanization.
Comparative example 3
The formula of the preparation method of the disposable low-temperature vulcanized fluororubber is the same as that of the example 1, and the method comprises the following steps:
1) crushing the blocky part in each component of the once low-temperature vulcanized fluororubber into powder;
2) heating an internal mixer to 120 ℃, adding 100 parts of fluororubber, 15 parts of magnesium oxide, 8 parts of 1, 4-butanediol and 20 parts of spray carbon black, and mixing for 10 minutes; then, adding the rest materials into an internal mixer to be mixed for 5-6 minutes to obtain a sizing material;
3) putting the rubber material into a vulcanizing tank, pressurizing the vulcanizing tank to 0.5MP, and then starting a vulcanization reaction;
the vulcanization reaction comprises the following steps:
① raising the temperature of the vulcanizing tank to 110 ℃ within 2 hours, keeping the temperature for vulcanizing for 1 hour, then raising the temperature of the vulcanizing tank to 130 ℃, keeping the temperature for vulcanizing for 2 hours, then raising the temperature of the vulcanizing tank to 150 ℃, keeping the temperature for vulcanizing for 10 hours, and then stopping heating;
② heating the vulcanizing tank to 230 ℃ and vulcanizing for 24h at constant temperature, then returning the vulcanizing tank to normal pressure and naturally cooling to 50 ℃ to obtain the product.
The mechanical properties of the fluororubber after secondary vulcanization by the method are not obviously different from those of the fluororubber in the example 1, the compression set is higher than that of the fluororubber in the example 1 by 0.7 percent, and the total impurity content is lower than that of the fluororubber in the secondary vulcanization by 0.3 percent.
Example 2
The fluororubber rubber roll with the outer skin made of the disposable low-temperature vulcanized fluororubber consists of a steel roll body and vulcanized fluororubber positioned outside the roll body. Wherein the fluororubber comprises the following components in parts by weight:
100 portions of fluororubber
12 portions of magnesium oxide
6 parts of 1, 4-butanediol
Spray carbon black 35 parts
Ethyl acetate 8 parts
0.8 part of anti-aging agent RD
1.5 parts of bisphenol A.
The preparation method of the fluororubber roll comprises the following steps:
1) crushing the block parts of the components into powder;
2) heating an internal mixer to 130 ℃, adding fluororubber, magnesium oxide, 1, 4-butanediol and 17.5 parts of spray carbon black, and mixing for 5 minutes; then, adding the rest materials into an internal mixer to be mixed for 4-6 minutes to obtain a sizing material;
3) performing thin-pass treatment on the rubber material, pressing into a sheet with the thickness of 0.3 mm, then beating into a triangular bag, repeating for 5 times, then pressing into a rubber sheet with the thickness of 5-6 mm on an open mill, and ventilating to reduce the temperature to the normal temperature to obtain a fluororubber rubber sheet;
4) coating a special (Megum 3290-1) adhesive for fluororubber on the surface of the steel roller body, processing the film into an adhesive tape, and lining the adhesive tape on the surface of the roller body in an extrusion or surface mounting mode; the lined roller body is wound and wrapped by a soaked nylon cloth strip;
5) putting the wrapped rubber roller into a vulcanizing tank, and starting a vulcanization reaction after the vulcanizing tank is pressurized to 0.6 MP;
the vulcanization reaction comprises the following steps:
raising the temperature of the vulcanizing tank to 100 ℃ within 2.5 hours, preserving heat and vulcanizing for 1.5 hours, then raising the temperature of the vulcanizing tank to 135 ℃, preserving heat and vulcanizing for 1.5 hours, then raising the temperature of the vulcanizing tank to 140 ℃, preserving heat and vulcanizing for 10 hours, and then stopping heating; and (4) recovering the vulcanizing tank to normal pressure, and naturally cooling to 50 ℃ to obtain the fluororubber roller.
After inspection, the tensile strength of the fluororubber vulcanized by the method is 16.1MPa, the tearing strength is 42KN/M, the elongation at break is 386 percent, the Shore hardness is 73HA, and the abrasion is 0.257cm3And/1.6 km. The compression set (23 ℃ 72 h) is 15 percent, the total impurity content is higher than 0.6 percent after secondary vulcanization, and the compression set is higher than 0.7 percent after secondary vulcanization.
Example 3
The fluororubber rubber roll with the outer skin made of the disposable low-temperature vulcanized fluororubber consists of a steel roll body and vulcanized fluororubber positioned outside the roll body. Wherein the fluororubber comprises the following components in parts by weight:
fluororubber FE 2603100 parts
18 portions of magnesium oxide
10 portions of 1, 4-butanediol
Spraying carbon black 45 parts
Ethyl acetate 12 parts
1.2 portions of antiager RD
2.5 parts of bisphenol A.
The preparation method of the fluororubber roll comprises the following steps:
1) crushing the block parts of the components into powder;
2) heating an internal mixer to 110 ℃, adding fluororubber, magnesium oxide, 1, 4-butanediol and 22.5 parts of spray carbon black, and mixing for 10 minutes; then, adding the rest materials into an internal mixer to be mixed for 4-6 minutes to obtain a sizing material;
3) performing thin-pass treatment on the rubber material, pressing into a sheet with the thickness of 0.7 mm, then beating into a triangular bag, repeating for 3 times, then pressing into a rubber sheet with the thickness of 5-6 mm on an open mill, and ventilating to reduce the temperature to the normal temperature to obtain a fluororubber rubber sheet;
4) coating a special (Megum 3290-1) adhesive for fluororubber on the surface of the steel roller body, processing the film into an adhesive tape, and lining the adhesive tape on the surface of the roller body in an extrusion or surface mounting mode; wrapping the lining with soaked nylon cloth;
5) putting the wrapped rubber roller into a vulcanizing tank, and starting a vulcanization reaction after the vulcanizing tank is pressurized to 0.4 MP;
the vulcanization reaction comprises the following steps:
raising the temperature of the vulcanizing tank to 105 ℃ within 2.3 hours, preserving heat and vulcanizing for 1.25 hours, then raising the temperature of the vulcanizing tank to 120 ℃, preserving heat and vulcanizing for 1.75 hours, then raising the temperature of the vulcanizing tank to 150 ℃, preserving heat and vulcanizing for 8 hours, and then stopping heating; and (4) recovering the vulcanizing tank to normal pressure, and naturally cooling to 50 ℃ to obtain the fluororubber roller.
The test shows that the fluororubber vulcanized by the method HAs the tensile strength of 17.5 MPa, the tearing strength of 43 KN/M, the elongation at break of 391 percent, the Shore hardness of 75HA and the abrasion of 0.210cm3And/1.6 km. Compression set (23 ℃ 72 h) of 10%, the total impurity content of which is lower than 0.4% after secondary vulcanization, and the compression set of which is lower than 0.2% after secondary vulcanization.
Claims (5)
1. The disposable low-temperature vulcanized fluororubber is characterized by comprising the following components in parts by mass:
100 portions of crude fluororubber
12-18 parts of magnesium oxide
6-10 parts of 1, 4-butanediol
35-45 parts of spray carbon black
8-12 parts of ethyl acetate
0.8-1.2 parts of anti-aging agent RD
1.5-2.5 parts of bisphenol A.
2. The one-time low-temperature vulcanized fluororubber according to claim 1, wherein the mooney viscosity of the fluororubber raw rubber is 50 to 60.
3. The process for the preparation of one-shot low temperature vulcanized fluororubber according to claim 1 or 2, characterized by comprising the steps of:
1) crushing the blocky part in each component of the once low-temperature vulcanized fluororubber into powder;
2) heating an internal mixer to 110-130 ℃, adding fluororubber raw rubber, magnesium oxide, 1, 4-butanediol and 1/2 formula parts of spray carbon black, and mixing for 5-10 minutes; then, adding the rest materials into an internal mixer to be mixed for 4-6 minutes to obtain a sizing material;
3) putting the rubber material into a vulcanizing tank, pressurizing the vulcanizing tank to 0.4-0.6 MPa, and then starting a vulcanization reaction;
the vulcanization reaction comprises the following steps:
raising the temperature of the vulcanizing tank to 100-110 ℃ within 2-2.5 hours, preserving heat and vulcanizing for 1-1.5 hours, then raising the temperature of the vulcanizing tank to 120-135 ℃, preserving heat and vulcanizing for 1.5-2 hours, then raising the temperature of the vulcanizing tank to 140-155 ℃, preserving heat and vulcanizing for 8-10 hours, and then stopping heating; and (4) recovering the vulcanizing tank to normal pressure, and naturally cooling to 50 ℃ or below to obtain the product.
4. Fluororubber roller, characterized in that it consists of a steel roller body and a one-time low-temperature vulcanized fluororubber skin according to claim 1 or 2 located outside the roller body.
5. The method for preparing the fluororubber roll according to claim 4, comprising the steps of:
1) crushing the blocky part in each component of the once low-temperature vulcanized fluororubber into powder;
2) heating an internal mixer to 110-130 ℃, adding fluororubber raw rubber, magnesium oxide, 1, 4-butanediol and 1/2 formula parts of spray carbon black, and mixing for 5-10 minutes; then, adding the rest materials into an internal mixer to be mixed for 4-6 minutes to obtain a sizing material;
3) performing thin-pass treatment on the rubber material, pressing the rubber material into a sheet with the thickness of 0.3-0.7 mm, then beating the sheet into a triangular bag, repeating the process for 3-5 times, then pressing the sheet into a rubber sheet with the thickness of 5-6 mm on an open mill, and ventilating and reducing the temperature to the normal temperature to obtain a fluororubber rubber sheet;
4) coating an adhesive on the surface of a steel roller body, processing a film into an adhesive tape, and lining the adhesive tape on the surface of the roller body in an extrusion or surface mounting mode; the lined roller body is wound and wrapped by a soaked nylon cloth strip;
5) putting the wrapped rubber roller into a vulcanizing tank, and starting a vulcanization reaction after the vulcanizing tank is pressurized to 0.4-0.6 MPa;
the vulcanization reaction comprises the following steps:
raising the temperature of the vulcanizing tank to 100-110 ℃ within 2-2.5 hours, preserving heat and vulcanizing for 1-1.5 hours, then raising the temperature of the vulcanizing tank to 120-135 ℃, preserving heat and vulcanizing for 1.5-2 hours, then raising the temperature of the vulcanizing tank to 140-150 ℃, preserving heat and vulcanizing for 8-10 hours, and then stopping heating; and (4) recovering the vulcanizing tank to normal pressure, and naturally cooling to 50 ℃ to obtain the fluororubber roller.
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| JPH11302416A (en) * | 1998-04-16 | 1999-11-02 | Fujikura Ltd | Rubber product and its manufacture thereof |
| CN104356559A (en) * | 2014-07-15 | 2015-02-18 | 蔡德扬 | Fluororubber compound and preparation method thereof |
| CN106317713A (en) * | 2016-08-31 | 2017-01-11 | 南京利德东方橡塑科技有限公司 | Abrasion-resistant high-temperature-resistant tear-resistant fluorine rubber and preparation method thereof |
| CN107434896A (en) * | 2017-08-29 | 2017-12-05 | 高科橡塑工业有限公司 | It is molded seamless vulcanizable fluororubber adhesive tape and preparation method thereof |
| CN108003400A (en) * | 2017-12-11 | 2018-05-08 | 上海双浦橡胶防腐衬里有限公司 | A kind of high-temperature resistant rubber liner compositions and its preparation method and application |
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