CN106589739A - Good-gas-barrier-property oil-extended cis-polybutadiene rubber used for hydraulic hammer high pressure oil pipe and preparation method thereof - Google Patents
Good-gas-barrier-property oil-extended cis-polybutadiene rubber used for hydraulic hammer high pressure oil pipe and preparation method thereof Download PDFInfo
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- CN106589739A CN106589739A CN201610987149.2A CN201610987149A CN106589739A CN 106589739 A CN106589739 A CN 106589739A CN 201610987149 A CN201610987149 A CN 201610987149A CN 106589739 A CN106589739 A CN 106589739A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L47/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds; Compositions of derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F136/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds
- C08F136/02—Homopolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds
- C08F136/04—Homopolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated
- C08F136/06—Butadiene
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/14—Gas barrier composition
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
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Abstract
The invention discloses good-gas-barrier-property oil-extended cis-polybutadiene rubber used for a hydraulic hammer high pressure oil pipe and a preparation method thereof, the good-gas-barrier-property oil-extended cis-polybutadiene rubber is made from the following raw materials by weight: 20-22 parts of carbon nanotubes, 6200-6400 parts of butadiene, a proper amount of hydrogasoline, 0.18-0.19 part of nickel naphthenate, 1.8-1.9 parts of triisobutyl aluminium, 2.1-2.3 parts of boron trifluoride diethyl etherate, 1.7-1.9 parts of octanal, 3400-3600 parts of heavy aromatic oil, 3-4 parts of tetrabutyl titanate, 150-170 parts of ethanol, 24-26 parts of ammonia, 15-17 parts of water, 4-5 parts of fluorine-containing benzoxazine, 2-3 parts of triallyl isocyanurate, 3-4 parts of flaky carbon powder and 3-4 parts of trifluoroethyl acrylate. Through use of the fluorine-containing benzoxazine, the triallyl isocyanurate and the flaky carbon powder, the compactness, gas-barrier property and oil resistance of the rubber are improved, and oil penetration is reduced.
Description
Technical field
The present invention relates to technical field of rubber material, more particularly to a kind of good hydraulic breaking hammer high-pressure oil pipe of gas barrier property is with filling
Oily butadiene rubber and preparation method thereof.
Background technology
《New oil-extended butadiene rubber development and production》Briefly describe the development course of domestic and international synthetic rubber technology, plant
Class, feature, polymerization reaction mechanism, and commercial production, situations such as apply.The new oil-extended butadiene rubber of this article research and development is produced
Product, change catalyst formulation and rate of polymerization using regulator method to synthesize high Mooney viscosity basis glue;Reselection is suitably filled
Oily technique productions oil-extended butadiene rubber.Using solution polymerization process, on 5L kettles and 50L kettles, with along 1,3- butadiene as monomer, nickel
Series catalysts are initiator, be prepared for oil-extended butadiene rubber, and lab scale and pilot scale research have been carried out to Technology, and industry
Trial production.Be investigated herein nickle catalyst system synthesize high Mooney viscosity butadiene rubber rule, investigated catalyst proportion,
Monomer concentration, polymerization time, the optimal addn of octanal, and to monomer conversion, crude rubber Mooney viscosity and average molecular matter
The impact of amount distribution, have found the relation between basic glue Mooney viscosity and oil-filled quantity, oil-filled glue Mooney viscosity, determines high Mooney
The synthesis condition of basic glue, determines the physical and mechanical propertiess of oil-filled glue.On the premise of monomer conversion more than 85%, synthesis
70～100 high Mooney viscosity butadiene rubber;Control in 80～95, oil-filled quantity to be 35～40 parts in the Mooney viscosity of basic glue
Under conditions of (quality), the high oil-extended butadiene rubber of physical and mechanical propertiess is obtained, one is provided to prepare oil-extended butadiene rubber
Reliable technology path.
The elasticity and anti-wear performance of the butadiene rubber for obtaining is good, and heat and vitrification point are low, it is adaptable to prepare tire and
Arctic rubber product, can be used for oil pipe making.But butadiene rubber processing characteristics, bond propertiess, antiskid performance and tear resistance
Can not be good, require further improvement, in addition it is also necessary to improve the gas barrier property of rubber.
The content of the invention
The object of the invention is exactly for the defect for making up prior art, there is provided a kind of good hydraulic breaking hammer hydraulic oil of gas barrier property
Effective oil-extended butadiene rubber and preparation method thereof.
The present invention is achieved by the following technical solutions：
A kind of good hydraulic breaking hammer high-pressure oil pipe oil-extended butadiene rubber of gas barrier property, is prepared by the raw materials in：Carbon is received
Mitron 20-22, butadiene 6200-6400, appropriate hydrogasoline, nickel naphthenate 0.18-0.19, triisobutyl aluminium 1.8-1.9, three
Fluorination borate ether 2.1-2.3, octanal 1.7-1.9, high aromatic oil 3400-3600, butyl titanate 3-4, ethanol 150-170, ammonia
Water 24-26, water 15-17, fluorine-containing benzoxazinyl 4-5, Triallyl isocyanurate 2-3, flakey carbon dust 3-4, acrylic acid three
Fluorine ethyl ester 3-4.
The preparation method of the good hydraulic breaking hammer high-pressure oil pipe oil-extended butadiene rubber of the gas barrier property, comprises the following steps：
（1）Butyl titanate, ethanol are mixed, stirring obtains butyl titanate ethanol solution, add CNT to stir,
Add water to stir Triallyl isocyanurate, flakey carbon dust, obtain dispersion liquid, homogeneous dispersion is added dropwise to into institute
State in solution, 1.5-1.8h is stirred under the conditions of 250-300r/min, obtain mixture, ammonia is slowly added dropwise into people then above-mentioned
In mixture, emulsion is being obtained after stirring reaction 3-3.5h at 30-35 DEG C, adding acrylic acid trifluoro ethyl ester, stir, mistake
Filter, is dried, obtains powder；
（2）Valve bag is put the powder into, irradiation is carried out, absorbed dose are 56-58kGy, crushed, crossed 200-250 mesh sieves, obtain
To modified carbon nano-tube；
（3）Butadiene is added in hydrogasoline, the solution of 100-105g/L is configured to, is added modified carbon nano-tube, stirred
Uniformly, water bath with thermostatic control is put into, is heated to 75-78 DEG C, high aromatic oil is mixed homogeneously with other residual componentss, butadiene is added dropwise to
Solution in, stirring reaction 2-2.3 hour obtains glue, and glue is carried out vapor cohesion, on 110-112 DEG C of cylinder roll
It is dry, obtain oil-filled glue；
（4）Oil-filled glue is sent in vulcanizing press and is vulcanized, conditions of vulcanization is 145 DEG C of * 35min, is obtained final product.
It is an advantage of the invention that：The present invention is modified to CNT using butyl titanate, in carbon nano tube surface
Titanium dioxide nanoparticle is defined, the dispersibility of CNT is improve, the compactness and ageing resistance of rubber is improve, is prevented
Leak-stopping gas；CNT is coated by using acrylic acid trifluoro ethyl ester, then carry out radiation crosslinking modified, improve nanometer
Titanium dioxide and the adhesive fastness of CNT, improve resistance to water, lipophile and the lubricity of CNT, divide in rubber
Dissipate more uniform reinforcing effect more preferably, improve the compactness and wearability of rubber.By using fluorine-containing benzoxazinyl, three allyls
Base isocyanuric acid ester, flakey carbon dust, it is good to improve rubber compactness, and gas barrier property is improved, and oil resistivity is improved, and reduces oil infiltration.
Specific embodiment
The good hydraulic breaking hammer high-pressure oil pipe oil-extended butadiene rubber of a kind of gas barrier property, by following weight portion（Kilogram）Raw material
Make：CNT 20, butadiene 6200, appropriate hydrogasoline, nickel naphthenate 0.18, triisobutyl aluminium 1.8, boron trifluoride second
Ether 2.1, octanal 1.7, high aromatic oil 3400, butyl titanate 3, ethanol 150, ammonia 24, water 15, fluorine-containing benzoxazinyl 4, triolefin
Propyl group isocyanuric acid ester 2, flakey carbon dust 3, acrylic acid trifluoro ethyl ester 3.
The preparation method of the good hydraulic breaking hammer high-pressure oil pipe oil-extended butadiene rubber of the gas barrier property, comprises the following steps：
（1）Butyl titanate, ethanol are mixed, stirring obtains butyl titanate ethanol solution, add CNT to stir,
Add water to stir Triallyl isocyanurate, flakey carbon dust, obtain dispersion liquid, homogeneous dispersion is added dropwise to into institute
State in solution, 1.5h is stirred under the conditions of 250r/min, obtain mixture, ammonia is slowly added dropwise into people's said mixture then
In, emulsion is being obtained after stirring reaction 3h at 30 DEG C, adding acrylic acid trifluoro ethyl ester, stir, filtered, be dried, obtain
Powder；
（2）Valve bag is put the powder into, irradiation is carried out, absorbed dose are 56kGy, crushed, crossed 200 mesh sieves, be modified
CNT；
（3）Butadiene is added in hydrogasoline, the solution of 100g/L is configured to, is added modified carbon nano-tube, stir,
Water bath with thermostatic control is put into, 75 DEG C are heated to, high aromatic oil is mixed homogeneously with other residual componentss, be added dropwise to the solution of butadiene
In, stirring reaction obtains glue in 2 hours, and glue is carried out vapor cohesion, rolls dry, obtain oil-filled glue on 110 DEG C of cylinders；
（4）Oil-filled glue is sent in vulcanizing press and is vulcanized, conditions of vulcanization is 145 DEG C of * 35min, is obtained final product.
Experimental data：
The tensile strength of the embodiment elastomeric material is 5.5MPa, and tearing strength is 29kN/m, and elongation rate of tensile failure is 481%, stretching
18.9% is permanently deformed to, 100% stress at definite elongation is 1.52MPa, and 300% stress at definite elongation is 2.6MPa, and shore a hardness is 53.8 degree,
Akron abrasion is 2.21cm3。
Claims (2)
1. the good hydraulic breaking hammer high-pressure oil pipe oil-extended butadiene rubber of a kind of gas barrier property, it is characterised in that：By following weight portion
Raw material is made：CNT 20-22, butadiene 6200-6400, appropriate hydrogasoline, nickel naphthenate 0.18-0.19, three isobutyls
Base aluminum 1.8-1.9, boron trifluoride diethyl etherate 2.1-2.3, octanal 1.7-1.9, high aromatic oil 3400-3600, butyl titanate 3-4,
Ethanol 150-170, ammonia 24-26, water 15-17, fluorine-containing benzoxazinyl 4-5, Triallyl isocyanurate 2-3, flakey carbon
Powder 3-4, acrylic acid trifluoro ethyl ester 3-4.
2. the preparation method of the good hydraulic breaking hammer high-pressure oil pipe oil-extended butadiene rubber of gas barrier property according to claim 1, its
It is characterised by comprising the following steps：
（1）Butyl titanate, ethanol are mixed, stirring obtains butyl titanate ethanol solution, add CNT to stir,
Add water to stir Triallyl isocyanurate, flakey carbon dust, obtain dispersion liquid, homogeneous dispersion is added dropwise to into institute
State in solution, 1.5-1.8h is stirred under the conditions of 250-300r/min, obtain mixture, ammonia is slowly added dropwise into people then above-mentioned
In mixture, emulsion is being obtained after stirring reaction 3-3.5h at 30-35 DEG C, adding acrylic acid trifluoro ethyl ester, stir, mistake
Filter, is dried, obtains powder；
（2）Valve bag is put the powder into, irradiation is carried out, absorbed dose are 56-58kGy, crushed, crossed 200-250 mesh sieves, obtain
To modified carbon nano-tube；
（3）Butadiene is added in hydrogasoline, the solution of 100-105g/L is configured to, is added modified carbon nano-tube, stirred
Uniformly, water bath with thermostatic control is put into, is heated to 75-78 DEG C, high aromatic oil is mixed homogeneously with other residual componentss, butadiene is added dropwise to
Solution in, stirring reaction 2-2.3 hour obtains glue, and glue is carried out vapor cohesion, on 110-112 DEG C of cylinder roll
It is dry, obtain oil-filled glue；
（4）Oil-filled glue is sent in vulcanizing press and is vulcanized, conditions of vulcanization is 145 DEG C of * 35min, is obtained final product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610987149.2A CN106589739A (en) | 2016-11-10 | 2016-11-10 | Good-gas-barrier-property oil-extended cis-polybutadiene rubber used for hydraulic hammer high pressure oil pipe and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610987149.2A CN106589739A (en) | 2016-11-10 | 2016-11-10 | Good-gas-barrier-property oil-extended cis-polybutadiene rubber used for hydraulic hammer high pressure oil pipe and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1635004A (en) * | 2003-12-28 | 2005-07-06 | 中国石化齐鲁股份有限公司 | Process for producing high cis-polybutadiene rubber |
| CN103172789A (en) * | 2012-12-14 | 2013-06-26 | 万达集团股份有限公司 | Method for preparing nickel series low-mooney high cis-1,4-polybutadiene rubber |
| CN104327323A (en) * | 2014-09-30 | 2015-02-04 | 青岛东泰诚恩新材料科技发展有限公司 | Butadiene rubber |
-
2016
- 2016-11-10 CN CN201610987149.2A patent/CN106589739A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1635004A (en) * | 2003-12-28 | 2005-07-06 | 中国石化齐鲁股份有限公司 | Process for producing high cis-polybutadiene rubber |
| CN103172789A (en) * | 2012-12-14 | 2013-06-26 | 万达集团股份有限公司 | Method for preparing nickel series low-mooney high cis-1,4-polybutadiene rubber |
| CN104327323A (en) * | 2014-09-30 | 2015-02-04 | 青岛东泰诚恩新材料科技发展有限公司 | Butadiene rubber |
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Application publication date: 20170426 |