CN105585647A - Preparation method of polyethylene special material for vehicle decorative non-woven fabric back glue - Google Patents
Preparation method of polyethylene special material for vehicle decorative non-woven fabric back glue Download PDFInfo
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- CN105585647A CN105585647A CN201410557322.6A CN201410557322A CN105585647A CN 105585647 A CN105585647 A CN 105585647A CN 201410557322 A CN201410557322 A CN 201410557322A CN 105585647 A CN105585647 A CN 105585647A
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Abstract
The invention belongs to the technical field of polymer synthesis and specifically relates to a preparation method of a polyethylene special material for vehicle decorative non-woven fabric back glue. On a tubular E-method high pressure polymerization process device, appropriate initiator and molecular weight regulator are selected, and ethylene feed mainstream and sidestream are added in appropriate proportion, and appropriate polymerization pressure and polymerization temperature are selected. Then, vehicle decorative non-woven fabric back glue special polyethylene with high melt index (22-32g/10min under conditions of 190 DEG C and 2.16 kg) and medium-low density (0.920-0.934g/cm<3>) is developed and prepared. The method is simple and is easy to operate.
Description
Technical field
The present invention relates to macromolecule synthesising technology field, specifically, relate in particular to a kind of for automotive trim fieldThe high molten high pressure tubular preparation method who refers to polyvinyl resin,
Background technology
Since the eighties in 20th century, Global Auto industry has obtained developing rapidly, and China also classifies auto industry asPillar industry. Enter after 21 century, along with Foreign Automobile manufacturer enters China one after another, the Automotive of China moreObtain significant progress. Automobile pulls domestic demand with house, the same conduct of education, supports gross national product GDP to increaseLong key factor more and more causes people's concern. Following Automobile Design will embody the distinctness spy that people-oriented morePoint. Meet the increasing demand of car steering person, the Functional Design of automotive interior trim becomes more important. PeopleThe time driving a car is more and more longer, also can be more and more higher to the expectation of comfortableness. Automobile is especially in station wagon carThe choice and operation of ornament materials, the sale on automobile and use also have very important impact. Domestic Automotive IndustryDevelop rapidly provide wide field for the application of various ornament materials in automobile, greater functionality has also been proposed simultaneouslyWith higher-quality requirement. For this reason, domestic automobile inside gadget supplementary material manufacturing enterprise also synchronously carry out production capacity expansion andThe raising of quality scale.
Taking car decorations nonwoven gum polyethylene special-purpose material as raw material, utilize high speed extrusion film technique and PE film gumTechnique is coated in PE film on nonwoven, to form gum and produce automotive interior material, thereby makes automotive trim nonwovenThe mass propertys such as tensile break stress, tension failure norminal strain, air-tightness and the moisture resistance of cloth are greatly improved.
The car decorations nonwoven gum polyethylene special-purpose material the present invention relates to is to produce enterprise for automotive upholstery supplementary materialThe special product that industry is made to measure. It has very high mobile performance, has moderate degree of crystallinity and density. HaveNarrow molecular weight distribution. Because molecular weight distribution is narrower, can make the large molecule non-Newtonianism of PE weaken, melt elasticity becomesLittle, make the gum applying shrink and diminish at melt state. Make product size stable.
The enterprise that produces at present car decorations nonwoven gum polyethylene special-purpose material is both at home and abroad very little, looks into through relevant authorityNew mechanism inquiry, so far there are no reports. The present invention, in tubular type E method high pressure polymerization plants, utilizes the tune of polymerization techniqueJoint, namely utilize the selection of initator, several initator (several different peroxide and oxygen) addition,Between different proportionings; Utilize selection and the addition of molecular weight adjusting agent, utilize different initators in ethene main flow andThe additional proportion of effluent; Utilize the process adjustments such as polymerization pressure, polymerization temperature means, develop this polyethylene of preparation specialMaterials, have great importance.
Summary of the invention
In order to overcome the deficiencies in the prior art, the object of the present invention is to provide a kind of car decorations nonwoven gum polyethyleneThe preparation method of PP Pipe Compound, this preparation method is simple, easy to operate. The polyethylene height obtaining melts finger, middle low-density and dividesSon amount narrow distribution, is adapted at forming on nonwoven gum.
The preparation method who the invention provides a kind of car decorations nonwoven gum polyethylene special-purpose material, adopts tubular type when it is preparedE method high-pressure polymerization process device, comprises the following steps:
(1) ethene, the first initator, the second initator and adjusting agent are compressed, after compression, be divided into two bursts of pressuresPower is master, the effluent feed gas of 230～250Mpa; Described main flow feed gas comprise ethene, the first initator andAdjusting agent, the content of described the first initator is 5 ± 0.5ppm, the content of adjusting agent is 225 ± 20ppm; DescribedEffluent feed gas comprises ethene and the second initator, and the content of described the second initator is 15 ± 2ppm; Wherein:Described the first initator is made up of the tertiary fourth fat of peroxidating neodecanoic acid and the tertiary fourth fat of peroxidating 2 ethyl hexanoic acid, peroxidating 2-The tertiary fourth fat of thylhexoic acid accounts for 80 ± 10% of initator gross weight; Described adjusting agent is C3～C10Aldehyde; DescribedTwo initators are through filtering and dry compressed air;
(2) main flow feed gas enters the first tubular reactor, is first heated to gradually 175 ± 10 DEG C with steam jacket,Carry out polymerisation at reaction zone again, polymerization temperature is 310～330 DEG C, and pressure is 240～250Mpa, the reaction timeIt is 7～8 seconds; Reaction finishes rear cooling, goes out the first reactor, then merges with the effluent feed gas that compressor is sent here;The reaction zone that enters the second tubular reactor carries out polymerisation, and polymerization temperature is 310～330 DEG C, and pressure is210～220Mpa, the reaction time is 11～12 seconds;
(3) after the second tubular reactor reaction, cooling, reactant mixture is again by the baiting valve of reactor exitStep-down, enters high stampings separator, carries out gas and feed separation; Then, the polyethylene product of molten entersLow stampings separator carries out gas and feed separation again, finally carries out extruding pelletization.
The tertiary fourth fat of peroxidating neodecanoic acid in the present invention, molecular formula is C15H30O3, within 10 hours, half life temperature is 43DEG C, within 1 hour, half life temperature is 61 DEG C, within 0.1 hour, half life temperature is 81 DEG C;
The tertiary fourth fat of peroxidating 2 ethyl hexanoic acid in the present invention, molecular formula is C12H24O3, 10 hours half life temperaturesBe 72 DEG C, within 1 hour, half life temperature is 91 DEG C, and within 0.1 hour, half life temperature is 113 DEG C;
In the present invention, adjusting agent is preferably propionic aldehyde. The molecular formula of propionic aldehyde is C3H6O, is liquid at normal temperatures, and it is moltenPoint is-81 DEG C, and boiling point is 48.8 DEG C, easily vaporization. It can slightly generate dimerization, trimerization propionic aldehyde under high-temperature.
In the present invention, the air in the second initator injects in leading portion compressor suction, the mistake in the first initatorOxide injects the first tubular reactor with super-pressure pump, and the propionic aldehyde of adjusting agent enters at back segment compressor with high-pressure metering pumpMouth injects.
The molten low density polyethylene (LDPE) that refers to of height for car decorations nonwoven gum that the present invention obtains, its melt index is22g/10min～32g/10min; Be preferably 25g/10min～29g/10min; Density is 0.920g/cm3～0.934g/cm3，Be preferably 0.921g/cm3～0.926g/cm3; Molecular weight distributing index is 3～10, is preferably 4.5～6.5; Hot strengthBe greater than 8Mpa, be preferably more than 9Mpa; Tension failure strain is greater than 100%, is preferably more than 500%.
Beneficial effect of the present invention is: the inventive method is simple, easy to operate, low energy consumption, the conversion per pass of reaction20～25%; The molecular weight of polyethylene narrow distribution that production obtains, has high molten finger, middle low-density, is applicable to applicationIn car decorations nonwoven production.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further details.
Process using tubular type E method high-pressure polymerization process device in the present invention, the main skill of the polymerization reactor equipment that usesArt parameter is as follows:
The first tubular reactor internal diameter: Φ 27mm, wall thickness: 17.5mm, length: 600m;
The second tubular reactor internal diameter: Φ 34mm; Wall thickness: 22mm, length: 504m.
Embodiment 1
(1) ethene, the first initator, the second initator and adjusting agent are compressed, after compression, be divided into two bursts of pressuresPower is master, the effluent feed gas of 230～250Mpa; Described main flow feed gas comprise ethene, the first initator andAdjusting agent, the content of the tertiary fourth fat of peroxidating neodecanoic acid in described the first initator is 1ppm, peroxidating 2-ethyl hexylThe content of the tertiary fourth fat of acid is 4ppm, and described adjusting agent is propionic aldehyde, and the content of propionic aldehyde is 225ppm; Described effluent entersMaterial gas comprises ethene and the second initator, and described the second initator is that it contains through filtering and dry compressed airAmount is 16ppm;
(2) main flow feed gas enters the first tubular reactor, is first heated to gradually 175 ± 10 DEG C with steam jacket,Carry out polymerisation at reaction zone again, polymerization temperature is 310～330 DEG C, and pressure is 240～250Mpa, the reaction timeIt is 7～8 seconds; Reaction finishes rear cooling, goes out the first reaction zone device, then merges with the effluent feed gas that compressor is sent here;The reaction zone that enters the second tubular reactor carries out polymerisation, and polymerization temperature is 320～330 DEG C, and pressure is210～220Mpa, the reaction time is 11～12 seconds;
(3) after the second tubular reactor reaction, cooling, reactant mixture is again by the baiting valve of reactor exitStep-down, enters high stampings separator, carries out gas and feed separation; Then, the polyethylene product of molten entersLow stampings separator carries out gas and feed separation again, finally carries out extruding pelletization.
Embodiment 2
Concrete steps are with embodiment 1.
Wherein: main, effluent feed gas pressure is 230～245Mpa, in the first initator in main flow feed gas,The content of the tertiary fourth fat of peroxidating neodecanoic acid is 1.1ppm, and the content of the tertiary fourth fat of peroxidating 2 ethyl hexanoic acid is 4.4ppm,Initator compressed air content in effluent feed gas is 17ppm, and in main flow feeding gas, molecular weight adjusting agent propionic aldehyde containsAmount is for 225ppm, and the reaction temperature control of the first tubular reactor is 310～320 DEG C, the second tubular reactor anti-Answering temperature control is 310～320 DEG C.
Embodiment 3
Concrete steps are with embodiment 1.
Wherein: main, effluent feed gas pressure is 230～240Mpa, in the first initator in main flow feed gas,The content of the tertiary fourth fat of peroxidating neodecanoic acid is 0.95ppm, and the content of the tertiary fourth fat of peroxidating 2 ethyl hexanoic acid is 3.8ppm,The second initator (compressed air) content in effluent feed gas is 16ppm, adjusting agent third in main flow feeding gasThe content of aldehyde is 225ppm, and the reaction temperature control of the first tubular reactor is 300～310 DEG C, the second pipe reactionThe reaction temperature control of device is 300～310 DEG C.
Embodiment 4
Concrete steps are with embodiment 1.
Wherein: main, effluent feed gas pressure is 230～240Mpa, in the first initator in main flow feed gas,The content of the tertiary fourth fat of peroxidating neodecanoic acid is 1ppm, and the content of the tertiary fourth fat of peroxidating 2 ethyl hexanoic acid is 4ppm, sideThe second initator (compressed air) content in stream feed gas is 16ppm, the adjusting agent third in main flow feeding gasThe content of aldehyde is 245ppm, and the reaction temperature control of the first tubular reactor is 300～320 DEG C, the second pipe reactionThe reaction temperature control of device is 300～320 DEG C.
Embodiment 5
Concrete steps are with embodiment 1.
Wherein: main, effluent feed gas pressure is 230～240Mpa, in the first initator in main flow feed gas,The content of the tertiary fourth fat of peroxidating neodecanoic acid is 1.1ppm, and the content of the tertiary fourth fat of peroxidating 2 ethyl hexanoic acid is 4.4ppm,The second initator (compressed air) content in effluent feed gas is 17ppm, the adjusting agent in main flow feeding gasThe content of propionic aldehyde is 210ppm, and the reaction temperature control of the first tubular reactor is 300～320 DEG C, and the second tubular type is anti-The reaction temperature control of answering device is 300～320 DEG C.
Embodiment 6
Concrete steps are with embodiment 1.
Wherein: main, effluent feed gas pressure is 230～240Mpa, in the first initator in main flow feed gas,The content of the tertiary fourth fat of peroxidating neodecanoic acid is 0.9ppm, and the content of the tertiary fourth fat of peroxidating 2 ethyl hexanoic acid is 3.6ppmThe second initator (compressed air) content in effluent feed gas is 15ppm, the adjusting agent in main flow feeding gasThe content of propionic aldehyde is 210ppm, and the reaction temperature control of the first tubular reactor is 300～310 DEG C, and the second tubular type is anti-The reaction temperature control of answering device is 300～310 DEG C.
Embodiment 7
Concrete steps are with embodiment 1.
Wherein: main, effluent feed gas pressure is 235～245Mpa, in the first initator in main flow feed gas,The content of the tertiary fourth fat of peroxidating neodecanoic acid is 0.9ppm, and the content of the tertiary fourth fat of peroxidating 2 ethyl hexanoic acid is 3.6ppm,The second initator (compressed air) content in effluent feed gas is 13ppm, the adjusting agent in main flow feeding gasThe content of propionic aldehyde is 245ppm, and the reaction temperature control of the first tubular reactor is 300～315 DEG C, and the second tubular type is anti-The reaction temperature control of answering device is 300～315 DEG C.
Embodiment 8
Concrete steps are with embodiment 1.
Wherein: main, effluent feed gas pressure is 230～240Mpa, in the first initator in main flow feed gas,The content of the tertiary fourth fat of peroxidating neodecanoic acid is 1ppm, and the content of the tertiary fourth fat of peroxidating 2 ethyl hexanoic acid is 4ppm, sideThe content of the second initator (compressed air) in stream feed gas is 16ppm, the adjusting agent in main flow feeding gasThe content of propionic aldehyde is 210ppm, and the reaction temperature control of the first tubular reactor is 300～320 DEG C, and the second tubular type is anti-The reaction temperature control of answering device is 300～320 DEG C.
In the present invention, the method for testing of polyethylene testing standard and method is as follows:
Molecular weight distribution test: tested by gel permeation chromatography (GPC)
High performance liquid chromatography, chromatographic column is 3 series connection Plgel10 μ mMIXED-B posts. Solvent and mobile phase are1,2,4-trichloro-benzenes (containing 0.025% antioxidant 2,6-DBPC), 150 DEG C of column temperatures, flow velocity 1.0ml/min,Adopt Narrow distribution polystyrene standard specimen to carry out universal calibration. Test result is as follows:
In the present invention, after polyethylene special-purpose material sample, processing situation is as follows:
Claims (4)
1. a preparation method for polyethylene special-purpose material for car decorations nonwoven gum, is characterized in that, it adopts tubular type E methodHigh-pressure polymerization process device is prepared, and concrete steps are as follows:
(1) ethene, the first initator, the second initator and adjusting agent are compressed, after compression, be divided into two bursts of pressuresPower is master, the effluent feed gas of 230～250Mpa; Described main flow feed gas comprise ethene, the first initator andAdjusting agent, the content of described the first initator is 5 ± 0.5ppm, the content of adjusting agent is 225 ± 20ppm; DescribedEffluent feed gas comprises ethene and the second initator, and the content of described the second initator is 15 ± 2ppm; Wherein:Described the first initator is made up of the tertiary fourth fat of peroxidating neodecanoic acid and the tertiary fourth fat of peroxidating 2 ethyl hexanoic acid, peroxidating 2-The tertiary fourth fat of thylhexoic acid accounts for 80 ± 10% of initator gross weight; Described adjusting agent is C3～C10Aldehyde; DescribedTwo initators are through filtering and dry compressed air;
(2) main flow feed gas enters the first tubular reactor, is first heated to gradually 175 ± 10 DEG C with steam jacket,Carry out polymerisation at reaction zone again, polymerization temperature is 310～330 DEG C, and pressure is 240～250Mpa, the reaction timeIt is 7～8 seconds; Reaction finishes rear cooling, goes out the first reactor, then merges with the effluent feed gas that compressor is sent here;The reaction zone that enters the second tubular reactor carries out polymerisation, and polymerization temperature is 310～330 DEG C, and pressure is210～220Mpa, the reaction time is 11～12 seconds;
(3) after the second tubular reactor reaction, cooling, reactant mixture is again by the baiting valve of reactor exitStep-down, enters high stampings separator, carries out gas and feed separation; Then, the polyethylene product of molten entersLow stampings separator carries out gas and feed separation again, finally carries out extruding pelletization.
2. preparation method according to claim 1, is characterized in that: described adjusting agent is propionic aldehyde.
3. preparation method according to claim 1, is characterized in that: the car decorations nonwoven gum preparing is with poly-Ethene PP Pipe Compound has the melt index between 22g/10min～32g/10min, has 0.920～0.934g/cm3CloseDegree, molecular weight distributing index is 3～10, and hot strength is for being greater than 8Mpa, and tension failure strain is greater than 100%.
4. preparation method according to claim 3, is characterized in that: the car decorations nonwoven gum preparing is with poly-The melt index of ethene PP Pipe Compound is 25g/10min～29g/10min (190 DEG C, 2.16kg); Density is 0.921g/cm3～0.926g/cm3; Molecular weight distributing index is 4.5～6.5; Hot strength is greater than 9Mpa; Tension failure strain is greater than500％。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107880193A (en) * | 2016-09-29 | 2018-04-06 | 中国石油化工股份有限公司 | A kind of preparation method of the high melting means LDPE PP Pipe Compounds of PUR |
| WO2023034685A1 (en) | 2021-09-01 | 2023-03-09 | Exxonmobil Chemical Patents Inc. | Variable temperature tubular reactor profiles and intermediate density polyethylene compositions produced therefrom |
| CN116063596A (en) * | 2021-10-29 | 2023-05-05 | 中国石油化工股份有限公司 | High-pressure polyethylene for fruit string bag and preparation method and application thereof |
| CN116063603A (en) * | 2021-10-29 | 2023-05-05 | 中国石油化工股份有限公司 | High-pressure polyethylene injection molding material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107880193A (en) * | 2016-09-29 | 2018-04-06 | 中国石油化工股份有限公司 | A kind of preparation method of the high melting means LDPE PP Pipe Compounds of PUR |
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| CN116063603A (en) * | 2021-10-29 | 2023-05-05 | 中国石油化工股份有限公司 | High-pressure polyethylene injection molding material and preparation method thereof |
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