CN111560148A - Low-temperature-resistant fluororubber material for gearbox oil seal and preparation method thereof - Google Patents

Low-temperature-resistant fluororubber material for gearbox oil seal and preparation method thereof Download PDF

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Publication number
CN111560148A
CN111560148A CN202010528188.2A CN202010528188A CN111560148A CN 111560148 A CN111560148 A CN 111560148A CN 202010528188 A CN202010528188 A CN 202010528188A CN 111560148 A CN111560148 A CN 111560148A
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temperature
parts
low
mixing
oil seal
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李华
侯向阳
臧运鹏
张�林
邓又木
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Beiwei Chongqing Science And Technology Co ltd
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Beiwei Chongqing Science And Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/002Methods
    • B29B7/005Methods for mixing in batches
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2206Oxides; Hydroxides of metals of calcium, strontium or barium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2217Oxides; Hydroxides of metals of magnesium
    • C08K2003/222Magnesia, i.e. magnesium oxide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2217Oxides; Hydroxides of metals of magnesium
    • C08K2003/2224Magnesium hydroxide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2296Oxides; Hydroxides of metals of zinc
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2310/00Masterbatches

Abstract

A low-temperature-resistant fluororubber material for a gearbox oil seal comprises the following specific components: fluororubber L636, superfine calcium hydroxide, an acid absorbing agent, a rubber processing aid, a filler, a color master batch, a vulcanizing agent and a vulcanizing aid. The preparation method comprises the following steps: the method comprises the following steps: plasticating fluororubber L636 raw rubber in an internal mixer; step two: adding a rubber processing aid for mixing; step three: adding a vulcanizing agent, a filler and color master batch for mixing; step four: adding the filler, the magnesium oxide and the calcium hydroxide again for mixing; step five: discharging, and thinly passing for 3-10 times after discharging.

Description

Low-temperature-resistant fluororubber material for gearbox oil seal and preparation method thereof
Technical Field
The invention relates to the technical field of rubber part materials for automobiles and manufacturing, in particular to a low-temperature-resistant fluororubber material for a gearbox oil seal and a preparation method thereof.
Background
Fluororubbers, which are copolymers of vinyl fluoride and hexafluoropropylene, have been marketed in the middle of the 50 th 20 th century, have different chemical and low-temperature resistance depending on their molecular structure and fluorine content, and are excellent in flame retardancy (self-extinguishing by fire), gas impermeability (vacuum degree of 1.33 × 10-7-1.33×10-8pa), ozone resistance, weather resistance, good aging resistance, and broad resistance properties are known as "rubber king".
Fluororubbers are used in a wide range of applications in everyday life, for example, as fillers, diaphragms and gaskets for valve seats and valve stems in automobile parts, aviation and aerospace, mechanical seals, pumps, reactors, mixers, compressor housings, valves, various instruments and other equipment, and also in the rubber sheet industry, the semiconductor manufacturing industry, and the food and pharmaceutical industries.
With the increasing demands of the automobile industry for reliability, safety and the like, the demand of fluororubber in the automobile industry is also showing a rapid growth trend. In the aspect of automobile engines, gearboxes and valve oil seals with higher technical content, the selected materials are mainly fluororubber, hydrogenated nitrile rubber and the like. The hydraulic system of the automobile engine gearbox has long continuous working time, the oil temperature and the temperature of parts rise quickly, common rubber cannot meet the working requirements, and fluororubber products can meet various harsh technical requirements by virtue of excellent temperature resistance. The temperature difference between north and south of China is large in winter, the requirements of oil sealing products are more strict, and the low temperature resistance requirement is higher.
Disclosure of Invention
The invention provides a low-temperature-resistant fluororubber material for a gearbox oil seal and a preparation method thereof, aiming at the defects of the prior art, and the specific technical scheme is as follows:
a low-temperature-resistant fluororubber material for a gearbox oil seal comprises the following specific components: fluororubber L636, superfine calcium hydroxide, an acid absorbing agent, a rubber processing aid, a filler, a color master batch, a vulcanizing agent and a vulcanizing aid.
As optimization, the specific component proportion is as follows:
fluororubber L636: 100 parts of (A);
ultra-fine calcium hydroxide: 3-10 parts;
acid-absorbing agent: 1-6 parts;
rubber processing aid: 2-6 parts;
filling: 10-50 parts;
color master batch: 3-10 parts;
vulcanizing agent and vulcanizing assistant: 1-3 parts.
As optimization, the acid absorbent adopts superfine magnesium hydroxide and high-activity magnesium oxide.
Preferably, the rubber processing aid is one or more of polyethylene wax, carnauba wax and WS 280.
Preferably, the filler is selected from wollastonite, diatomite and zinc oxide.
A preparation method of a low-temperature-resistant fluororubber material for a gearbox oil seal comprises the following specific steps:
the method comprises the following steps: plasticating fluororubber L636 raw rubber in an internal mixer;
step two: adding a rubber processing aid for mixing;
step three: adding a vulcanizing agent, a filler and color master batch for mixing;
step four: adding the filler, the magnesium oxide and the calcium hydroxide again for mixing;
step five: discharging, and thinly passing for 3-10 times after discharging.
As optimization, the processing environment of the first step is that the set temperature is: 25-50 ℃, rotation speed: 30-50r/min, upper roof plug pressure: 4KG, plastication time: 10-40S;
the processing environment of the second step is that the set temperature is as follows: 25-50 ℃, rotation speed: 30-50r/min, upper roof plug pressure: 4KG, mixing for 30s-2 min;
the processing environment of the third step is that the set temperature is as follows: 25-50 ℃, rotation speed: 30-50r/min, upper roof plug pressure: 4KG, mixing for 1-3 min;
the processing environment of the fourth step is that the set temperature is as follows: 25-50 ℃, rotation speed: 30-50r/min, upper roof plug pressure: 4KG, mixing for 3-5 min.
The invention has the beneficial effects that: by adopting the feeding sequence in the method, the formula, the mixing temperature, the rotating speed and the time are adjusted, the process and equipment parameters are optimized, the dispersion of the vulcanizing agent and the filler is completed, the obtained rubber compound filler and the auxiliary agent are uniformly dispersed, the material performance is excellent, and the cost is greatly saved by adopting a bisphenol system for vulcanization under the same performance requirement.
Detailed Description
The following detailed description of the preferred embodiments of the present invention is provided to enable those skilled in the art to more readily understand the advantages and features of the present invention, and to clearly and unequivocally define the scope of the present invention.
The first embodiment is as follows:
a low-temperature-resistant fluororubber material for a gearbox oil seal comprises the following specific components in proportion:
fluororubber L636: 100 parts of (A);
ultra-fine calcium hydroxide: 6 parts of (1);
150-1 parts of magnesium oxide: 6 parts of (1);
WS 280: 1 part;
color master batch: 8 parts of a mixture;
zinc oxide: 20 parts of (1);
bisphenol AF: 2 parts of (1);
and (3) BPP: 0.6 part.
The preparation method of the low-temperature-resistant fluororubber material for the gearbox oil seal comprises the following steps: s1, plasticating the raw rubber in an internal mixer, setting the temperature: 35 ℃, rotation speed: 30r/min, upper plug pressure: 4KG, plastication time: 20S; because the viscosity of the fluororubber is very high, real plastic is not needed, and only short-time plastication is needed to ensure that the rubber has a large contact area. Mixing starts at a very low rotor speed, preventing a rapid rise in temperature.
S2, adding a processing aid, setting the temperature: 35 ℃, rotation speed: 30r/min, upper plug pressure: 4KG, mixing for 2 min; because the mineral filler is easy to absorb water, if the humidity of the mineral filler is higher, the mineral filler is easy to be adhered to the surface of metal during mixing, the processing aid is added firstly, so that the viscosity of the rubber material can be reduced while the adhesion of the rubber material and the metal is prevented, and the processing is easy.
S3, adding a vulcanizing agent, a filler and a color master batch, wherein only half of the filler is added in the step, and the temperature is set as follows: 35 ℃, rotation speed: 25r/min, upper plug pressure: 4KG, mixing for 90 s; since inert fillers are used and a mesh-type internal mixer is used, there is no problem in achieving the desired degree of dispersion.
S4, adding the other half of filler, magnesium oxide and calcium hydroxide, setting the temperature: 35 ℃, rotation speed: 25r/min, upper plug pressure: 4KG, mixing for 50 s;
s5, discharging at a temperature not higher than 120 ℃, and passing through the pipe 3-10 times after discharging.
In the embodiment, because the meshing internal mixer is adopted, the filling coefficient can be improved to 70%, and compared with the open mixing efficiency, the production efficiency is improved by at least 300%. Compared with the common shearing internal mixer, the filling amount is also increased by 15-20%. The production efficiency is greatly improved, and the cost is saved.
Example two:
a low-temperature-resistant fluororubber material for a gearbox oil seal comprises the following specific components in proportion:
fluororubber L636: 100 parts of (A);
ultra-fine calcium hydroxide: 6 parts of (1);
150-1 parts of magnesium oxide: 3 parts of a mixture;
WS 280: 1 part;
1 part of polyethylene wax;
diatomaceous earth AZ-90: 20 parts of (1);
color master batch: 8 parts of a mixture;
bisphenol AF: 1.5 parts;
and (3) BPP: 0.6 part.
Example three:
a low-temperature-resistant fluororubber material for a gearbox oil seal comprises the following specific components in proportion:
fluororubber L636: 100 parts of (A);
ultra-fine calcium hydroxide: 6 parts of (1);
150-1 parts of magnesium oxide: 3 parts of a mixture;
WS 280: 1 part;
1.5 parts of palm wax;
wollastonite: 30 parts of (1);
color master batch: 8 parts of a mixture;
bisphenol AF: 1.5 parts;
and (3) BPP: 0.6 part.
Example four:
a low-temperature-resistant fluororubber material for a gearbox oil seal comprises the following specific components in proportion:
fluororubber L636: 100 parts of (A);
ultra-fine calcium hydroxide: 6 parts of (1);
150-1 parts of magnesium oxide: 3 parts of a mixture;
WS 280: 1 part;
1.5 parts of palm wax;
wollastonite: 20 parts of (1);
color master batch: 8 parts of a mixture;
bisphenol AF: 1.5 parts;
and (3) BPP: 0.6 part.
The test results show that the properties of the first, second, third and fourth examples are as follows:
Figure BDA0002534391380000061
the fluororubber materials obtained in the first, second, third and fourth examples have good low-temperature resistance, and the compression set property after high-temperature aging is also very excellent. The rubber compound prepared by changing the formula and the process meets the requirements of customers through bench tests of customers, has no oil leakage phenomenon and good sealing performance in long-time oil-resistant tests, and the prepared sealing element has low rejection rate and low cost.

Claims (7)

1. The utility model provides a gearbox oil blanket is with low temperature resistant fluororubber material which characterized in that, concrete component is: fluororubber L636, superfine calcium hydroxide, an acid absorbing agent, a rubber processing aid, a filler, a color master batch, a vulcanizing agent and a vulcanizing aid.
2. The low-temperature-resistant fluororubber material for the gearbox oil seal as defined in claim 1, wherein the specific component proportions are as follows:
fluororubber L636: 100 parts of (A);
ultra-fine calcium hydroxide: 3-10 parts;
acid-absorbing agent: 1-6 parts;
rubber processing aid: 2-6 parts;
filling: 10-50 parts;
color master batch: 3-10 parts;
vulcanizing agent and vulcanizing assistant: 1-3 parts.
3. The low-temperature-resistant fluororubber material for the gearbox oil seal according to claim 1, characterized in that: the acid absorbent adopts superfine magnesium hydroxide and high-activity magnesium oxide.
4. The low-temperature-resistant fluororubber material for the gearbox oil seal according to claim 1, characterized in that: the rubber processing aid is one or more of polyethylene wax, carnauba wax and WS 280.
5. The low-temperature-resistant fluororubber material for the gearbox oil seal according to claim 1, characterized in that: the filler is selected from wollastonite, diatomite and zinc oxide.
6. The preparation method of the low-temperature-resistant fluororubber material for the gearbox oil seal according to any one of claims 1 to 5, which is characterized by comprising the following steps:
the method comprises the following steps: plasticating fluororubber L636 raw rubber in an internal mixer;
step two: adding a rubber processing aid for mixing;
step three: adding a vulcanizing agent, a filler and color master batch for mixing;
step four: adding the filler, the magnesium oxide and the calcium hydroxide again for mixing;
step five: discharging, and thinly passing for 3-10 times after discharging.
7. The preparation method of the low-temperature-resistant fluororubber material for the gearbox oil seal according to claim 6, characterized by comprising the following steps: the processing environment of the first step is that the set temperature is as follows: 25-50 ℃, rotation speed: 30-50r/min, upper roof plug pressure: 4KG, plastication time: 10-40S;
the processing environment of the second step is that the set temperature is as follows: 25-50 ℃, rotation speed: 30-50r/min, upper roof plug pressure: 4KG, mixing for 30s-2 min;
the processing environment of the third step is that the set temperature is as follows: 25-50 ℃, rotation speed: 30-50r/min, upper roof plug pressure: 4KG, mixing for 1-3 min;
the processing environment of the fourth step is that the set temperature is as follows: 25-50 ℃, rotation speed: 30-50r/min, upper roof plug pressure: 4KG, mixing for 3-5 min.
CN202010528188.2A 2020-06-11 2020-06-11 Low-temperature-resistant fluororubber material for gearbox oil seal and preparation method thereof Pending CN111560148A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114957795A (en) * 2022-06-16 2022-08-30 江西广源化工有限责任公司 Composite filler and preparation method thereof, and fluororubber composite material and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102504448A (en) * 2011-11-30 2012-06-20 南京金三力橡塑有限公司 Low-temperature-resistant and novel-fuel-resistant low-pressure-change fluorine rubber gross rubber and preparation method thereof
CN104356562A (en) * 2013-10-30 2015-02-18 东莞市长安东阳光铝业研发有限公司 Fluororubber rubber compound and preparation method thereof
CN104403238A (en) * 2014-11-25 2015-03-11 大连郑氏橡胶有限公司 Low-temperature resistant modified fluoro-rubber mixed compound and preparation method
CN105566816A (en) * 2015-11-24 2016-05-11 南京利德东方橡塑科技有限公司 Formula and preparation method of high-elongation high-temperature-resistant fluororubber for rubber pipes

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102504448A (en) * 2011-11-30 2012-06-20 南京金三力橡塑有限公司 Low-temperature-resistant and novel-fuel-resistant low-pressure-change fluorine rubber gross rubber and preparation method thereof
CN104356562A (en) * 2013-10-30 2015-02-18 东莞市长安东阳光铝业研发有限公司 Fluororubber rubber compound and preparation method thereof
CN104403238A (en) * 2014-11-25 2015-03-11 大连郑氏橡胶有限公司 Low-temperature resistant modified fluoro-rubber mixed compound and preparation method
CN105566816A (en) * 2015-11-24 2016-05-11 南京利德东方橡塑科技有限公司 Formula and preparation method of high-elongation high-temperature-resistant fluororubber for rubber pipes

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114957795A (en) * 2022-06-16 2022-08-30 江西广源化工有限责任公司 Composite filler and preparation method thereof, and fluororubber composite material and preparation method thereof

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Application publication date: 20200821