CN1884358A - Chlorinated polyethylene composite elastomer production method - Google Patents
Chlorinated polyethylene composite elastomer production method Download PDFInfo
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- CN1884358A CN1884358A CN 200510016905 CN200510016905A CN1884358A CN 1884358 A CN1884358 A CN 1884358A CN 200510016905 CN200510016905 CN 200510016905 CN 200510016905 A CN200510016905 A CN 200510016905A CN 1884358 A CN1884358 A CN 1884358A
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Abstract
The invention provides a method for preparing chlorinated polyethylene composite elastic body, belonging to radiation crosslinking field of high molecular material. The method comprises: employ CPE as main body, adding polyolefine, filler, stabilizer and plasticizing agent, stirring at room temperature with stirrer, granulating with extrusion machine, moulding wit hmolding press, and radiation crosslinking with cobalt. The invention is characterized by homogeneity, simpler process, wide processing temperature range and reusable material. The continuous pipe, sheet material and section bar can also be prepared, which enlarges application range of composite material.
Description
Technical field
The invention belongs to the radiation crosslinking field of macromolecular material.
Technical background
Chlorinatedpolyethylene (be called for short CPE) on polyethylene (PE) basis through chlorine atom replacement molecular chain top hydrogen atom and form.Because the introducing of polar group chloro.PE is become macroscopical homogeneous phase, the microcosmic heterogenetic macromolecular compound of polarity one nonpolar district coexistence by non-polar high polymer, show diverse characteristic with PE, topmost have: vinyl-chloride-containing has elasticity as the rubber, flame retardant resistance, ozone resistance etc. after crosslinked.Simultaneously, with the particularly also significantly increase of consistency of polar material of other material, thereby obtained to use widely.In the last few years, CPE was used for modified hard polyethylene chloride (PVC) in a large number, produced low temperature resistant electric wire, coating, tackiness agent, transition pipeline, pneumatic tube, sealing member etc.
Have manyly about the research of CPE, adopt CPE to make the thermal-insulating waterproof coiled materials as Chinese patent 98110127; " elastomerics " (1992 second volume fourth phases) discussed the performance of CPE/ neoprene latex composite water-proof rolled material; JP2001226546 makes high pressure resistant pipe with the crosslinked CPE of organo-peroxide; JP2002061757, US5914195 are with the compound material system valve seal of CPE pad; EP1227127 makes with the CPE/PVC mixture and intercepts CO
2Moulding compound; US5584950, US5639545 makes the sound insulation film with the PVC/CPE/EVA mixture; US5587419, US5641826 extrudes the hard section bar with the PVC/CPE blend; US6140423 is with the CPE/MBS extruding pipe material, and US5728772 makes thermoplastic elastomer with CPE/ polyester block polymkeric substance.From these research materials as can be seen, CPE and many macromolecular materials all have good consistency, can make multiple composite modification material, are used for different occasions.In addition, also just because of CPE is the polymer of doping region and the heterogeneous distribution in nonpolar district, so under suitable temperature, can show as plasticity, and its visco-elasticity significantly improves under higher temperature, is difficult to show the viscosity flow of plasticlike, by obtaining comparatively ideal elasticity after crosslinked.
In CPE content less material, CPE fully shows the visco-elasticity of its unit molecule state, can obviously improve shock resistance, the lower temperature resistance of matrix material; In matrix material, have only through just obtaining the product of higher-strength and other performance after crosslinked based on CPE.At present this class matrix material substantially all be with superoxide, sulfide as linking agent, process by the method consistent with processing rubber.This technology more complicated, main is to prevent the linking agent premature decomposition, simultaneously sulfidation is had strict control, facility investment, labour intensity are all very high.If with higher polymer blended of fusing point, the then more difficult control of technology, need, cause tooling cost to rise through the high low temperature course of processing of multiple.
Summary of the invention
The objective of the invention is:
A kind of chlorinated polyethylene composite elastomer production method is provided, this method adopts the method that does not add vulcanizing agent to make CPE blend composite elastic material, make and give behind the work in-process crosslinkedly again with method of radiating, finally obtain high performance elasticity tubing, sheet material or other moulded work.
Manufacture method of the present invention is:
1, based on CPE, its content is counted with parts by weight: 100; Add polyolefine, parts by weight: 0～200; Filler (comprising strengthening agent) parts by weight: 20～200; Stablizer parts by weight: 1～10; Softening agent parts by weight: 5～60.
2, after these materials stir through stirrer at normal temperatures, use twin screw extruder or two roller mill, make modification CPE masterbatch at 80～140 ℃ of temperature range mixing granulators.
3, this masterbatch can be through forcing machine extruding pipe material, sheet material, profiled material 80～140 ℃ of temperature ranges, and rolling press extrudes sheet material, and the moulding press mold pressing goes out abnormal member, gasket etc.
4, promptly through the cobalt source
60C0 source or rumbatron radiation crosslinking, irradiation dose is 4～20Mrad, becomes finished product.
CPE is the chlorinatedpolyethylene of cl content in 20～49% scopes.
Polyolefine is the polymkeric substance based on the ethene chain link, and this polyolefine has high density polyethylene(HDPE) (HDPE), new LDPE (film grade) (LDPE), linear low density polyethylene (LLDPE), polyethylene vinyl acetate (EVA).
Filler has carbon black, white carbon black, magnesium oxide, magnesium hydroxide, talcum powder, lime carbonate, Magnesium Silicate q-agent, kaolin.
The one package stabilizer that stablizer has lead silicate, dibasic lead phosphite, lead sulfate tribasic, toxilic acid dibutyl tin, lauric acid butyl tin, barium stearate, calcium stearate and contains these stablizers.
Softening agent has ISOPROPYL PHENYL DIPHENYL PHOSPHATE, trioctyl phosphate, three different monooctyl esters, the phthalic acid alkyl esters, and the alkyl in the phthalic acid alkyl esters is made of 4～20 methynes.
The phthalic acid alkyl esters has dioctyl phthalate (DOP), phthalic acid tridecyl ester, trioctyl trimellitate, epoxy soybean oil, polyester polyol, certain herbaceous plants with big flowers two dioctyl phthalates, Octyl adipate.
The invention has the beneficial effects as follows:
Because high-energy, the high penetrating power of ray, the integral body of energy atarting material is evenly crosslinked, solved the unhomogeneity of chemically crosslinked, owing to do not add vulcanizing agent, so whole process flow is much simple relatively, can adopt common extrusion equipment to process, but also greatly widens in the processing temperature interval of material, two defective materials can also reuse, and do not influence performance.Also can make crosslinked tubing, sheet material, the section bar of continuous length simultaneously.Thereby improved the range of application of matrix material, can also increase with the macromolecular material kind of CPE blend.
Embodiment
CPE chlorinity selected in the prescription is between 20～49%, and this CPE replaces partly with chlorine that hydrogen atom makes on the basis of PE, and its reparation technology is referring to patent US5525651 etc.When its cl content was too low, CPE mainly presented plasticity, was difficult to form elastomerics; When cl content was too high, material plasticity also improved, and thermostability descends simultaneously.Selected polyolefine can be various polyethylene in the prescription, as the polyethylene of high-density, middle density, low density, extremely-low density, also can be other polyolefine such as ethylene-vinyl acetate copolymer (EVA), ethylene-propylene copolymer.Adding one of polyolefinic purpose is mechanical property, the raising processing characteristics of strongthener.
Also add various fillers in the prescription, comprise strengthening agent and general fillibility filler.Mainly contain carbon black, white carbon black, magnesium oxide, magnesium hydroxide, talcum powder, lime carbonate, Magnesium Silicate q-agent, kaolin.Add filler and can promote to process, reduce cost, improve performance.
Suitably add stablizer in the prescription and in the course of processing, degrade, prolong its work-ing life simultaneously to avoid material.The one package stabilizer that such stablizer has lead silicate, dibasic lead phosphite, lead sulfate tribasic, toxilic acid dibutyl tin, lauric acid butyl tin, barium stearate, calcium stearate and contains these stablizers.
In order to reduce the material viscosity that adds man-hour, also should add softening agent, phosphoric acid ester such as ISOPROPYL PHENYL DIPHENYL PHOSPHATE, trioctyl phosphate, three different monooctyl esters are wherein arranged; The phthalic acid alkyl esters, wherein alkyl is made of 4～20 methynes, and is main as dioctyl phthalate (DOP), phthalic acid tridecyl ester; Trioctyl trimellitate; Epoxy soybean oil; Polyester polyol: certain herbaceous plants with big flowers two dioctyl phthalates; Octyl adipate.
The mixing of these materials is at room temperature carried out, and various pulverulent materials is added in the stirrer to stir earlier, adds liquid adjuvants then, and the back that stirs adds pelletized polyolefin, continues to be stirred to evenly discharging.Compound is plasticated between 80～140 ℃ in flakes through mill, pelletizing; Or in this temperature range through the twin screw extruder extruding pelletization.Pellet packing back is standby.
This pellet can be with common single screw extrusion machine equipment (special single screw extrusion machine is preferably arranged) extruding pipe material, sheet material or section bar; Also can directly be molded as various elastic components such as gasket, snubber etc.
The sulfuration of product at room temperature uses cobalt source or rumbatron to carry out, and total irradiation dose scope is at 4～20Mrad.When dosage was too low, clearly the degree of crosslinking of product was also low, did not reach suitable mechanics requirement, when dosage is too high, because energetic ray or rumbatron ejected electron that the cobalt source produces all are high energy particles, its energy is enough to activate polymer, and it is intermolecular crosslinked that it is taken place, also be enough to interrupt molecular chain, produce degraded, on the other hand, if the free radical that produces is too many, also can react, cause degraded with oxygen in the environment, moisture content etc.So the appropriate dosage scope is right.When extrude be continuous long products the time, also can carry out the successive radiation crosslinking, thereby significantly improve production efficiency.
The performance test of product can be according to the testing method of general-purpose plastics or rubber, and main indexes has anti-ozone ageing, heat-proof aging, mechanical property etc.
Embodiment one: proportioning: CPE (20% cl content is weight ratio, down together): 100; Linear low density polyethylene (LLDPE7042): 20; Lead silicate: 10; Light calcium carbonate: 50; Dioctyl phthalate (DOP): 20; Carbon black (N 330): 40.Earlier each pulverulent material (CPE, lead silicate, light calcium carbonate, carbon black) is added in the stirrer and stirred 3～6 minutes down, add the plasticizer phthalic acid dioctyl ester, stirred 2 minutes, add pellet LLDPE again, continue to stir discharging 2 minutes in low speed.Mixture uses the twin screw extruder extruding pelletization, and 80～140 ℃ of prilling temperatures, gained pellet are extruded diameter 8mm under 80～140 ℃, and the continuous long tube material of wall thickness 2mm through electron accelerator irradiation 8Mrad, gets production tube.
Embodiment two: CPE (35% chlorine): 100; EVA (1405): 10; Dibutyl tin laurate: 1; Light calcium carbonate: 10; Trioctyl phosphate: 10; Carbon black: 10; Magnesium oxide: 5; Stearic acid: 2.Material is taked the technology identical with embodiment one, adopts multiple roll machine rolling out film material, and crosslinked through cobalt-60 radiosterilize, dosage is 10Mrad, and resulting sheet has good soft elasticity.
Embodiment three: CPE (49% chlorine): 100; LDPE (18D): 100; Toxilic acid dibutyl tin: 1; Antioxidant 1010: 0.2; Water-ground limestone: 100, carbon black (general): 60; Magnesium oxide: 10; Stearic acid: 2; Trioctyl trimellitate: 40.Material through with embodiment one similar granulation process after, the wide 50cm of extrusion sheet, thick 2mm, continuous irradiation 20Mrad under the cobalt source, sheet material has tough elasticity.
Embodiment four: proportioning: CPE (25% chlorine); 50; CPE (49% chlorine): 50; HDPE:200; White carbon black: 100; Magnesium oxide: 2; Hard ester acid: 1; Polyester polyol: 10; Epoxy soybean oil: 10.Material according to the identical technology mixing granulation of embodiment one after, be molded into the elasticity abnormal member, through cobalt-60 radiosterilize 6Mrad, crosslinked back product can be used for the buffer substrate tablet of anti-ozone, sealing member.
Embodiment five: CPE (35% chlorine): 100; LLDPE (7042): 40; LDPE (1I20A): 20; Lead sulfate tribasic: 6; Magnesium hydroxide (Mg (OH)
2): 30; Light calcium carbonate: 30; Carbon black: 40; ISOPROPYL PHENYL DIPHENYL PHOSPHATE: 20; Epoxy soybean oil: 10; Stearic acid: 5.Material according to the identical technology mixing granulation of embodiment one after, be used to make waterproof roll, through the cobalt source or electron accelerator irradiation 4Mrad.Can obtain the finished product sheet material.
Embodiment six: CPE (35% chlorine): 100; Lead silicate: 8; Mg (OH)
2: 10; MgO:8; Stearic acid: 3: trioctyl phosphate: 30; Water-ground limestone: 50; Carbon black: 60.Material according to the identical technology mixing granulation of embodiment one after, extrude flexible pipe through forcing machine, through the cobalt source or accelerator irradiation 8～12Mrad, become crosslinked elastic hose, can be used for oil pipe, water pipe, have good alkali resistance, oil-proofness.
Embodiment seven: CPE (25% chlorine): 100; Lead sulfate tribasic: 2; Barium stearate: 2; Calcium stearate: 1; Dioctyl sebacate: 20; Octyl adipate: 20; Talcum powder: 30; Kaolin: 30; Carbon black: 30.Material according to the identical technology mixing granulation of embodiment one after, through forcing machine extrusion profile sealed strip, adopt electron accelerator irradiation 10Mrad, the gained sealed strip has excellent resistance to low temperature.
Claims (7)
1, a kind of chlorinated polyethylene composite elastomer production method, its method is:
A, based on CPE, its content is counted with parts by weight: 100; Add polyolefine, parts by weight: 0～200; Filler weight umber: 20～200; Stablizer parts by weight: 1～10; Softening agent parts by weight: 5～60;
B, these materials use twin screw extruder or two roller mill at 80～140 ℃ of temperature range mixing granulators after stirring through stirrer at normal temperatures, make modification CPE masterbatch;
C, this masterbatch can be through forcing machine extruding pipe material, sheet material, profiled materials 80～140 ℃ of temperature ranges, and rolling press extrudes sheet material, and the moulding press mold pressing goes out abnormal member, gasket etc.;
D, promptly through the cobalt source
60Co source or rumbatron radiation crosslinking, irradiation dose is 4～20Mrad, becomes finished product.
2, a kind of chlorinated polyethylene composite elastomer production method according to claim 1, its method is: CPE is the chlorinatedpolyethylene of cl content in 20～49% scopes.
3, a kind of chlorinated polyethylene composite elastomer production method according to claim 1, its method is: polyolefine is the polymkeric substance based on the ethene chain link, and this polyolefine has high density polyethylene(HDPE) (HDPE), new LDPE (film grade) (LDPE), linear low density polyethylene (LLDPE), polyethylene vinyl acetate (EVA).
4, a kind of chlorinated polyethylene composite elastomer production method according to claim 1, its method is: filler has carbon black, white carbon black, magnesium oxide, magnesium hydroxide, talcum powder, lime carbonate, Magnesium Silicate q-agent, kaolin.
5, a kind of chlorinated polyethylene composite elastomer production method according to claim 1, its method is: the one package stabilizer that stablizer has lead silicate, dibasic lead phosphite, lead sulfate tribasic, toxilic acid dibutyl tin, lauric acid butyl tin, barium stearate, calcium stearate and contains these stablizers.
6, a kind of chlorinated polyethylene composite elastomer production method according to claim 1, its method is: softening agent has ISOPROPYL PHENYL DIPHENYL PHOSPHATE, trioctyl phosphate, three different monooctyl esters, the phthalic acid alkyl esters, the alkyl in the phthalic acid alkyl esters is made of 4～20 methynes.
7, according to claim 1 and 6 described a kind of chlorinated polyethylene composite elastomer production methods, its method is: the phthalic acid alkyl esters has dioctyl phthalate (DOP), phthalic acid tridecyl ester, trioctyl trimellitate, epoxy soybean oil, polyester polyol, certain herbaceous plants with big flowers two dioctyl phthalates, Octyl adipate.
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| CN101781426A (en) * | 2010-03-02 | 2010-07-21 | 扬州华声电子实业有限公司 | CPE/POE (chlorinated polyethylene/polyolefin elastomer) component type electro-insulating rubber and preparation method thereof |
| CN101920549A (en) * | 2009-06-17 | 2010-12-22 | 北京化工大学 | Preparation of Wide Width Chlorinated Polyethylene Waterproof Membrane by Extrusion |
| CN102276935A (en) * | 2011-05-10 | 2011-12-14 | 广东华声电器股份有限公司 | Parallel flexible cord for heater and preparation method thereof |
| CN101942151B (en) * | 2009-07-10 | 2012-05-02 | 广东华声电器股份有限公司 | CPE/POE/LDPE component type insulating rubber and preparation method thereof |
| CN102432958A (en) * | 2010-11-03 | 2012-05-02 | 如皋市中如化工有限公司 | Cold-resistance and flame-retardant level PVC (polyvinyl chloride) cable material |
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| CN105037982A (en) * | 2015-07-31 | 2015-11-11 | 苏州新区特氟龙塑料制品厂 | Modified chlorinated polyethylene used for cables |
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| CN101920549A (en) * | 2009-06-17 | 2010-12-22 | 北京化工大学 | Preparation of Wide Width Chlorinated Polyethylene Waterproof Membrane by Extrusion |
| CN101942151B (en) * | 2009-07-10 | 2012-05-02 | 广东华声电器股份有限公司 | CPE/POE/LDPE component type insulating rubber and preparation method thereof |
| CN101781426A (en) * | 2010-03-02 | 2010-07-21 | 扬州华声电子实业有限公司 | CPE/POE (chlorinated polyethylene/polyolefin elastomer) component type electro-insulating rubber and preparation method thereof |
| CN101781426B (en) * | 2010-03-02 | 2013-09-11 | 扬州华声电子实业有限公司 | CPE/POE (chlorinated polyethylene/polyolefin elastomer) component type electro-insulating rubber and preparation method thereof |
| CN102432958B (en) * | 2010-11-03 | 2014-05-07 | 如皋市中如化工有限公司 | Cold-resistance and flame-retardant level PVC (polyvinyl chloride) cable material |
| CN102432958A (en) * | 2010-11-03 | 2012-05-02 | 如皋市中如化工有限公司 | Cold-resistance and flame-retardant level PVC (polyvinyl chloride) cable material |
| CN102276935A (en) * | 2011-05-10 | 2011-12-14 | 广东华声电器股份有限公司 | Parallel flexible cord for heater and preparation method thereof |
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| CN102924836A (en) * | 2012-11-27 | 2013-02-13 | 江苏达胜高聚物有限公司 | Twisting-resistant flexible cable material for wind power generation and preparation method for same |
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