CN101704929B - Polyethylene-polystyrene resin and preparation method thereof - Google Patents
Polyethylene-polystyrene resin and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a polyethylene-polystyrene resin and a preparation method thereof. The preparation method comprises the following steps of: performing pre-irradiation treatment on polyethylene resin by using beta rays or gamma rays; adding the polyethylene resin after the pre-irradiation treatment, a dispersing agent, a functional monomer, an emulsifying agent, a nucleating agent and a homopolymerization inhibiting agent into a reactor to perform suspension graft polymerization reaction for a certain period of time at a certain temperature; and filtering, washing and drying a suspension graft product to obtain the polyethylene-polystyrene resin. The concentrations of macromolecular peroxides generated by the pre-irradiation are distributed evenly, so side reactions such as monomer homopolymerization, polymer crosslinking and/or degradation and the like caused by a micromolecule chemical initiator are avoided; the percent grafting ratio reaches 21 to 42 percent; the homopolymerization inhibiting agent reduces the homopolymerization of the monomer in the suspension grafting process; and the polyethylene-polystyrene resin has the tensile strength of more than 22 MPa, breaking elongation of over 90 percent and elastic modulus of more than 480 MPa, and has good mechanical properties such as strength, tenacity, impact strength and the like.
Description
Technical field
The present invention relates to a kind of polyethylene-polystyrene resin and preparation method thereof.
Background technology
Polyethylene and polystyrene all are widely used universal macromolecular materials, and these two kinds of polymkeric substance have its separately performance advantage and Application Areas of uniqueness.Polyethylene is a kind of material with higher-strength and toughness of crystallization, although and polystyrene has higher modulus and tensile strength, toughness is very poor, material itself is highly brittle and easy fracture.Because the difference of the chemical structure between this bi-material, crystallization behavior etc. causes the consistency extreme difference between these two kinds of polymkeric substance.
Functionalization and high performance are that polyolefine material improves product specification and the ratio of performance to price, expanded application field and market capacity, the main path that enhances the competitiveness and developing direction.Aspect polyolefine enforcement high performance, grafting, blend, alloying then are the Main Means of taking.Desired high-performance is mainly reflected in high strength, high-modulus, high rigidity, high ductility and the aspects such as high low-temperature impact resistance and energy absorption capacity, and this can obtain by the form of introducing corresponding chemical reaction or control co-mixing system between component.Because the consistency of polyethylene and polystyrene is poor, people attempt to obtain having concurrently from polyethylene and polystyrene blend the high-performance polymer of the two denominator.Although added expanding material, also be prone to being separated of polyethylene and polystyrene in the blend, impact processing and product properties.Chinese invention patent (the patent No.: ZL97105383.9) adopt the lightly crosslinked preparation polystyrene/polyethylene blend of micromolecular chemical initiator, although be lightly crosslinked, gel is arranged in the blend, will affect the machine-shaping of goods.If polyethylene and polystyrene can be linked together with covalent chemical bond, make it with polystyrene and poly characteristic, being separated in the course of processing can not appear just.
Contriver issued patents " a kind of functionalized polyolefin long-acting trickle film and preparation method thereof " (patent No. ZL200610016615.9), by adopting pre-irradiation and reaction to extrude function monomer is grafted on the molecular polyolefin chain, has prepared functionalized polyolefin long-acting trickle film.
Summary of the invention
One of purpose of the present invention provides a kind of polyethylene-polystyrene resin; Another object of the present invention provides a kind of preparation method of polyethylene-polystyrene resin.
A kind of polyethylene-polystyrene resin of the present invention, grafted polystyrene on the sub polyethylene subchain makes polyethylene be connected covalent chemical bond with polystyrene and connects, and the content of grafted polystyrene is at 21-42% (mass ratio).
Another object of the present invention provides a kind of preparation method of polyethylene-polystyrene resin, and its step and condition are:
(1) pre-irradiation of polyvinyl resin
Adopt
60Co carries out pre-irradiation with gamma-rays to polyvinyl resin as irradiation source, and the pre-irradiation dosage range is 5KGy-80KGy; Or adopt rumbatron as irradiation source, and with the β ray polyvinyl resin being carried out pre-irradiation, the pre-irradiation dosage range is 5KGy-80KGy;
(2) suspension polymerization of pre-irradiation polyvinyl resin
The pre-irradiation polyvinyl resin that step (1) is obtained, dispersion agent, function monomer, emulsifying agent, nucleator and equal polygalacturonase inhibitor join in the reactor, wherein, pre-irradiation polyethylene: dispersion agent: function monomer: emulsifying agent: nucleator: all the ratio of quality and the number of copies of polygalacturonase inhibitor is 5-12: 70-105: 1.5-3.6: 0.08-1: 0.05-0.2: 0.08-0.5, pass into nitrogen, heated and stirred, fluid temperature in the reactor is raised to 70-110 ℃, react after 4-6 hour, again add function monomer in reactor, the add-on of function monomer is with for the first time identical, continue reaction and finished reaction in 5-8 hour, reaction product is through overanxious, washing, drying obtains polyethylene-polystyrene resin;
Described polyvinyl resin is Low Density Polyethylene, high density polyethylene(HDPE) or linear low density polyethylene;
A kind of in described linear low density polyethylene optimal ethylene-butene-1 copolymer, ethene-1-hexene copolymer and the ethene-1-octene copolymer;
Described function monomer is vinylbenzene;
Described dispersion agent is deionized water;
Described emulsifying agent is Sodium dodecylbenzene sulfonate or sodium lauryl sulphate;
Described nucleator is one or more in phosphoric acid calcium powder, silicon dioxide powder and the titanium dioxide powder;
Described equal polygalacturonase inhibitor is ferrous sulfate or cuprous sulfate.
The preparation method of a kind of polyethylene-polystyrene resin provided by the invention by the pre-irradiation to polyvinyl resin, produces polymeric peroxide at the molecular chain of polyvinyl resin; Utilize the polymeric peroxide on the pre-irradiation polyvinyl resin molecular chain to be initiator, employing suspension polymerization technology is carried out graft polymerization with polyethylene and the vinylbenzene of pre-irradiation, with styrene-grafted on the sub polyethylene subchain, as carrying out polymerization, nuclear generates polystyrene take the vinylbenzene that is grafted on the sub polyethylene subchain, polystyrene is bonded together with covalent chemical bond mode and sub polyethylene subchain, because polyethylene is connected with covalent linkage with polystyrene, therefore the situation that is separated in the course of processing can not occur.
Beneficial effect: the polymeric peroxide concentration distribution that (1) adopts pre-irradiation to produce is even, has avoided homopolymerization and the side reactions such as crosslinked polymer and/or degraded of the monomer that the small molecules chemical initiator causes; (2) suspension polymerization long reaction time, percentage of grafting reach 21-42% (mass ratio), adopt equal polygalacturonase inhibitor to reduce the homopolymerization of monomer in the Suspension Graft process; (3) tensile strength of polyethylene-polystyrene resin is greater than 22MPa, and elongation at break is greater than 90%, and Young's modulus is greater than 480MPa, and the mechanical properties such as intensity, toughness, impact are good.
Embodiment
Embodiment 1 carries out pre-irradiation at the rumbatron device with the β ray with Low Density Polyethylene (LDPE), and pre-irradiation dosage is 5KGy.
Will be through 5 parts of the LDPE (quality) of pre-irradiation, 70 parts of deionized waters (quality), 1.5 parts of vinylbenzene (quality), 0.08 part of Sodium dodecylbenzene sulfonate (quality), 0.05 part in calcium phosphate (quality), agitator is equipped with in 0.08 part of (quality) adding of ferrous sulfate, thermometer, reflux condensing tube, liquid drips pipe, nitrogen is poured in the reactor of pipe and heating unit, pass into nitrogen, heated and stirred, fluid temperature in the reactor is raised to 70 ℃, react after 4 hours, again place liquid to drip pipe vinylbenzene 1.5 parts (quality), open liquid and drip the pipe switch, begin to drip liquid, time for adding 20 minutes, after dropwising, continue reaction 5 hours, finish reaction.Through washing, oven dry, obtaining percentage of grafting is 21% (mass ratio) polyethylene-polystyrene resin with reaction product.The tensile strength of polyethylene-polystyrene resin is (22.3MPa), and elongation at break is (128%), and Young's modulus is (492MPa).
Embodiment 2 is ethene-butene-1 copolymer, butene content 5% (quality),
60Carry out pre-irradiation with gamma-rays on the Co device, pre-irradiation dosage is 80KGy.
Will be through 12 parts of the ethene-butene-1 copolymers (quality) of pre-irradiation, 105 parts of deionized waters (quality), 3.6 parts of vinylbenzene (quality), 1 part of Sodium dodecylbenzene sulfonate (quality), 0.2 part in calcium phosphate (quality), agitator is equipped with in 0.5 part of (quality) adding of ferrous sulfate, thermometer, reflux condensing tube, liquid drips pipe, nitrogen is poured in the reactor of pipe and heating unit, pass into nitrogen, heated and stirred, fluid temperature in the reactor is raised to 105 ℃, react after 6 hours, again place liquid to drip pipe vinylbenzene 3.6 parts (quality), open liquid and drip the pipe switch, begin to drip liquid, time for adding 20 minutes, after dropwising, continue reaction 8 hours, finish reaction.Through washing, oven dry, obtaining percentage of grafting is 42% (mass ratio) polyethylene-polystyrene resin with reaction product.The tensile strength of polyethylene-polystyrene resin is 22.5MPa, and elongation at break is 99%, and Young's modulus is 546MPa.
Embodiment 3 is with ethene-1-octene copolymer, and octene content 9% (quality) is carried out pre-irradiation at the rumbatron device with the β ray, and pre-irradiation dosage is 40KGy.
Will be through the ethene of pre-irradiation-10 parts of 1-octene copolymers (quality), 100 parts of deionized waters (quality), 2.5 parts of vinylbenzene (quality), 0.5 part of Sodium dodecylbenzene sulfonate (quality), 0.15 part in calcium phosphate (quality), agitator is equipped with in 0.3 part of (quality) adding of ferrous sulfate, thermometer, reflux condensing tube, liquid drips pipe, nitrogen is poured in the reactor of pipe and heating unit, pass into nitrogen, heated and stirred, fluid temperature in the reactor is raised to 90 ℃, react after 5 hours, again place liquid to drip pipe vinylbenzene 2.5 parts (quality), open liquid and drip the pipe switch, begin to drip liquid, time for adding 20 minutes, after dropwising, continue reaction 7 hours, finish reaction.Through washing, oven dry, obtaining percentage of grafting is 30% (mass ratio) polyethylene-polystyrene resin with reaction product.The tensile strength of polyethylene-polystyrene resin is 23.2, and elongation at break is 131%, and Young's modulus is 512MPa.
Embodiment 4 is with ethene-1-hexene copolymer, and hexene content 8% (quality) carries out pre-irradiation at the rumbatron device with the β ray, and pre-irradiation dosage is 80KGy.
Will be through the ethene of pre-irradiation-9 parts of 1-hexene copolymers (quality), 95 parts of deionized waters (quality), 2 parts of vinylbenzene (quality), 0.65 part of Sodium dodecylbenzene sulfonate (quality), 0.15 part in calcium phosphate (quality), agitator is equipped with in 0.3 part of (quality) adding of ferrous sulfate, thermometer, reflux condensing tube, liquid drips pipe, nitrogen is poured in the reactor of pipe and heating unit, pass into nitrogen, heated and stirred, fluid temperature in the reactor is raised to 85 ℃, react after 5 hours, again place liquid to drip pipe vinylbenzene 2 parts (quality), open liquid and drip the pipe switch, begin to drip liquid, time for adding 20 minutes, after dropwising, continue reaction 6 hours, finish reaction.Through washing, oven dry, obtaining percentage of grafting is 27% (mass ratio) polyethylene-polystyrene resin with reaction product.The tensile strength of polyethylene-polystyrene resin is 23.9MPa, and elongation at break is, 152%, and Young's modulus is 495MPa.
Embodiment 5 carries out pre-irradiation at the rumbatron device with the β ray with high density polyethylene(HDPE), and pre-irradiation dosage is 60KGy.
Will be through 12 parts of the high density polyethylene(HDPE)s (quality) of pre-irradiation, 95 parts of deionized waters (quality), 3.4 parts of vinylbenzene (quality), 0.5 part of Sodium dodecylbenzene sulfonate (quality), 0.2 part in calcium phosphate (quality), agitator is equipped with in 0.4 part of (quality) adding of ferrous sulfate, thermometer, reflux condensing tube, liquid drips pipe, nitrogen is poured in the reactor of pipe and heating unit, pass into nitrogen, heated and stirred, fluid temperature in the reactor is raised to 100 ℃, react after 4 hours, again place liquid to drip pipe vinylbenzene 3.4 parts (quality), open liquid and drip the pipe switch, begin to drip liquid, time for adding 20 minutes, after dropwising, continue reaction 7 hours, finish reaction.Through washing, oven dry, obtaining percentage of grafting is 35% (mass ratio) polyethylene-polystyrene resin with reaction product.The tensile strength of polyethylene-polystyrene resin is 23.5MPa, and elongation at break is 123%, and modulus in tension is 487MPa.
Embodiment 6 is ethene-butene-1 copolymer, butene content 5% (quality),
60Carry out pre-irradiation with gamma-rays on the Co device, pre-irradiation dosage is 50KGy.
Will be through 10 parts of the ethene-butene-1 copolymers (quality) of pre-irradiation, 90 parts of deionized waters (quality), 2.5 parts of vinylbenzene (quality), 0.8 part of Sodium dodecylbenzene sulfonate (quality), 0.15 part in calcium phosphate (quality), agitator is equipped with in 0.35 part of (quality) adding of ferrous sulfate, thermometer, reflux condensing tube, liquid drips pipe, nitrogen is poured in the reactor of pipe and heating unit, pass into nitrogen, heated and stirred, fluid temperature in the reactor is raised to 90 ℃, react after 4 hours, again place liquid to drip pipe vinylbenzene 2.5 parts (quality), open liquid and drip the pipe switch, begin to drip liquid, time for adding 20 minutes, after dropwising, continue reaction 8 hours, finish reaction.Through washing, oven dry, obtaining percentage of grafting is 31% (mass ratio) polyethylene-polystyrene resin with reaction product.The tensile strength of polyethylene-polystyrene resin is 23.1MPa, and elongation at break is 122%, and modulus in tension is 473MPa.
Claims (3)
1. a polyethylene-polystyrene resin is characterized in that, grafted polystyrene on the sub polyethylene subchain makes polyethylene be connected covalent chemical bond with polystyrene and connects, and the mass content of grafted polystyrene is 21-42%, and is made by following methods:
(1) adopts
60Co carries out pre-irradiation with gamma-rays to polyvinyl resin as irradiation source, and the pre-irradiation dosage range is 5KGy-80KGy; Perhaps, adopt rumbatron as irradiation source, with the β ray polyvinyl resin is carried out pre-irradiation, the pre-irradiation dosage range is 5KGy-80KGy;
(2) the pre-irradiation polyvinyl resin that step (1) is obtained, dispersion agent, function monomer, emulsifying agent, nucleator, all polygalacturonase inhibitor joins in the reactor, wherein, pre-irradiation polyethylene: dispersion agent: function monomer: emulsifying agent: nucleator: all the ratio of quality and the number of copies of polygalacturonase inhibitor is 5-12: 70-105: 1.5-3.6: 0.08-1: 0.05-0.2: 0.08-0.5, pass into nitrogen, heated and stirred, fluid temperature in the reactor is raised to 70-110 ℃, react after 4-6 hour, again add function monomer in reactor, the add-on of function monomer is with for the first time identical, continue reaction and finished reaction in 5-8 hour, reaction product after filtration, washing, drying obtains polyethylene-polystyrene resin;
Described polyvinyl resin is Low Density Polyethylene, high density polyethylene(HDPE) or linear low density polyethylene;
Described function monomer is vinylbenzene;
Described dispersion agent is deionized water;
Described emulsifying agent is Sodium dodecylbenzene sulfonate or sodium lauryl sulphate;
Described nucleator is one or more in phosphoric acid calcium powder, silicon dioxide powder, the titanium dioxide powder;
Described equal polygalacturonase inhibitor is ferrous sulfate or cuprous sulfate.
2. the preparation method of a kind of polyethylene-polystyrene resin as claimed in claim 1 is characterized in that, its step and condition are as follows:
(1) pre-irradiation of polyvinyl resin
Adopt
60Co carries out pre-irradiation with gamma-rays to polyvinyl resin as irradiation source, and the pre-irradiation dosage range is 5KGy-80KGy; Perhaps, adopt rumbatron as irradiation source, with the β ray polyvinyl resin is carried out pre-irradiation, the pre-irradiation dosage range is 5KGy-80KGy;
(2) suspension polymerization of pre-irradiation polyvinyl resin
The pre-irradiation polyvinyl resin that step (1) is obtained, dispersion agent, function monomer, emulsifying agent, nucleator, all polygalacturonase inhibitor joins in the reactor, wherein, pre-irradiation polyethylene: dispersion agent: function monomer: emulsifying agent: nucleator: all the ratio of quality and the number of copies of polygalacturonase inhibitor is 5-12: 70-105: 1.5-3.6: 0.08-1: 0.05-0.2: 0.08-0.5, pass into nitrogen, heated and stirred, fluid temperature in the reactor is raised to 70-110 ℃, react after 4-6 hour, again add function monomer in reactor, the add-on of function monomer is with for the first time identical, continue reaction and finished reaction in 5-8 hour, reaction product after filtration, washing, drying obtains polyethylene-polystyrene resin;
Described polyvinyl resin is Low Density Polyethylene, high density polyethylene(HDPE) or linear low density polyethylene;
Described function monomer is vinylbenzene;
Described dispersion agent is deionized water;
Described emulsifying agent is Sodium dodecylbenzene sulfonate or sodium lauryl sulphate;
Described nucleator is one or more in phosphoric acid calcium powder, silicon dioxide powder, the titanium dioxide powder;
Described equal polygalacturonase inhibitor is ferrous sulfate or cuprous sulfate.
3. the preparation method of a kind of polyethylene-polystyrene resin claimed in claim 2 is characterized in that, described linear low density polyethylene is a kind of in ethene-butene-1 copolymer, ethene-1-hexene copolymer and the ethene-1-octene copolymer.
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| CN102492096A (en) * | 2011-11-11 | 2012-06-13 | 中国科学院长春应用化学研究所 | Polypropylene-polystyrene resin and preparation method thereof |
| CN102505474B (en) * | 2011-11-29 | 2013-12-18 | 中国科学院上海应用物理研究所 | Modified ultrahigh molecular weight polyethylene fiber and preparation method thereof |
| CN105940025A (en) * | 2014-03-12 | 2016-09-14 | 积水化成品工业株式会社 | Composite resin particles, foamable particles, pre-foamed particles, and foam molded body |
| CN109265791B (en) * | 2018-08-01 | 2020-07-10 | 西安交通大学 | High-voltage direct-current cable insulating material and preparation method thereof |
| CN109265803B (en) * | 2018-09-11 | 2021-02-09 | 江南大学 | Polystyrene/polyethylene interpolymer composite material and preparation method thereof |
| CN111925481A (en) * | 2020-08-24 | 2020-11-13 | 安徽联科水基材料科技有限公司 | Corrosion-resistant PE/PS alloy suitable for refrigerator liner and preparation method thereof |
| CN112280184A (en) * | 2020-11-10 | 2021-01-29 | 中嘉卫华（固安）新材料科技有限公司 | Electron irradiation crosslinking foaming polypropylene heat preservation belt and preparation method thereof |
| CN115850834B (en) * | 2022-11-28 | 2023-06-27 | 南通大学 | High-performance polyethylene/nano silicon dioxide composite cable insulating resin and preparation method and application thereof |
| CN116285068A (en) * | 2023-04-20 | 2023-06-23 | 东莞市塘厦鸿联吸塑厂 | High-elasticity toughened PE modified material and preparation method thereof |
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| US6849688B2 (en) * | 2002-03-26 | 2005-02-01 | Sachem, Inc. | Polymer grafted support polymers |
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