CN100572441C - A kind of bonded polyolefine resin composition - Google Patents
A kind of bonded polyolefine resin composition Download PDFInfo
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- CN100572441C CN100572441C CNB2006100808362A CN200610080836A CN100572441C CN 100572441 C CN100572441 C CN 100572441C CN B2006100808362 A CNB2006100808362 A CN B2006100808362A CN 200610080836 A CN200610080836 A CN 200610080836A CN 100572441 C CN100572441 C CN 100572441C
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Abstract
The invention discloses a kind of bonded polyolefine resin composition, with the composition quality be absolutely than, mainly consist of: (1) 0.1～40% graft polypropylene, MFR:1～40; (2) 20～48% polypropylene, MFR:0.3～40; (3) 20～40% linear low density polyethylenes, MFR:0.8～10; (4) 10～30% high density polyethylene(HDPE)s, MFR:2～5; (5) 1～20% ethene and octene copolymers, the copolymerization in 1: 1 of ethene and octene, MFR:0.5～30; (6) 1～10% polystyrene; Wherein, graft polypropylene is to be first grafted monomer with unsaturated carboxylic acid, acid anhydrides or carboxylicesters, and vinylbenzene is that second grafted monomer obtains, and the percentage of grafting of the unsaturated carboxylic acid on the polypropylene, acid anhydrides or carboxylicesters is 1%～10%.Metallic substance such as resin combination of the present invention and steel, iron, aluminium show good cohesiveness, its stripping strength 〉=80N/10mm, and the Vicat softening point of this material 〉=120 ℃ (GB 1613-90) satisfies the high temperature service requirements of pressure vessels for the chemical industry, pipeline.
Description
Technical field
The present invention relates to a kind of polyolefine resin composition, particularly is major ingredient with the acrylic resin, has the bonded polyolefine resin composition of high-peeling strength.
Background technology
The plastics impregnating material kind that is used for fields such as chemical industry, oil field, machinery, building at present is a lot, as Resins, epoxy, vibrin etc.But this resinoid belongs to thermosetting resin, and its processing is difficulty relatively.Polypropylene is as thermoplastics, have advantages such as physical and mechanical properties excellence, forming process is easy, density is little, but because polypropylene is a non-polar polymer, binding property, static resistance, wetting ability and all relatively poor with the consistency of other polarity polymers and mineral filler or metal have limited the application of polypropylene in this field.The polypropylene fusion graft monomer being made its polar, utilize the polarity and the reactivity of polar group, improve the deficiency on its performance, increase new character again simultaneously, is a kind of simple and efficient ways that enlarges the polypropylene material purposes.
In " modified poly propylene powdered coating and the preparation method " that deliver " chemical industry corrosion and protection " (Vol24.No.4 1996) at first with small portion polypropylene, grafts, initiator mixing in high-speed mixer, obtain the pellet of modified master, granulation then, in pulverize at low temperature, pulverize pellet at last, get modified polypropene coating, its stripping strength of filming reaches (N/10mm) 〉=2.5.
Chinese patent 92109066.8 disclosed a kind of modified poly propylene powdered coatings that are used for the metal base coating, with unsaturated carboxylic acid and acid anhydrides and organo-peroxide modification crystalline polypropylene, form blend with polyethylene, ethylene-alpha-olefin-non-conjugated diene hydrocarbon ter-polymer rubber, have excellent decoration and protection effect, stripping strength is greater than 32N/10mm, Vicat softening point is 140 ℃, is used for the anticorrosion of chemical pipeline, pail pack, pond groove etc.Chinese patent 99103515.1 relates to a kind of method for preparing high-polarity modified polypropylene material with maleic anhydride graft; this preparation method is parent stock with the polypropylene; add a certain proportion of maleic anhydride, cografting monomer and initiator; reacted 1-3 minute down at 170-220 ℃; use the tablets press granulation, be modified polypropylene material.This invents the high-polarity polypropylene material for preparing, and can improve the polarity of goods, improves the surface daub on a wall of goods, keeps the good mechanical property of pp material, and is low to the production unit requirement, but does not relate to its application.Chinese patent 96109985.2 has related to a kind of modified polypropene of the monomer graft modification that contains at least a unsaturated carboxylic acid and derivative thereof or has contained the composition of modified polypropene and contain at least a adhesive polypropylene resin composite that is selected from the monomer-grafted modified polyolefin of unsaturated carboxylic acid and derivative thereof, mainly uses three layers of composite laminates tack coat between polyolefine material and urethane.Chinese patent 01109835.x has related to a kind of by the part or all of grafted modified polypropene of unsaturated carboxylic acid or derivatives thereof and amorphous or low-crystallinity ethylene/alpha-olefin copolymer and a kind of modified poly propylene composition of styrenic elastomer blended, be mainly used in the laminating material matrix material more than three layers or three layers of the two-layer or three-decker between polyolefine material and the EVOH, this laminating material has intensity between excellent lamination, under 80～125 ℃ of high temperature, during thermal treatment, can prevent to reduce interlaminar strength.Chinese patent 01131134.7 provides a kind of tackifying resin composition, said composition is the hybrid resin of various kinds of resin such as grafted polyethylene and polyethylene, polypropylene, POE, polystyrene, this resin not only shows excellent bond performance with aluminium plastic material, stripping strength (N/10mm) 〉=40 physicals satisfies the requirement of aluminum-plastic laminated tube serialization manufacture, and also shows good cohesiveness with other materials.Particularly reach (N/10mm) 80 with firm band bounding force.
The high strength of patent JP2004075984 report and the acrylic resin synthetics of sur-face peeling are made up of acrylic resin and an epoxide modified acrylonitritrile-styrene resin mixing of a graft modification; Patent JP2150481 discloses and a kind ofly has been used for bonding between polypropylene and the polymeric amide by graft polypropylene and polypropylene compound tackifying resin, and maximum peeling strength can reach 42N/10mm; RU2144051 discloses and a kind ofly has been made up of isotaxy regular polypropylene or propylene, ethene crystal multipolymer etc., is used for its stripping strength of polyolefin compositions that metal tube applies and reaches 20～40N/mm; US4049355 discloses certain anticorrosion process, has kind of the material can be with metal and unvulcanized epoxy resin layer bonding in this technology, and the composition of this material is the graft-modified polyolefin of dicarboxylic acid graft polyolefin, the stripping strength＞19.6N/10mm of itself and metal; US5,441,999 have related to the modified polyolefin of a kind of low molecular weight propylene or propylene and ethylene butadiene terpolymer polyolefine and carboxylic acid graft modification and high score sub level functional polyolefin or multipolymer or vinyl-containing monomers gets a kind of tackifying resin of polymer combination, and this tackifying resin is mainly as packing, bookbinding tackifying resin; US5695838 discloses modified polypropene and other polyolefine adhesive polypropylene resin mixed with the modified polyolefin that contains a kind of carboxylic acid and derivative thereof at least of the grafted monomer grafting preparation of a kind of polypropylene and at least a carboxylic acid and derivative thereof, is mainly used in the MULTILAYER COMPOSITE laminating material of multi-layer composition and polyolefin layer/adhesive polypropylene/polymeric amide-ethylene copolymer layer; It mainly is by the polypropylene of propylene homopolymerization or propylene and ethylene, the terpolymer of propylene and ethylene butylene that US6426388 discloses a kind of polyolefine tackifying resin and toxilic acid is sweet, this material of styrene-grafted modified polyolefine material is mainly used in the bonding of non-polar material.
In sum, adopt copolymerization and grafting modification technology, the modified polypropene thermosol or the coating material of preparation pipeline corrosion protection, existing both at home and abroad bibliographical information, but stripping strength is substantially below 80N/10mm.
Summary of the invention
It is a kind of good with bonding effect metal to the purpose of this invention is to provide, and resistance toheat and physicals all satisfy the polyolefine resin composition of pressure vessels for the chemical industry and pipeline corrosion protection needs.
Resin combination provided by the invention is absolutely in the composition quality, mainly consists of:
0.1～40% graft polypropylene melt flow rate (MFR): 1～40
20～48% melt polypropylene flow rates: 0.3～40
20～40% linear low density polyethylene melt flow rate (MFR)s: 0.8～10
10～30% high density polyethylene(HDPE) melt flow rate (MFR)s: 2～5
1～20% ethene and octene copolymer ethene and octene copolymerization in 1: 1,
Melt flow rate (MFR): 0.5～30
1～10% polystyrene
Graft polypropylene is to be first grafted monomer with unsaturated carboxylic acid, acid anhydrides or carboxylicesters, vinylbenzene is second grafted monomer, superoxide is an initiator, and the weight ratio of polypropylene and grafted monomer is obtaining by fusion-grafting or solution graft copolymerization for 10: 1～5: 1 times; Wherein, it is 10: 1～1: 1 that first and second monomer adds weight ratio, and the percentage of grafting of the unsaturated carboxylic acid on the polypropylene, acid anhydrides or carboxylicesters is 1%～10%.
The present invention does not have particular requirement to peroxide initiator, and its transformation period and temperature of reaction and reaction times are complementary and get final product, and commonly used is dicumyl peroxide, tertbutyl peroxide, and its consumption is 0.1 ‰～5 ‰ in composition absolutely.
Unsaturated carboxylic acid, acid anhydrides or carboxylicesters can have following selection: vinylformic acid, methacrylic acid, maleic acid, 2-methylene-succinic acid, along wherein a kind of of pyrovinic acid, methyl 2-Succinic Acid, MALEIC ANHYDRIDE, 4-methyl-4-tetrahydrobenzene-1,2 dicarboxylic anhydride diolefine maleate, diolefine 2-methylene radical butylene diester, methyl methacrylate, methacrylic ester, alkylmethacrylate or vinylformic acid carboxylic propyl ester.Preferred MALEIC ANHYDRIDE (MAH).
The preparation of graft polypropylene can be carried out in twin screw extruder or Brabender pony mixer, and processing temperature is 190～230 ℃, reaction times 5～10min; Also can in acidproof, alkaline-resisting corrosion resistant reaction vessel, carry out solution graft copolymerization, 80～120 ℃ of temperature of reaction, the reaction times is 1.5～2h.
The polypropylene of mentioning in the above-mentioned composition comprises the polypropylene that polypropylene that grafting is used and blend are used, and can be identical, also can be different polypropylene.Can be various homo-polypropylene, atactic copolymerized polypropene or block copolymerization polypropylene, its melt flow rate (MFR) be 0.3～40.Wherein the polypropylene of melt flow rate (MFR) 0.3～10 mainly is satisfied with the anticorrosion preparation with graft polypropylene of small-bore MULTILAYER COMPOSITE pipeline, and heavy caliber MULTILAYER COMPOSITE pipeline is satisfied with by the polypropylene of melt flow rate (MFR) 10～40 and pressure vessels for the chemical industry applies anticorrosion preparation with graft polypropylene.For the selection of graft polypropylene base-material, preferably adopt block copolymerization polypropylene.
Composition of the present invention can also add Hinered phenols, suffocated amine antioxidant in preparation process, oxidation inhibitor can be to mix oxidation inhibitor, also can be single oxidation inhibitor.In the composition is that absolutely its consumption is 0～2.5 ‰.
Preparation of compositions can be carried out in forcing machine, and the forcing machine processing temperature is 170～280 ℃, and be 30s～15min process period; Also can carry out in mill or Banbury mixer, its processing temperature is 150～260 ℃, mixing time 〉=5min.
The present invention has adopted the monomer-grafted system of two-pack, because vinylbenzene is to the reactivity ratio MAH height of polypropylene macromolecular radical, vinylbenzene preferentially is grafted on the polypropylene, form more stable styryl macromolecular radical, react with MAH more afterwards, therefore its speed of reaction can improve percentage of grafting, and can effectively reduce polyacrylic DeR much larger than the speed of reaction of MAH and polypropylene macromolecular radical.
Simultaneously, the adding of linear low density polyethylene (LLDPE), high density polyethylene(HDPE) (HDPE) makes composition have better elongation, tear resistance.The side chain that LLDPE is short and small can make and form hydrogen bond and the Van der Waals force that is evenly distributed between LLDPE and graft polypropylene, the polypropylene, mixes more even.Ethene and octene copolymer (POE) are as a kind of thermoplastic elastomer in the component, in polypropylene, form less rubber areas and be dispersed in the toughness that has improved material in the hybrid resin material uniformly, prevent the infringement of thump pressure vessels for the chemical industry and pipeline with polypropylene.
In addition, in the continuous course of processing, particularly in the continuous flow procedure of anti-corrosion pipeline, need mixing material better in the molten state current downflow, but after mixing, graft polypropylene and polypropylene, polyethylene particularly add the similar netted structure that polyolefinic C-H long-chain forms behind the POE elastomerics, mixing material is restricted in the molten state current downflow, adds polystyrene introducing rigid radical and can improve material in the molten state current downflow.Analyzing reason, to think that the adding of rigid radical makes in the system that the C-H long-chain is subjected to " obstruct " similar reticulated structure destroyed, and the molecular weight distribution of material has been widened in macromolecular introducing, improve mixing material molten state current downflow, thereby improved the processing characteristics of mixing material.
Metallic substance such as resin combination of the present invention and steel, iron, aluminium show good cohesiveness, its stripping strength 〉=80N/10mm, and the Vicat softening point of this material 〉=120 ℃ (GB 1613-90) satisfies the high temperature service requirements of pressure vessels for the chemical industry, pipeline.
Embodiment
Analysis test method
1. the mensuration of the percentage of grafting of MAH on the polypropylene
Polypropylene grafted thing is put into three-necked bottle, add 100mL dimethylbenzene reflux to sample and all dissolve, add acetone then; Unreacted monomer and autopolymer thereof are dissolved in solution, and polypropylene and grafts precipitate, and throw out is dried 24h behind suction filtration.Grafts after the purification carries out Infrared spectroscopy with infrared spectrometer to sample through 190 ℃ of compressing tablet film forming, and the result calculates the ratio of characteristic peak absorbancy.During quantitative analysis with 2723cm
-1The polypropylene characteristic peak at place is as interior mark, respectively to the maleic anhydride characteristic peak (1782cm on the infrared spectrum
1And 1790cm
-1) and polypropylene characteristic peak (2723cm
-1) peak area measure, the ratio of its peak area is the ratio of two group absorbancys.It has reflected the relative size of MAH grafting amount on the polypropylene.Again according to semi-rational formula G=(K A (1790)/A (2723)+R) * 9.8% is tried to achieve the massfraction G of MAH in the graft polypropylene, the percentage of grafting of MAH just, K=0.469 wherein, R=-0.023, A represents peak area.
2. the stripping strength of composition
With reference to GB 2791-81
3. melt flow rate (MFR)
With reference to 1238,230 ℃ of ASTM D, load 2.16kg
Embodiment 1:
With the dicumyl peroxide initiator, with melt flow rate (MFR) be 2.5g/10min homo-polypropylene (Lanzhou Petrochemical Company F401) and MAH, vinylbenzene with 10: 1: 0.25 weight ratio (initiator is 0.125wt ‰) exist
React in the parallel dual-screw, the screw zones temperature of reaction (℃) be followed successively by 170,180,190,200,210,210,210,190,180,170; Reaction times: 6min.The percentage of grafting of MAH is 2% on the polypropylene after measured;
Exist according to following proportioning
Blending in the parallel dual-screw adds primary antioxidant 1010 and aid anti-oxidants 168 (being Jin Haiyabao production) during blending, its consumption accounts for 0.5 ‰ and 1 ‰ of composition total mass respectively.The screw zones temperature (℃) be followed successively by: 200,210,220,230,230,, 240,230,220, screw speed is 60 commentaries on classics/min.The product that obtains carries out The performance test results and sees Table 1.
Polypropylene-g-MAH 5
Polypropylene (melt flow rate (MFR) 0.4g/10min) 35 Yanshan Petrochemical C4220
LLDPE (melt flow rate (MFR) 1.0g/10min) 25 Lanzhou petrochemical industry 103AA
HDPE (melt flow rate (MFR) 4.5g/10min) 25 Daqing petrochemical 2100J
POE (melt flow rate (MFR) 16g/10min) 5 du pont companies
PS (melt flow rate (MFR) 7.0g/10min) 5 Yanshan Petrochemical 666D
Comparative Examples 1:
With the dicumyl peroxide initiator, with melt flow rate (MFR) be 2.5g/10min homo-polypropylene (Lanzhou Petrochemical Company production) and MAH with 10: 1 weight ratio (initiator is 0.125wt ‰) exist
React in the parallel dual-screw, the screw zones temperature of reaction (℃) be followed successively by 170,180,190,200,210,210,210,190,180,170; Reaction times: 6min.The percentage of grafting of grafting PP is 0.8% after measured;
Carry out twin screw blending reaction according to the condition identical with embodiment 1, the product that obtains carries out The performance test results and sees Table 1.
Comparative Examples 2:
With the dicumyl peroxide is initiator, is 28g/10min with MFR, density be 0.90 block polypropylene (Yanshan Petrochemical production) with MAH, vinylbenzene with 10: 1: 0.25 weight ratio (initiator is 0.125wt ‰) exist
React in the parallel dual-screw, the screw zones temperature of reaction (℃) be followed successively by 170,180,190,200,210,210,210,190,180,170; Reaction times: 6min, percentage of grafting are 4% grafting PP;
Exist according to following proportioning
Blending in the parallel dual-screw adds primary antioxidant 1010 and aid anti-oxidants 168 (being Jin Haiyabao production) during blending, its consumption accounts for 0.5 ‰ and 1 ‰ of composition total mass respectively.The screw zones temperature (℃) be followed successively by: 200,210,220,230,230,, 240,230,220, screw speed is 60 commentaries on classics/min.Product is carried out The performance test results see Table 1.
PP-g-MAH 20
PP (MFR 28g/10min, ρ 0.90, block PP) 68 Yanshan Petrochemical K7726
POE 10 du pont companies
PS (MFR 7.0g/10min) 2 Yanshan Petrochemical 666D
Embodiment 2:
With the dicumyl peroxide is initiator, with melt flow rate (MFR) be 28g/10min block polypropylene (Yanshan Petrochemical 7726) and MAH, vinylbenzene with 10: 1: 0.25 weight ratio (initiator is 0.125wt ‰) exist
React in the parallel dual-screw, the screw zones temperature of reaction (℃) be followed successively by 170,180,190,200,210,210,210,190,180,170; Reaction times: 6min, the relative percentage of grafting of MAH are 4% graft polypropylene;
Exist according to following proportioning
Blending in the parallel dual-screw adds primary antioxidant 1010 and aid anti-oxidants 168 (being Jin Haiyabao production) during blending, its consumption accounts for 0.5 ‰ and 1 ‰ of composition total mass respectively.The screw zones temperature (℃) be followed successively by: 200,210,220,230,230,, 240,230,220, screw speed is 60 commentaries on classics/min.Product is carried out The performance test results see Table 1.
Polypropylene-g-MAH 20
Polypropylene (melt flow rate (MFR) 28g/10min) 28 Yanshan Petrochemicals 7726
LLDPE (melt flow rate (MFR) 1.0g/10min) 20 Lanzhou petrochemical industry 103AA
HDPE (melt flow rate (MFR) 4.5g/10min) 20 Daqing petrochemical 2100J
POE 10 du pont companies
PS (melt flow rate (MFR) 7.0g/10min) 2 Yanshan Petrochemical 666D
Embodiment 3:
With melt flow rate (MFR) be 28g/10min block polypropylene (Yanshan Petrochemical 7726) and MAH, vinylbenzene with 10: 1: 0.25 weight ratio (initiator is 0.125wt ‰) in the there-necked flask of 2L with dimethylbenzene do solvent reaction temperature 100 (℃); Reaction times: 2h solution graft copolymerization, the relative percentage of grafting of MAH are 7% graft polypropylene;
Exist according to following proportioning
Blending in the parallel dual-screw adds primary antioxidant 1010 and aid anti-oxidants 168 (being Jin Haiyabao production) during blending, its consumption accounts for 0.5 ‰ and 1 ‰ of composition total mass respectively.The screw zones temperature (℃) be followed successively by: 200,210,220,230,230,, 240,230,220, screw speed is 60 commentaries on classics/min.Product is carried out The performance test results see Table 1.
Polypropylene-g-MAH 28
Polypropylene (melt flow rate (MFR) 2.5g/10min) 20 Lanzhou petrochemical industry F401
LLDPE (melt flow rate (MFR) 1.0g/10min) 25 Lanzhou petrochemical industry 103AA
HDPE (melt flow rate (MFR) 4.5g/10min) 15 Daqing petrochemical 2100J
POE 10 du pont companies
PS (melt flow rate (MFR) 7.0g/10min) 2 Yanshan Petrochemical 666D
Table 1
Claims (5)
1. a bonded polyolefine resin composition is absolutely in the composition quality, and the mobile speed of resin melt adopts 1238,230 ℃ of ASTM D, measures under the load 2.16kg standard, mainly consists of:
0.1～40% graft polypropylene melt flow rate (MFR): 1～40g/10min
20～48% melt polypropylene flow rate: 0.3～40g/10min
20～40% linear low density polyethylene melt flow rate (MFR): 0.8～10g/10min
10～30% high density polyethylene(HDPE) melt flow rate (MFR): 2～5g/10min
1～20% ethene and octene copolymer ethene and octene copolymerization in 1: 1,
Melt flow rate (MFR): 0.5～30g/10min
1～10% polystyrene
Graft polypropylene is to be first grafted monomer with unsaturated carboxylic acid, acid anhydrides or carboxylicesters, vinylbenzene is second grafted monomer, superoxide is an initiator, and the weight ratio of polypropylene and grafted monomer is obtaining by fusion-grafting or solution graft copolymerization for 10: 1～5: 1 times; Wherein, it is 10: 1～1: 1 that first and second monomer adds weight ratio, and the percentage of grafting of the unsaturated carboxylic acid on the polypropylene, acid anhydrides or carboxylicesters is 1%～10%.
2. polyolefine resin composition according to claim 1, it is characterized in that unsaturated carboxylic acid, acid anhydrides or carboxylicesters are selected from wherein a kind of of vinylformic acid, methacrylic acid, maleic acid, MALEIC ANHYDRIDE, 4-methyl-4-tetrahydrobenzene-1,2 dicarboxylic anhydride, methacrylic ester or vinylformic acid carboxylic propyl ester.
3. polyolefine resin composition according to claim 2 is characterized in that unsaturated acid anhydride is meant MALEIC ANHYDRIDE.
4. polyolefine resin composition according to claim 3 is characterized in that the polypropylene in the composition is homo-polypropylene, atactic copolymerized polypropene or block copolymerization polypropylene, and its melt flow rate (MFR) is 0.3～40g/10min.
5. polyolefine resin composition according to claim 1 is characterized in that the polypropylene that grafting is used is a block copolymerization polypropylene.
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| US8383246B2 (en) * | 2008-05-22 | 2013-02-26 | Exxonmobil Oil Corporation | Polypropylene-based shrink films |
| CN101798420B (en) * | 2010-01-26 | 2012-01-04 | 金发科技股份有限公司 | Easy-die-cutting polypropylene film and preparation method thereof |
| CN102070839B (en) * | 2011-01-10 | 2012-08-08 | 广东华盛塑料有限公司 | Modified plastic |
| 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 |
| CN102850857B (en) * | 2012-09-28 | 2014-12-03 | 四川仁智油田技术服务股份有限公司 | Steel pipeline anticorrosive material and preparation method of steel pipeline anticorrosive material |
| CN103739941B (en) * | 2013-12-05 | 2016-04-27 | 宁波康德新材料有限公司 | A kind of modified plastics |
| CN103740185B (en) * | 2014-01-14 | 2016-05-11 | 南京金陵塑胶化工有限公司 | A kind of atactic copolymerized polypropene coating material |
| TWI580718B (en) * | 2014-03-12 | 2017-05-01 | 財團法人工業技術研究院 | Polymer composition |
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| CN109971270A (en) * | 2017-12-28 | 2019-07-05 | 佛山市因诺维生物科技有限公司 | A kind of ceramic anticorrosive paint |
| CN115028916A (en) * | 2022-06-08 | 2022-09-09 | 广州丽盈塑料有限公司 | High-barrier light plastic for plastic packaging container and preparation method thereof |
| CN115260945B (en) * | 2022-08-22 | 2024-02-20 | 赣州能之光新材料有限公司 | Polypropylene adhesive resin and preparation method and application thereof |
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