CN101717528B - Starch acetate-polydioxanone graft copolymer/inorganic particulate nano composite material and preparation method thereof - Google Patents
Starch acetate-polydioxanone graft copolymer/inorganic particulate nano composite material and preparation method thereof Download PDFInfo
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- CN101717528B CN101717528B CN2009102161793A CN200910216179A CN101717528B CN 101717528 B CN101717528 B CN 101717528B CN 2009102161793 A CN2009102161793 A CN 2009102161793A CN 200910216179 A CN200910216179 A CN 200910216179A CN 101717528 B CN101717528 B CN 101717528B
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Abstract
The invention discloses a starch acetate-polydioxanone graft copolymer/inorganic particulate nano composite material which is prepared from a starch acetate-polydioxanone graft copolymer base material and nanometer inorganic particulates, wherein the weight ratio of starch acetate to graft copolymers is 1 to 40:100, and the weight ratio of the nanometer inorganic particulates to the starch acetate-polydioxanone graft copolymers is 0.5 to 10:100. The invention also discloses a preparation method of the starch acetate-polydioxanone graft copolymer/inorganic particulate nano composite material. Because the starch acetate and the nanometer inorganic particulates are introduced into the copolymer, the production cost is reduced, the thermal property, the mechanical property and the biodegradation rate of the polydioxanone are increased, and the preparation method has lower requirements for a monomer and a reaction condition and has simple operation, high production efficiency and no environment pollution.
Description
Technical field
The invention belongs to polymkeric substance and inorganic nano-filler matrix material and preparing technical field thereof, be specifically related to a kind of starch acetate-PPDO graft copolymer/inorganic particulate nano composite material and preparation method thereof.
Background technology
Most polymers material that uses at present such as Vilaterm, Vestolen PP 7052, PS, SE etc., all very stable at occurring in nature, be difficult to degraded.The use of these materials is especially used in the agricultural of one-time consumption and packing business in a large number, has caused serious white pollution.In agricultural, packing business and medical industry, many plastics do not need oversize work-ing life, and therefore, researcher both domestic and external had all both had the plastics premium properties, the plastics of new generation that can degrade again simultaneously being devoted to exploitation.
PPDO (PPDO) is a kind of of aliphatic polyester, because it has excellent biocompatibility and biological degradability, is successfully applied to already and makes surgical sutures, hone lamella and tissue renovation material, like surgery devices such as screw, hook, sheet and pincers.PPDO is except have excellent biocompatibility and the biological degradability, it also should obtain confirmation (Nishida, H. at present at the biological degradability of occurring in nature in vivo; Konno, M.; Ikeda, A.; Tokiwa, Y.Polym.Degrad.Stab.2000,68,205-217).But to but there be bigger obstacle in it as general purpose material: the one, the monomer whose price is higher, and production cost is comparatively expensive; The 2nd, synthesize PPDO and usually monomer purity, catalyst activity and polymeric reaction condition required very highly with practical value, and polymerization time is long, and the polymerisate crystallization velocity is slow, and melt strength is low, the forming process difficulty.
The inventor was the preparation method that starch acetate-PPDO graft copolymer is provided among the CN 101337994 at number of patent application once.Because this graft copolymerization is in homogeneous system, to carry out, so the graft copolymer of its preparation not only has higher productive rate and grafting efficiency, and it is simple also to have building-up process, and production cost is low, characteristics such as fully biodegradable.But the melt strength of this graft copolymer is lower, is unfavorable for machine-shaping, has limited its widespread use as general-purpose plastics.
Summary of the invention
The objective of the invention is problem, at first provide a kind of and carry out starch acetate-PPDO graft copolymer/inorganic particulate nano composite material that modification obtains through adding inorganic nano-particle to the prior art existence.
Another object of the present invention provides a kind of method for preparing above-mentioned starch acetate-PPDO graft copolymer/inorganic particulate nano composite material.
Starch acetate provided by the invention-PPDO graft copolymer/inorganic particulate nano composite material; This matrix material is to be made up of starch acetate-PPDO graft copolymer body material and nano grade inorganic particle; Wherein the weight ratio of starch acetate and graft copolymer is 1～40: 100, and the weight ratio of nano grade inorganic particle and starch acetate-PPDO graft copolymer is 0.5～10: 100.
Nano grade inorganic particle in this matrix material is that any in the stone taken off in polynite, layered double-hydroxide, sepiolite or tired.
The substitution value of the starch acetate in this matrix material is 1.5～2.9, and molecular weight is 15000～100000.
The method of the above-mentioned starch acetate of preparation provided by the invention-PPDO graft copolymer/inorganic particulate nano composite material is that the starch acetate of 1～40 weight part and 60～99 weight parts are counted 100: 0.5～10 parts nano grade inorganic particle to dioxy pimelinketone monomer with the weight of starch acetate-PPDO graft copolymer; Under the nitrogen atmosphere protection; Ultra-sonic dispersion 1～2 hour; Be warming up to 60～120 ℃ then, add and the catalyzer that to the monomeric mol ratio of dioxy pimelinketone is 1: 0.001～0.004, react and got final product in 6～20 hours; Or directly with starch acetate-PPDO graft copolymer and nano grade inorganic particle; Ratio by weight 100: 0.5～10, melt blending again behind premix, the melt blending temperature is 85～140 ℃.
The used nano grade inorganic particle of aforesaid method is that any in the stone taken off in polynite, layered double-hydroxide, sepiolite or tired; And the polynite of selecting for use; Layered double-hydroxide (LDH), sepiolite, the tired stone that takes off can be without the processing that organises, also can be through the processing that organises.Polynite, layered double-hydroxide, sepiolite, the tired stone that takes off are organised that to handle be known technology; Concrete grammar is seen CN 1300231C, and organic modification agent commonly used has OTAC, palmityl trimethyl ammonium chloride, hexadecyldimethyl benzyl ammonium hydroxyethyl brometo de amonio, hexadecyl methyl dihydroxy ethyl brometo de amonio etc.
The substitution value of the starch acetate that aforesaid method is used is 1.5～2.9, and molecular weight is 15000～100000.
The used catalyzer of aforesaid method is aluminum alkyls or alkoxy compound.
The present invention has the following advantages:
1, because the present invention has added a spot of inorganic nano-particle in starch acetate-PPDO graftomer; Thereby not only improved the melt strength of this graftomer; Also further improved the use properties of material; Especially the mechanical property of material makes starch acetate-PPDO graft copolymer/inorganic particulate nano composite material be expected to become a kind of new both have plastics premium properties, the plastics of new generation that can degrade again simultaneously.
2, because the starch acetate-PPDO graft copolymer/inorganic particulate nano composite material of the present invention's preparation has been introduced greatly cheap starch acetate and the nano grade inorganic particle of comparison dioxy pimelinketone price; Thereby on the one hand the production cost of the nano composite material of acquisition is reduced greatly; Also improved the biodegradation rate of PPDO on the other hand; It both can be degraded in physical environment fully, be suitable for compost degraded requirement again.
3, since the starch acetate-PPDO graft copolymer/inorganic particulate nano composite material of the present invention preparation through in body material, introducing the starch acetate segment and adopting ultransonic mode to improve the dispersion situation of inorganic nano-particle in polymkeric substance; Strengthened the interfacial interaction of inorganic nano-particle and starch acetate-PPDO graft copolymer, avoided disperseing the inhomogeneous influence that material property is brought because of inorganic nano-particle.
4, the nano composite material of the inventive method preparation is lower, simple to operate to monomer and reaction conditions requirement, and production efficiency is high, environmentally safe.
Embodiment
Provide embodiment below so that the present invention is described further; It is important to point out that following examples can not be interpreted as the restriction to protection domain of the present invention; The person skilled in the art in this field is according to the content of the invention described above, and the improvement and the adjustment of some non-intrinsically safe property that the present invention is made still belong to protection scope of the present invention.
Embodiment 1
With substitution value is 2.3; Molecular weight is 30000 5 parts of starch acetates, new distillatory to 5 parts of 95 parts of dioxy pimelinketone monomers and polynites; Add successively in the reaction flask, ultra-sonic dispersion is 2 hours under the nitrogen atmosphere protection, and starch acetate is dissolved in the dioxy pimelinketone monomer fully; Make the polynite swelling simultaneously; Be warmed up to 80 ℃ then, add again and the triethylaluminium catalyst that to dioxy pimelinketone mol ratio is 0.002, react and promptly obtained starch acetate-PPDO graft copolymer/inorganic particulate nano composite material in 6 hours.
Embodiment 2
With substitution value is 2.3; Molecular weight is 50000 15 parts of starch acetates, new distillatory to 7 parts of 85 parts of dioxy pimelinketone monomers and polynites; Add successively in the reaction flask, ultra-sonic dispersion is 2 hours under the nitrogen atmosphere protection, and starch acetate is dissolved in the dioxy pimelinketone monomer fully; Make the polynite swelling simultaneously; Be warmed up to 120 ℃ then, add again and the aluminum isopropylate catalyzer that to dioxy pimelinketone mol ratio is 0.004, react and promptly obtained starch acetate-PPDO graft copolymer/inorganic particulate nano composite material in 12 hours.
Embodiment 3
With substitution value is 2.9; Molecular weight is 50000 40 parts of starch acetates, new distillatory to 0.5 part of 60 parts of dioxy pimelinketone monomers and polynite; Add successively in the reaction flask, ultra-sonic dispersion is 1 hour under the nitrogen atmosphere protection, and starch acetate is dissolved in the dioxy pimelinketone monomer fully; Make the polynite swelling simultaneously; Be warmed up to 90 ℃ then, add again and the triethylaluminium catalyst that to dioxy pimelinketone mol ratio is 0.004, react and promptly obtained starch acetate-PPDO graft copolymer/inorganic particulate nano composite material in 12 hours.
Embodiment 4
With substitution value is 1.6; Molecular weight is 15000 1 part of starch acetate, new distillatory to 5 parts of 95 parts of dioxy pimelinketone monomers and LDH; Add successively in the reaction flask, ultra-sonic dispersion is 2 hours under the nitrogen atmosphere protection, and starch acetate is dissolved in the dioxy pimelinketone monomer fully; Make the LDH swelling simultaneously; Be warmed up to 90 ℃ then, add again and the stannous octoate catalyst that to dioxy pimelinketone mol ratio is 0.001, react and promptly obtained starch acetate-PPDO graft copolymer/inorganic particulate nano composite material in 20 hours.
Embodiment 5
With substitution value is 2.7; Molecular weight is 70000 20 parts of starch acetates, new distillatory to 3 parts of 80 parts of dioxy pimelinketone monomers and LDH; Join successively in the reaction flask, ultra-sonic dispersion is 1 hour under the nitrogen atmosphere protection, and starch acetate is dissolved in the dioxy pimelinketone monomer fully; Make the LDH swelling simultaneously; Be warmed up to 60 ℃ then, add again and the triethylaluminium catalyst that to dioxy pimelinketone mol ratio is 0.002, react and promptly obtained starch acetate-PPDO graft copolymer/inorganic particulate nano composite material in 12 hours.
Embodiment 6
With substitution value is 2.0; Molecular weight is that 30000 5 parts of starch acetates, new distillatory are to 95 parts of dioxy pimelinketone monomers and tired 1 part in the stone that takes off; Join successively in the reaction flask, ultra-sonic dispersion is 1 hour under the nitrogen atmosphere protection, and starch acetate is dissolved in the dioxy pimelinketone monomer fully; Make the tired stone swelling of taking off simultaneously; Be warmed up to 60 ℃ then, add again and the butyl(tetra)titanate catalyzer that to dioxy pimelinketone mol ratio is 0.004, react and promptly obtained starch acetate-PPDO graft copolymer/inorganic particulate nano composite material in 12 hours.
Embodiment 7
With substitution value is 2.3; Molecular weight is 100000 10 parts of starch acetates, new distillatory to 5 parts of 90 parts of dioxy pimelinketone monomers and sepiolites; Join successively in the reaction flask, ultra-sonic dispersion is 2 hours under the nitrogen atmosphere protection, and starch acetate is dissolved in the dioxy pimelinketone monomer fully; Make the sepiolite swelling simultaneously; Be warmed up to 80 ℃ then, add again and the triethylaluminium catalyst that to dioxy pimelinketone mol ratio is 0.002, react and promptly obtained starch acetate-PPDO graft copolymer/inorganic particulate nano composite material in 10 hours.
Embodiment 8
With substitution value is 1.5; Molecular weight is 30000 15 parts of starch acetates, new distillatory to 10 parts of 85 parts of dioxy pimelinketone monomers and LDH; Join successively in the reaction flask, ultra-sonic dispersion is 2 hours under the nitrogen atmosphere protection, and starch acetate is dissolved in the dioxy pimelinketone monomer fully; Make the LDH swelling simultaneously; Be warmed up to 120 ℃ then, add again and the stannous octoate catalyst that to dioxy pimelinketone mol ratio is 0.003, react and promptly obtained starch acetate-PPDO graft copolymer/inorganic particulate nano composite material in 18 hours.
Embodiment 9
With substitution value is 1.6; Molecular weight is 30000 3 parts of starch acetates, new distillatory to 7 parts of 95 parts of dioxy pimelinketone monomers and sepiolites; Join successively in the reaction flask, ultra-sonic dispersion is 1.5 hours under the nitrogen atmosphere protection, and starch acetate is dissolved in the dioxy pimelinketone monomer fully; Make the sepiolite swelling simultaneously; Be warmed up to 60 ℃ then, add again and the aluminum isopropylate catalyzer that to dioxy pimelinketone mol ratio is 0.0015, react and promptly obtained starch acetate-PPDO graft copolymer/inorganic particulate nano composite material in 15 hours.
Embodiment 10
With substitution value is 2.3; Molecular weight is that 50000 30 parts of starch acetates, new distillatory are to 70 parts of dioxy pimelinketone monomers and tired 3 parts in the stone that takes off; Join successively in the reaction flask, ultra-sonic dispersion is 2 hours under the nitrogen atmosphere protection, and starch acetate is dissolved in the dioxy pimelinketone monomer fully; Make the tired stone swelling of taking off simultaneously; Be warmed up to 90 ℃ then, add again and the trimethylaluminium catalyzer that to dioxy pimelinketone mol ratio is 0.004, react and promptly obtained starch acetate-PPDO graft copolymer/inorganic particulate nano composite material in 10 hours.
Embodiment 11
The synthetic of starch acetate-PPDO graft copolymer is that the method that 200410081645.9 patent application specification is put down in writing prepares according to application number.
With the 100g intrinsic viscosity is starch acetate-PPDO graft copolymer of 1.8dL/g, and wherein the content of starch acetate is 5%, and substitution value is 2.3; Molecular weight is 15000, at first in impeller, mixes with 5g polynite one, in twin screw extruder, presses 90 ℃ of feeding sections then; 120 ℃ of mixing sections; 125 ℃ of fluxing zones, 120 ℃ of heads, screw speed are melt blending under the condition of 9rpm; Extruding pelletization promptly obtains starch acetate-PPDO graft copolymer/inorganic particulate nano composite material.
Embodiment 12
Starch acetate-PPDO graft copolymer synthetic the same.
With the 100g intrinsic viscosity is starch acetate-PPDO graft copolymer of 1.7dL/g, and wherein the content of starch acetate is 40%, and substitution value is 2.9; Molecular weight is 30000, with 10gLDH one at first in impeller blend even, in twin screw extruder, press 85 ℃ of feeding sections then; 115 ℃ of mixing sections; 120 ℃ of fluxing zones, 115 ℃ of heads, screw speed are melt blending under the condition of 9rpm; Extruding pelletization promptly obtains starch acetate-PPDO graft copolymer/inorganic particulate nano composite material.
Embodiment 13
Starch acetate-PPDO graft copolymer synthetic the same.
With the 100g intrinsic viscosity is starch acetate-PPDO graft copolymer of 2.0dL/g, and wherein the content of starch acetate is 20%, and substitution value is 2.7; Molecular weight is 30000, with 3g LDH one at first in impeller blend even, in twin screw extruder, press 90 ℃ of feeding sections then; 120 ℃ of mixing sections; 125 ℃ of fluxing zones, 120 ℃ of heads, screw speed are melt blending under the condition of 9rpm; Extruding pelletization promptly obtains starch acetate-PPDO graft copolymer/inorganic particulate nano composite material.
Embodiment 14
Starch acetate-PPDO graft copolymer synthetic the same.
With the 100g intrinsic viscosity is starch acetate-PPDO graft copolymer of 1.6dL/g, and wherein the content of starch acetate is 30%, and substitution value is 2.3; Molecular weight is 50000; With 0.5g tired take off stone one at first in impeller blend even, in twin screw extruder, press 85 ℃ of feeding sections then, 115 ℃ of mixing sections; 120 ℃ of fluxing zones; 115 ℃ of heads, screw speed are melt blending under the condition of 9rpm, promptly obtain starch acetate-PPDO graft copolymer/inorganic particulate nano composite material.
Embodiment 15
Starch acetate-PPDO graft copolymer synthetic the same.
With the 100g intrinsic viscosity is starch acetate-PPDO graft copolymer of 2.0dL/g, and wherein the content of starch acetate is 15%, and substitution value is 1.5; Molecular weight is 15000, with the 7g sepiolite, one at first in impeller blend even; In twin screw extruder, press 100 ℃ of feeding sections then; 120 ℃ of mixing sections, 125 ℃ of fluxing zones, 120 ℃ of heads; Screw speed is a melt blending under the condition of 9rpm, promptly obtains starch acetate-PPDO graft copolymer/inorganic particulate nano composite material.
Embodiment 16
Starch acetate-PPDO graft copolymer synthetic the same.
With the 100g intrinsic viscosity is starch acetate-PPDO graft copolymer of 1.9dL/g, and wherein the content of starch acetate is 30%, and substitution value is 1.6; Molecular weight is 50000; With 7g polynite one at first in impeller blend even, in twin screw extruder, press 90 ℃ of feeding sections then, 120 ℃ of mixing sections; 125 ℃ of fluxing zones; 120 ℃ of heads, screw speed are melt blending under the condition of 9rpm, promptly obtain starch acetate-PPDO graft copolymer/inorganic particulate nano composite material.
Embodiment 17
Starch acetate-PPDO graft copolymer synthetic the same.
With the 100g intrinsic viscosity is starch acetate-PPDO graft copolymer of 2.2dL/g, and wherein the content of starch acetate is 1%, and substitution value is 2.7; Molecular weight is 75000, with 1g polynite one at first in impeller blend even, in twin screw extruder, press 125 ℃ of feeding sections then; 135 ℃ of mixing sections; 140 ℃ of fluxing zones, 120 ℃ of heads, screw speed are melt blending under the condition of 9rpm; Extruding pelletization promptly obtains starch acetate-PPDO graft copolymer/inorganic particulate nano composite material.
Embodiment 18
Starch acetate-PPDO graft copolymer synthetic the same.
With the 100g intrinsic viscosity is starch acetate-PPDO graft copolymer of 1.7dL/g, and wherein the content of starch acetate is 10%, and substitution value is 2.3; Molecular weight is 100000; With 5g tired take off stone one at first in impeller blend even, in twin screw extruder, press 90 ℃ of feeding sections then, 120 ℃ of mixing sections; 125 ℃ of fluxing zones; 120 ℃ of heads, screw speed are melt blending under the condition of 9rpm, promptly obtain starch acetate-PPDO graft copolymer/inorganic particulate nano composite material.
Comparative Examples 1
With substitution value is 2.3; Molecular weight be 30000 5 parts of starch acetates, new distillatory to 95 parts of dioxy pimelinketone monomers, join in the reaction flask under nitrogen protection ultrasonic 2 hours successively; Starch acetate is dissolved in the dioxy pimelinketone monomer fully; Be warmed up to 80 ℃ then, add again and the triethylaluminium catalyst that to dioxy pimelinketone mol ratio is 0.002, react and promptly obtained starch acetate-PPDO graft copolymer in 6 hours.
Comparative Examples 2
New distillatory is joined in the reaction flask dioxy pimelinketone monomer, be warmed up to 80 ℃ then, add again and the triethylaluminium catalyst that to dioxy pimelinketone mol ratio is 0.002, react and promptly obtained the PPDO homopolymer in 6 hours.
Mechanical property for starch acetate-PPDO graft copolymer/inorganic particulate nano composite material of investigating preparation; The present invention is prepared into batten with the nano composite material of embodiment and Comparative Examples acquisition; Press the regulation of GB1040-79G and measure its tensile strength and elongation at break, its result sees table 1.
Table 1
The biodegradability of starch acetate-PPDO graft copolymer/inorganic particulate nano composite material that the present invention is obtained is tested according to the standard of ASTM D5338 (the biodegradable standard law of the mensuration aerobic type of plastics under the tip environment of simcity).Be placed on the batten that starch acetate-the PPDO graft copolymer/inorganic particulate nano composite material is processed under the tip environment of simcity, period sampling measuring batten intrinsic viscosity over time.Its result sees table 2.
Table 2
Claims (2)
1. the preparation method of starch acetate-PPDO graft copolymer/inorganic particulate nano composite material; This method be with the starch acetate of 1～40 weight part and 60～99 weight parts count 0.5～10% nano grade inorganic particle to dioxy pimelinketone monomer with the weight of starch acetate-PPDO graft copolymer, under nitrogen atmosphere protection, ultra-sonic dispersion 1～2 hour; Be warming up to 60～120 ℃ then; Add and the catalyzer that to the monomeric mol ratio of dioxy pimelinketone is 1: 0.001～0.004, react and got final product in 6～20 hours, or directly with starch acetate-PPDO graft copolymer and nano grade inorganic particle; Ratio by weight 100: 0.5～10; Melt blending again behind premix, the melt blending temperature is 85～140 ℃
Wherein used nano grade inorganic particle is that any in the stone taken off in polynite, layered double-hydroxide, sepiolite or tired; The substitution value of used starch acetate is 1.5～2.9, and molecular weight is 15000～100000.
2. the preparation method of starch acetate according to claim 1-PPDO graft copolymer/inorganic particulate nano composite material, the used catalyzer of this method is any in aluminum alkyls or the alkoxy compound.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1709969A (en) * | 2005-07-13 | 2005-12-21 | 四川大学 | Fully-biodegradable film using poly P-dioxy cyclohexanone as matrix and its preparing method |
| CN1919892A (en) * | 2006-08-29 | 2007-02-28 | 四川大学 | Method of preparing poly p-dioxanone and montmorillonite nano composite material thereof by microwave radiation |
| CN101337994A (en) * | 2008-08-08 | 2009-01-07 | 四川大学 | Starch acetate/PPDO-grafted copolymer, preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1709969A (en) * | 2005-07-13 | 2005-12-21 | 四川大学 | Fully-biodegradable film using poly P-dioxy cyclohexanone as matrix and its preparing method |
| CN1919892A (en) * | 2006-08-29 | 2007-02-28 | 四川大学 | Method of preparing poly p-dioxanone and montmorillonite nano composite material thereof by microwave radiation |
| CN101337994A (en) * | 2008-08-08 | 2009-01-07 | 四川大学 | Starch acetate/PPDO-grafted copolymer, preparation method and application thereof |
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