CN102675707A - Quaternary phosphonium salt montmorillonoid enhanced polyolefin nanocomposite and preparation method thereof - Google Patents
Quaternary phosphonium salt montmorillonoid enhanced polyolefin nanocomposite and preparation method thereof Download PDFInfo
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- CN102675707A CN102675707A CN2012100110943A CN201210011094A CN102675707A CN 102675707 A CN102675707 A CN 102675707A CN 2012100110943 A CN2012100110943 A CN 2012100110943A CN 201210011094 A CN201210011094 A CN 201210011094A CN 102675707 A CN102675707 A CN 102675707A
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Abstract
The invention discloses a quaternary phosphonium salt montmorillonoid enhanced polyolefin nanocomposite and a preparation method thereof. The quaternary phosphonium salt montmorillonoid enhanced polyolefin nanocomposite is prepared from the following raw materials in parts by weight: 80-95 parts of polyolefin, 5-10 parts of compatilizer and 0.5-5 parts of quaternary phosphonium salt montmorillonoid, wherein the quaternary phosphonium salt montmorillonoid is prepared from 100 parts of montmorillonoid and 10 parts of quaternary phosphonium salt of which the general formula is PR3YX, wherein P is a phosphorus atom, R is C1-4 linear alkyl or phenyl, Y is the linear alkyl of C12, C14, C16 and C18, and X is a chlorine atom or a bromine atom. The polyolefin nanocomposite disclosed by the invention is characterized in that filler montmorillonoid adopts the quaternary phosphonium salt montmorillonoid, the montmorillonoid is modified by the quaternary phosphonium salt, the interlayer spacing of the montmorillonoid is improved, and the montmorillonoid is unlikely to decompose and change color at high temperature and has high high-temperature stability. When the quaternary phosphonium salt montmorillonoid of the quaternary phosphonium salt montmorillonoid enhanced polyolefin nanocomposite is used as a filler which is fused and blended with polyolefin, the color of the polyolefin nanocomposite does not darken.
Description
Technical field
The present invention relates to a kind of olefin polymerization nanometer composite material, particularly a kind of quaternary alkylphosphonium salt polynite enhanced olefin polymerization nanometer composite material belongs to the inorganic macromolecule material technical field.
Background technology
Nano composite polymer-montmorillonoid material is one type of matrix material of being made up of organic polymer matrix and montmorillonite-based nano particle, generally comprises polyolefine, compatilizer and polynite.Because nano effect, mechanical property, flame retardant resistance, barrier properties for gases, dimensional stability and the heat-drawn wire of material all can be significantly improved behind the Nano filling that adds very small amount.Polynite is a kind of layered silicate, because its strong wetting ability is very difficult compatible with most polymerization, thereby must carry out chemical modification to it.The general method of modifying that adopts is to carry out IX with it with organic cation, makes the surface of polynite not only have hydrophobic nature, and makes interlamellar spacing become big.In the presence of compatilizer, can make organo montmorillonite further peel off into nanometer lamella two with an amount of organo montmorillonite melt blending polyolefine and be dispersed in macromolecule matrix and form a kind of high molecule nano composite material.At present, to imvite modified mostly be to adopt quaternary ammonium salt-modifiedly because quaternary ammonium salt produces darkening of polyolefine material that decomposition makes modification in the high-temperature fusion blend, thereby limited the range of application of this type material, especially as wrapping material.
Summary of the invention
The purpose of this invention is to provide a kind of quaternary alkylphosphonium salt polynite enhanced olefin polymerization nanometer composite material, the problem of avoiding olefin polymerization nanometer composite material to darken.
In order to realize above purpose; The technical scheme that nanometer composite polypropylene material of the present invention adopted is: a kind of quaternary alkylphosphonium salt polynite enhanced olefin polymerization nanometer composite material is to be processed by the raw material of following weight part: polyolefine 80-95 part, compatilizer 5-10 part 、 quaternary alkylphosphonium salt polynite 0.5-5 part; The quaternary alkylphosphonium salt polynite be by
The sodium basePolynite and general formula are PR
3The IX of YX De quaternary alkylphosphonium salt is processed, and P is a phosphorus atom in the general formula, and R is C
1-4Straight chained alkyl or phenyl, Y is C
12-18Straight chained alkyl, X is chlorine atom or bromine atoms.
Said quaternary alkylphosphonium salt and polynite reaction can excessively be used, and excessive degree can surpass based on the consideration of cost
The sodium baseThe ion-exchange equivalent 5-20% of polynite.Said general formula PR
3Y is that Y is C among the YX
12, C
14, C
16Or C
18Straight chained alkyl.Said polyolefine is Vilaterm, Vestolen PP 7052 or PS.Said compatilizer is the graft copolymer of corresponding polyolefine and maleic anhydride.The molecular weight of said graft copolymer is 20000-100000, and percentage of grafting is about 1%.The loading capacity of said sodium-based montmorillonite is 90-120mmol/100g.
Said quaternary alkylphosphonium salt be positive dodecyl trimethylammonium phosphonium bromide, positive dodecyl triethyl phosphonium bromide, positive dodecyl tripropyl phosphonium bromide, positive dodecyl tributyl phosphonium bromide, positive dodecyl three phenyl phosphonium bromides, positive tetradecyl trimethylammonium phosphonium bromide, positive tetradecyl triethyl phosphonium bromide, positive tetradecyl tripropyl phosphonium bromide, positive tetradecyl tributyl phosphonium bromide, positive tetradecyl three phenyl phosphonium bromides, positive hexadecyl triethyl phosphonium bromide, positive hexadecyl tripropyl phosphonium bromide, positive hexadecyl tributyl phosphonium bromide, positive hexadecyl three phenyl phosphonium bromides,, positive octadecyl trimethylammonium phosphonium bromide, positive octadecyl triethyl phosphonium bromide, positive octadecyl tripropyl phosphonium bromide, positive octadecyl tributyl phosphonium bromide, positive octadecyl three phenyl phosphonium bromides, or the muriate of above-mentioned respective compound.
The preferred dodecyl tributyl of quaternary alkylphosphonium salt of the present invention phosphonium bromide, dodecyl three phenyl phosphonium bromides or Octadecane base three phenyl phosphonium bromides.
Olefin polymerization nanometer composite material of the present invention; Wherein the quaternary alkylphosphonium salt polynite is adopted in the weighting agent polynite; Adopt quaternary alkylphosphonium salt that modification is carried out in polynite, improved the interlamellar spacing of polynite, at high temperature be difficult for decomposing variable color; High-temperature stability is high, and quaternary alkylphosphonium salt polynite of the present invention can not make olefin polymerization nanometer composite material darken during as weighting agent and the blend of polyolefine high-temperature fusion.Wherein compatilizer can adopt conventional compatilizer; Promptly reach evenly compatible getting final product of polyolefine and quaternary alkylphosphonium salt polynite; Compatilizer of the present invention can be preferably the graft copolymer of corresponding polyolefine and maleic anhydride, and the compatilizer that promptly can select for use to the preferred polyolefine of the present invention is grafted polyvinyl-maleic anhydride copolymer, Vestolen PP 7052-maleic anhydride graft copolymer, polystyrene-maleic anhydride grafted multipolymer.
The preparation of following method is adopted in quaternary alkylphosphonium salt polynite of the present invention: polynite is joined in 80 ℃ the deionized water; Under vigorous stirring, add quaternary alkylphosphonium salt reaction 24 hours; To not having cl ions or not having bromide anion, lyophilize promptly gets the quaternary alkylphosphonium salt polynite with deionized water wash in reaction end back.
Quaternary alkylphosphonium salt polynite of the present invention in addition is as the weighting agent of olefin polymerization nanometer composite material; Can improve the physical and mechanical property of matrix material; Wherein tensile strength improved more than 30% than originally, and resistance to impact shock improved more than 40% than originally, and the xanthochromia index is less than 3.
Nanometer composite polypropylene material of the present invention adopts following method preparation: with polyolefine, the polynite of compatilizer ， quaternary alkylphosphonium salt is processed in 130～185 ℃ of mixing extruding.
Embodiment
Below technical scheme of the present invention is done concrete description, but and non-limiting technical scheme of the present invention.
Embodiment 1
The olefin polymerization nanometer composite material of present embodiment is to be processed by the raw material of following weight part: Vilaterm 850g, compatilizer 100g 、 quaternary alkylphosphonium salt polynite 50g; The quaternary alkylphosphonium salt polynite is by 10 parts of 100 parts of polynites and dodecyl trimethyl phosphonium bromides, i.e. general formula PR
3P is a phosphorus atom among the YX, and R is a methyl, and Y is a n-nonyl, and X is a bromine atoms.Compatilizer adopts grafted polyvinyl-maleic anhydride copolymer.Vilaterm can specifically be selected high-pressure polyethylene.
The preparation of following method is adopted in the quaternary alkylphosphonium salt polynite: with the 100g loading capacity is that the sodium-based montmorillonite of 110mmol/100g joins in 1000ml, 80 ℃ the deionized water; The n-nonyl trimethylammonium phosphonium bromide that under vigorous stirring, adds 10g; Reacted 24 hours; To there not being bromide anion, lyophilize promptly obtains the polynite of title product n-nonyl trimethylammonium phosphonium bromide with deionized water wash in reaction end back.
Olefin polymerization nanometer composite material adopts following method preparation: Vilaterm, compatilizer He quaternary alkylphosphonium salt polynite are processed in 130 ℃ of mixing extruding.
Embodiment 2
The olefin polymerization nanometer composite material of present embodiment is to be processed by the raw material of following weight part: Vestolen PP 7052 800g, compatilizer 75g 、 quaternary alkylphosphonium salt polynite 30g; The quaternary alkylphosphonium salt polynite is by 10 parts of 100 parts of polynites and dodecyl tributyl phosphonium bromides, i.e. general formula PR
3P is a phosphorus atom among the YX, and R is a butyl, and Y is a dodecyl, and X is a bromine atoms.Compatilizer adopts Vestolen PP 7052-maleic anhydride graft copolymer.Vestolen PP 7052 can specifically be selected HOPP.
The preparation of following method is adopted in the quaternary alkylphosphonium salt polynite: with the 100g loading capacity is that the sodium-based montmorillonite of 90mmol/100g joins in 1000ml, 80 ℃ the deionized water; The dodecyl tributyl phosphonium bromide that under vigorous stirring, adds 10g; Reacted 24 hours; To there not being bromide anion, lyophilize promptly obtains the polynite of title product dodecyl tributyl phosphonium bromide with deionized water wash in reaction end back.
Olefin polymerization nanometer composite material adopts following method preparation: Vestolen PP 7052, compatilizer He quaternary alkylphosphonium salt polynite are processed in 145 ℃ of mixing extruding.
Embodiment 3
The olefin polymerization nanometer composite material of present embodiment is to be processed by the raw material of following weight part: PS 900g, compatilizer 70g 、 quaternary alkylphosphonium salt polynite 20g; The quaternary alkylphosphonium salt polynite is by 10 parts of 100 parts of polynites and Octadecane base three phenyl phosphonium bromides, i.e. general formula PR
3P is a phosphorus atom among the YX, and R is a phenyl, and Y is the Octadecane base, and X is a bromine atoms.Compatilizer adopts polystyrene-maleic anhydride grafted multipolymer.
The preparation of following method is adopted in the quaternary alkylphosphonium salt polynite: with the 100g loading capacity is that the sodium-based montmorillonite of 100mmol/100g joins in 1000ml, 80 ℃ the deionized water; The Octadecane base three phenyl phosphonium bromides that under vigorous stirring, add 10g; Reacted 24 hours; To there not being bromide anion, lyophilize promptly obtains the three phenyl phosphonium bromide polynites of title product Octadecane base with deionized water wash in reaction end back.
Olefin polymerization nanometer composite material adopts following method preparation: PS, compatilizer He quaternary alkylphosphonium salt polynite are processed in 160 ℃ of mixing extruding.
Embodiment 4
The olefin polymerization nanometer composite material of present embodiment is to be processed by the raw material of following weight part: PS 950g, compatilizer 50g 、 quaternary alkylphosphonium salt polynite 5g; The quaternary alkylphosphonium salt polynite is by 10 parts of 100 parts of polynites and n-hexadecyl San Yi Ji phosphonium chlorides, i.e. general formula PR
3P is a phosphorus atom among the YX, and R is an ethyl, and Y is a n-hexadecyl, and X is the chlorine atom.Compatilizer adopts polystyrene-maleic anhydride grafted multipolymer.
The preparation of following method is adopted in the quaternary alkylphosphonium salt polynite: with the 100g loading capacity is that the sodium-based montmorillonite of 110mmol/100g joins in 1000ml, 80 ℃ the deionized water; The n-hexadecyl San Yi Ji phosphonium chloride that under vigorous stirring, adds 10g; Reacted 24 hours; To there not being bromide anion, lyophilize promptly obtains the three second base phosphonium chloride polynites of title product n-hexadecyl with deionized water wash in reaction end back.
Olefin polymerization nanometer composite material adopts following method preparation: PS, compatilizer He quaternary alkylphosphonium salt polynite are processed in 185 ℃ of mixing extruding.
Embodiment 5
The olefin polymerization nanometer composite material of present embodiment is to be processed by the raw material of following weight part: Vilaterm 850g, compatilizer 100g 、 quaternary alkylphosphonium salt polynite 50g; The quaternary alkylphosphonium salt polynite is by 10 parts of 100 parts of polynites and dodecyl tri-phenyl-phosphorus bromides, i.e. general formula PR
3P is a phosphorus atom among the YX, and R is an ethyl, and Y is a n-hexadecyl, and X is the chlorine atom.Compatilizer adopts grafted polyvinyl-maleic anhydride copolymer.Vilaterm can specifically be selected high-pressure polyethylene.
The preparation of following method is adopted in the quaternary alkylphosphonium salt polynite: with the 100g loading capacity is that the sodium-based montmorillonite of 120mmol/100g joins in 1000ml, 80 ℃ the deionized water; The dodecyl tri-phenyl-phosphorus bromide that under vigorous stirring, adds 10g; Reacted 24 hours; To there not being bromide anion, lyophilize promptly obtains the polynite of title product dodecyl tri-phenyl-phosphorus bromide with deionized water wash in reaction end back.
Olefin polymerization nanometer composite material adopts following method preparation: Vilaterm, compatilizer He quaternary alkylphosphonium salt polynite are processed in 185 ℃ of mixing extruding.
Embodiment 6
The olefin polymerization nanometer composite material of present embodiment is to be processed by the raw material of following weight part: Vilaterm 900g, compatilizer 80g 、 quaternary alkylphosphonium salt polynite 20g; The quaternary alkylphosphonium salt polynite is by 10 parts of 100 parts of polynites and dodecyl tributyl phosphonium bromides.Compatilizer adopts grafted polyvinyl-maleic anhydride copolymer.Vilaterm can specifically be selected high-pressure polyethylene.
The preparation method of quaternary alkylphosphonium salt polynite and olefin polymerization nanometer composite material is not described in detail in this with embodiment 2.
Embodiment 7
The olefin polymerization nanometer composite material of present embodiment is to be processed by the raw material of following weight part: PS 850g, compatilizer 100g 、 quaternary alkylphosphonium salt polynite 50g; The quaternary alkylphosphonium salt polynite is by 10 parts of 100 parts of polynites and dodecyl three phenyl phosphonium bromides.Compatilizer adopts polystyrene-maleic anhydride grafted multipolymer.PS can specifically be selected high impact polyethylene.
The preparation method of quaternary alkylphosphonium salt polynite and olefin polymerization nanometer composite material is not described in detail in this with embodiment 5.
Comparative Examples
The olefin polymerization nanometer composite material of present embodiment is to be processed by the raw material of following weight part: Vestolen PP 7052 800g, compatilizer 75g, quaternary ammonium salt montmorillonite 30g; Quaternary ammonium salt montmorillonite is by 10 parts of 100 parts of polynites and dodecyl tributyl brometo de amonios, i.e. general formula PR
3P is a nitrogen-atoms among the YX, and R is a butyl, and Y is a dodecyl, and X is a bromine atoms.Compatilizer adopts Vestolen PP 7052-maleic anhydride graft copolymer.Vestolen PP 7052 can specifically be selected HOPP.
Quaternary ammonium salt montmorillonite adopts the preparation of following method: with the 100g loading capacity is that the sodium-based montmorillonite of 90mmol/100g joins in 1000ml, 80 ℃ the deionized water; The dodecyl tributyl brometo de amonio that under vigorous stirring, adds 10g; Reacted 24 hours; To there not being bromide anion, lyophilize promptly obtains the polynite of title product dodecyl tributyl brometo de amonio with deionized water wash in reaction end back.
Olefin polymerization nanometer composite material adopts following method preparation: Vestolen PP 7052, compatilizer and quaternary ammonium salt montmorillonite are processed in 145 ℃ of mixing extruding.
The olefin polymerization nanometer composite material of embodiment 1-7 and Comparative Examples is carried out performance measurement; Compare with the simple polypropylene material that under identical preparation condition, does not add polynite; Concrete mensuration and comparing result result are as shown in table 1, and wherein tensile strength and shock strength are the contrast percent value.
Table 1 olefin polymerization nanometer composite material performance table
Claims (9)
1. a quaternary alkylphosphonium salt polynite enhanced olefin polymerization nanometer composite material is characterized in that: be to be processed by the raw material of following weight part: polyolefine 80-95 part, compatilizer 5-10 part, quaternary alkylphosphonium salt polynite 0.5-5 part; The quaternary alkylphosphonium salt polynite is to be PR by sodium-based montmorillonite and general formula
3The IX of YX De quaternary alkylphosphonium salt is processed, and P is a phosphorus atom in the general formula, and R is C
1-4Straight chained alkyl or phenyl, Y is C
12-18Straight chained alkyl, X is chlorine atom or bromine atoms.
2. olefin polymerization nanometer composite material according to claim 1 is characterized in that: said quaternary alkylphosphonium salt surpasses
The sodium baseThe ion-exchange equivalent 5-20% of polynite.
3. olefin polymerization nanometer composite material according to claim 1 is characterized in that: said general formula PR
3Y is that Y is C among the YX
12, C
14, C
16Or C
18Straight chained alkyl.
4. olefin polymerization nanometer composite material according to claim 1 is characterized in that: said polyolefine is Vilaterm, Vestolen PP 7052 or PS.
5. olefin polymerization nanometer composite material according to claim 1 is characterized in that: said compatilizer is the graft copolymer of corresponding polyolefine and maleic anhydride.
6. olefin polymerization nanometer composite material according to claim 5 is characterized in that: the molecular weight of said graft copolymer is 20000-100000, and percentage of grafting is about 1%.
7. olefin polymerization nanometer composite material according to claim 1 is characterized in that: the loading capacity of said sodium-based montmorillonite is 90-120mmol/100g.
8. olefin polymerization nanometer composite material according to claim 1; It is characterized in that: said quaternary alkylphosphonium salt be positive dodecyl trimethylammonium phosphonium bromide, positive dodecyl triethyl phosphonium bromide, positive dodecyl tripropyl phosphonium bromide, positive dodecyl tributyl phosphonium bromide, positive dodecyl three phenyl phosphonium bromides, positive tetradecyl trimethylammonium phosphonium bromide, positive tetradecyl triethyl phosphonium bromide, positive tetradecyl tripropyl phosphonium bromide, positive tetradecyl tributyl phosphonium bromide, positive tetradecyl three phenyl phosphonium bromides, positive hexadecyl triethyl phosphonium bromide, positive hexadecyl tripropyl phosphonium bromide, positive hexadecyl tributyl phosphonium bromide, positive hexadecyl three phenyl phosphonium bromides,, positive octadecyl trimethylammonium phosphonium bromide, positive octadecyl triethyl phosphonium bromide, positive octadecyl tripropyl phosphonium bromide, positive octadecyl tributyl phosphonium bromide, positive octadecyl three phenyl phosphonium bromides, or the muriate of above-mentioned respective compound.
9. preparation method of olefin polymerization nanometer composite material according to claim 1 is characterized in that: with polyolefine, and compatilizer, the quaternary alkylphosphonium salt polynite is processed in 130～185 ℃ of mixing extruding.
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| CN104497563A (en) * | 2014-12-25 | 2015-04-08 | 贵州师范大学 | Hindered phenol quaternary phosphine salt modified montmorillonoid antioxidant-containing polyamide and preparation method thereof |
| CN105670079A (en) * | 2016-02-25 | 2016-06-15 | 联塑科技发展(贵阳)有限公司 | HDPE pipe material and preparing method thereof |
| CN107418177A (en) * | 2017-05-24 | 2017-12-01 | 武汉理工大学 | A kind of high-toughness halogen-free flame enhancing PC/ASA alloys and preparation method thereof |
| CN116948547A (en) * | 2023-06-15 | 2023-10-27 | 宁波勤邦新材料科技股份有限公司 | Novel white reinforced photovoltaic backboard base film, preparation method and application thereof |
| CN118165419A (en) * | 2024-04-11 | 2024-06-11 | 江门江东华普塑料容器有限公司 | Polymer composite material for plastic container and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104497563A (en) * | 2014-12-25 | 2015-04-08 | 贵州师范大学 | Hindered phenol quaternary phosphine salt modified montmorillonoid antioxidant-containing polyamide and preparation method thereof |
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| CN107418177A (en) * | 2017-05-24 | 2017-12-01 | 武汉理工大学 | A kind of high-toughness halogen-free flame enhancing PC/ASA alloys and preparation method thereof |
| CN116948547A (en) * | 2023-06-15 | 2023-10-27 | 宁波勤邦新材料科技股份有限公司 | Novel white reinforced photovoltaic backboard base film, preparation method and application thereof |
| CN118165419A (en) * | 2024-04-11 | 2024-06-11 | 江门江东华普塑料容器有限公司 | Polymer composite material for plastic container and preparation method thereof |
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Application publication date: 20120919 |