CN101906241A - Polydiethylene glycol sebacate/silsesquioxane composition - Google Patents
Polydiethylene glycol sebacate/silsesquioxane composition Download PDFInfo
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- CN101906241A CN101906241A CN2009101438900A CN200910143890A CN101906241A CN 101906241 A CN101906241 A CN 101906241A CN 2009101438900 A CN2009101438900 A CN 2009101438900A CN 200910143890 A CN200910143890 A CN 200910143890A CN 101906241 A CN101906241 A CN 101906241A
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- butylene succinate
- poly butylene
- silicious sesquioxane
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Abstract
The invention discloses a polydiethylene glycol sebacate/silsesquioxane composition, which is prepared from polydiethylene glycol sebacate, silsesquioxane and chain extender by melt blending, extruding and granulating. The composition has high comprehensive performance and biodegradability and has wide applications.
Description
Technical field
The present invention relates to class poly butylene succinate/silicious sesquioxane composition.Specifically, relate to poly butylene succinate and cage type or not exclusively clathrasil sesquioxyalkane and chainextender, through melt blending, extrude, composition that granulation obtains.
Background technology
Poly butylene succinate (polybutylene succinate PBS) is formed through polycondensation by Succinic Acid and butyleneglycol, be a kind of can Biodegradable Materials, different according to the height of molecular weight and molecular weight distribution, degree of crystallinity is about 30%-50%.PBS has thermostability and higher molecular weight preferably, heat-drawn wire and goods use temperature near or above 100 ℃, PBS has favorable mechanical and processing characteristics, can carry out the service requirements that all kinds of forming process also satisfy general-purpose plastics substantially on general processing units; Can be widely used in packing, agricultural, field of medical materials.
Polyhedral oligomeric silsesquioxane (Polyhedral Oligomeric Silsesquioxane, POSS) monomer is at present unique inorganic-organic hybridization nano chemistry filler, it not only combines organic constituent and inorganic component high-performance separately, but also has the new capability that is produced by both synergistic effects.Can think that the POSS molecule is minimum silicon dioxide microparticle.Its molecular formula can be expressed as (RSiO
1.5)
n(n generally can be 6,8,10,12 etc.), it is the hybrid compounds that shell is formed by the rigid structure nano grade inorganic kernel of D S i-O chain formation with the organic group that is connected by covalent linkage.The advantage of hybrid material can be mixed, be brought into play to the nano level cage modle skeleton of POSS effectively, gives good toughness of hybrid material and workability, and this special construction more and more is applied in the modification of material POSS.Its modification is used and is mainly contained: 1. as additive, can improve the mechanical property of polymers matrix, improve thermostability, reduce viscosity, improve the shock resistance and the flame retardant resistance of material.2. as reactant,, POSS is participated in the polymer reaction as catalyzer by to the POSS structure Design.Can also be used as big monomer and linking agent.3. can be used as lubricant and expanding material.(specifically referring to 1.Yiwang Chen, Lie Chen, Huarong Nie, E.T.Kang, Journal ofApplied Polymer Science, 2006,99:2226-2232; 2.Yiwang Chen, En-Tang Kang.Materials Letters, 2004,58:3716-3719; 3.Cuirong Pan, James E.Mark, Dale W.Schaefer.Journal of Polymer Science:Part B:Polymer Physics, 2003,41:3314-3323.)
The chainextender blending and modifying is extruded and is meant that utilizing forcing machine to add chainextender as reactor carries out the chemical group coupling, chainextender can reduce the influence of thermal destruction to polymericular weight in melt blending, it is a kind of compound of bifunctional normally, is easy to the radical reaction with a kind of oligomer chain end of or two kinds of polymkeric substance.By its functional group reactions different, be divided into hydroxyl add-on type, carboxyl add-on type and hydroxyl, carboxyl add-on type with polymkeric substance.Chainextender commonly used mainly contains compounds such as bisoxazoline, epoxide, vulcabond, two lactan, dicarboxylic anhydride.(specifically referring to Tuornmen J., Kim B.O., Jun H.S., et al, PolymerBulletin, 1995,35 (4): 415-421.)
Present research does not all relate to the report that poly butylene succinate, silicious sesquioxane and chainextender prepare composition.Said composition has good comprehensive performances, has a extensive future.
Summary of the invention
The objective of the invention is to propose class poly butylene succinate/silicious sesquioxane composition.The composition that this poly butylene succinate/silicious sesquioxane composition is with poly butylene succinate, silicious sesquioxane and expansion connection agent blend under molten state, extrude, granulation obtains.
The objective of the invention is to propose class poly butylene succinate/silicious sesquioxane composition.The composition that this poly butylene succinate/silicious sesquioxane composition is with poly butylene succinate, silicious sesquioxane and expansion connection agent blend under molten state, extrude, granulation obtains, wherein chainextender is 0.1～5% (quality percentage composition), silicious sesquioxane is 0.5-20% (a quality percentage composition), poly butylene succinate 99.4%～72% (quality percentage composition).
Poly butylene succinate/silicious sesquioxane composition that the present invention proposes, wherein silicious sesquioxane comprises clathrasil sesquioxyalkane or incomplete clathrasil sesquioxyalkane.
Poly butylene succinate/silicious sesquioxane composition that the present invention proposes, wherein silicious sesquioxane is the clathrasil sesquioxyalkane, comprises for example octaphenyl silicious sesquioxane, ten phenylbenzene silicious sesquioxanes, eight isobutyl-silicious sesquioxanes, prestox silicious sesquioxane, eight cyclohexyl silicious sesquioxanes, eight poly-(trimethyl silicon based) silicious sesquioxanes etc.
Poly butylene succinate/silicious sesquioxane composition that the present invention proposes, wherein not exclusively the clathrasil sesquioxyalkane comprises for example seven phenyl silicious sesquioxanes, three silanols, seven isobutyl-silicious sesquioxanes, three silanols etc.
Poly butylene succinate/silicious sesquioxane composition that the present invention proposes, wherein the chainextender that is adopted is the polyester chain extender that those skilled in the art are familiar with, comprise bisoxazoline compounds, for example 1, two (2-oxazoline) benzene (PBO) of 3-, 2,2 '-two (2-oxazolines), 1, two (2-oxazoline) benzene of 4-; Epoxy compounds, for example E51 Resins, epoxy; Vulcabond, for example tolylene diisocyanate; N, the two lactan of N '-carbonyl; The two lactam compounds of two acyl groups, for example two hexanolactams of hexanedioyl, the two hexanolactams of terephthaloyl, the two hexanolactams of isophthaloyl; Anhydride compounds, for example pyromellitic acid acid anhydride.
Poly butylene succinate/silicious sesquioxane composition that the present invention proposes, its preparation method is the melting mixing method of being familiar with for those skilled in the art, after soon poly butylene succinate, silicious sesquioxane, chainextender will mix, in screw extrusion press, under molten state, mix, extrude, granulation and obtain composition, wherein chainextender is 0.1～5% (quality percentage composition), silicious sesquioxane is 0.5-20% (a quality percentage composition), poly butylene succinate 99.4%～72% (quality percentage composition).
A series of poly butylene succinates/silicious sesquioxane composition that the present invention proposes has the good mechanical performance, is Biodegradable material, is a kind of environmentally friendly material.Have good thermostability and favorable mechanical processing characteristics, and satisfy the service requirements of general-purpose plastics substantially.All kinds of forming process can be carried out, as extrusion moulding, injection molding, compression moulding, calendering formation etc. on general processing units.The present invention prepares poly butylene succinate/silicious sesquioxane composition, can be used as the high-performance environment protection type material and be applied in a lot of fields: as wrapping material, as electron device packing, agricultural materials, as slow-release fertilizer material etc., can also be used for biomaterial for medical purpose.
Embodiment
Comparative Examples 1
50 gram PBS pellets are standby 70 ℃ of vacuum oven 12 hours, use Dynisco LME-230 mixing forcing machine to carry out extruding pelletization at 150 ℃; Prepare test bars by Dynisco PMM-4-230 injection moulding machine again, treat the batten placement after 24 hours, according to testing standard ASTM1708 measurement tensile strength, tensile strength is 36MPa, and elongation at break is 225%.
Comparative Examples 2
PBS pellet and octaphenyl silicious sesquioxane (OPS) powder is standby 70 ℃ of vacuum oven 12 hours, with the two is 0.5% ratio in the OPS massfraction, total mass 50 grams use the yniscoLME-230 of this D. Lab mixing forcing machine to carry out the blend extruding pelletization at 150 ℃; According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 33MPa, and elongation at break is 227%.
Comparative Examples 3
PBS pellet and octaphenyl silicious sesquioxane (OPS) powder is standby 70 ℃ of vacuum oven 12 hours, with the two is 1% ratio in the OPS massfraction, total mass 50 grams, with reference to Comparative Examples 2 method blend granulations, according to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 34MPa, and elongation at break is 221%.
Comparative Examples 4
PBS pellet and OPS powder is standby 70 ℃ of vacuum oven 12 hours, with the two is 5% ratio in the OPS massfraction, total mass 50 grams, with reference to Comparative Examples 2 method blend granulations, according to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 35MPa, and elongation at break is 266%.
Comparative Examples 5
PBS pellet and OPS powder is standby 70 ℃ of vacuum oven 12 hours, with the two is 8% ratio in the OPS massfraction, total mass 50 grams, with reference to Comparative Examples 2 method blend granulations, according to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 32MPa, and elongation at break is 236%.
Comparative Examples 6
PBS pellet and OPS powder is standby 70 ℃ of vacuum oven 12 hours, with the two is 15% ratio in the OPS massfraction, total mass 50 grams, with reference to Comparative Examples 2 method blend granulations, according to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 36MPa, and elongation at break is 285%.
Comparative Examples 7
PBS pellet and OPS powder is standby 70 ℃ of vacuum oven 12 hours, with the two is 20% ratio in the OPS massfraction, total mass 50 grams, with reference to Comparative Examples 2 method blend granulations, according to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 35MPa, and elongation at break is 270%.
Comparative Examples 8
PBS pellet and eight isobutyl-silicious sesquioxane (OIBS) powders are standby 70 ℃ of vacuum oven 12 hours, with the two is 1% ratio in the OIBS massfraction, total mass 50 grams, with reference to Comparative Examples 2 method blend granulations, according to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 33MPa, and elongation at break is 248%.
Comparative Examples 9
PBS pellet and OIBS powder is standby 70 ℃ of vacuum oven 12 hours, with the two is 2% ratio in the OIBS massfraction, total mass 50 grams, with reference to Comparative Examples 2 method blend granulations, according to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 32MPa, and elongation at break is 230%.
Comparative Examples 10
PBS pellet and OIBS powder is standby 70 ℃ of vacuum oven 12 hours, with the two is 5% ratio in the OIBS massfraction, total mass 50 grams, with reference to Comparative Examples 2 method blend granulations, according to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 31MPa, and elongation at break is 209%.
Comparative Examples 11
With PBS pellet and phenyl T
7The POSS powder is standby 70 ℃ of vacuum oven 12 hours, and the two is pressed phenyl T
7The POSS massfraction is 1% ratio, total mass 50 grams, and with reference to Comparative Examples 2 method blend granulations, according to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 34MPa, elongation at break is 205%.
Comparative Examples 12
With PBS pellet and isobutyl-T
7The POSS powder is standby 70 ℃ of vacuum oven 12 hours, and the two is pressed isobutyl-T
7The POSS massfraction is 5% ratio, total mass 50 grams, and with reference to Comparative Examples 2 method blend granulations, according to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 30MPa, elongation at break is 133%.
Embodiment 1
According to Comparative Examples 2, with PBS, OPS and chainextender PBO total mass 50 grams, wherein the massfraction of OPS and PBO is respectively 0.5% and 0.1%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 38MPa, and elongation at break is 211%.
Embodiment 2
According to Comparative Examples 2, with PBS, OPS and chainextender PBO total mass 50 grams, wherein the massfraction of OPS and PBO is respectively 0.5% and 3%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 40MPa, and elongation at break is 283%.
Embodiment 3
According to Comparative Examples 2, with PBS, OPS and chainextender PBO total mass 50 grams, wherein the massfraction of OPS and PBO is respectively 0.5% and 5%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 41MPa, and elongation at break is 290%.
Embodiment 4
According to Comparative Examples 3, with PBS, OPS and chainextender PBO total mass 50 grams, wherein the massfraction of OPS and PBO is respectively 1% and 3%, and melt blending is extruded by carrying out, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 40MPa, and elongation at break is 301%.
Embodiment 5
According to Comparative Examples 3, with PBS, OPS and chainextender PBO total mass 50 grams, wherein the massfraction of OPS and PBO is respectively 1% and 5%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 40MPa, and elongation at break is 308%.
Embodiment 6
According to Comparative Examples 4, with PBS, OPS and chainextender PBO total mass 50 grams, wherein the massfraction of OPS and PBO is respectively 5% and 3%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 43MPa, and elongation at break is 339%.
Embodiment 7
According to Comparative Examples 4, with PBS, OPS and chainextender PBO total mass 50 grams, wherein the massfraction of OPS and PBO is respectively 5% and 5%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 42MPa, and elongation at break is 370%.
Embodiment 8
According to Comparative Examples 5, with PBS, OPS and chainextender PBO total mass 50 grams, wherein the massfraction of OPS and PBO is respectively 8% and 3%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 43MPa, and elongation at break is 397%.
Embodiment 9
According to Comparative Examples 5, with PBS, OPS and chainextender PBO total mass 50 grams, wherein the massfraction of OPS and PBO is respectively 8% and 5%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 37MPa, and elongation at break is 319%.
Embodiment 10
According to Comparative Examples 6, with PBS, OPS and chainextender PBO total mass 50 grams, wherein the massfraction of OPS and PBO is respectively 15% and 5%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 37MPa, and elongation at break is 312%.
Embodiment 11
According to Comparative Examples 7, with PBS, OPS and chainextender PBO total mass 50 grams, wherein the massfraction of OPS and PBO is respectively 20% and 5%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 38MPa, and elongation at break is 286%.
Embodiment 12
According to Comparative Examples 8, with PBS, OIBS and chainextender PBO total mass 50 grams, wherein the massfraction of OIBS and PBO is respectively 1% and 3%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 38MPa, and elongation at break is 291%.
Embodiment 13
According to Comparative Examples 9, with PBS, OIBS and chainextender PBO total mass 50 grams, wherein the massfraction of OIBS and PBO is respectively 2% and 3%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 40MPa, and elongation at break is 302%.
Embodiment 14
According to Comparative Examples 10, with PBS, OIBS and chainextender PBO total mass 50 grams, wherein the massfraction of OIBS and PBO is respectively 5% and 3%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 39MPa, and elongation at break is 262%.
Embodiment 15
According to Comparative Examples 11, with PBS, phenyl T
7POSS and chainextender PBO total mass 50 gram, wherein phenyl T
7The massfraction of POSS and PBO is respectively 5% and 3%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 36MPa, and elongation at break is 244%.
Embodiment 16
According to Comparative Examples 12, with PBS, isobutyl-T
7POSS and chainextender PBO total mass 50 gram, wherein isobutyl-T
7The massfraction of POSS and PBO is respectively 5% and 3%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 35MPa, and elongation at break is 215%.
Embodiment 17
According to Comparative Examples 3, with PBS, OPS and chainextender Resins, epoxy E51 total mass 50 grams, wherein the massfraction of OPS and E51 is respectively 0.5% and 3%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 38MPa, and elongation at break is 233%.
Embodiment 18
According to Comparative Examples 3, with PBS, OPS and chainextender Resins, epoxy E51 total mass 50 grams, wherein the massfraction of OPS and E51 is respectively 5% and 3%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 41MPa, and elongation at break is 309%.
Embodiment 19
According to Comparative Examples 3, with two hexanolactam total masses 50 grams of PBS, OPS and terephthaloyl, wherein the massfraction of the two hexanolactams of OPS and terephthaloyl is respectively 5% and 3%, carries out that melt blending is extruded, granulation, injection moulding batten.According to Comparative Examples 1 described method sample preparation and test, recording tensile strength is 40.5MPa, and elongation at break is 286%.
Claims (5)
1. the composition that class poly butylene succinate/silicious sesquioxane composition is poly butylene succinate, silicious sesquioxane and expansion connection agent blend under molten state, extrude, granulation obtains.
2. poly butylene succinate according to claim 1/silicious sesquioxane composition, it is characterized in that chainextender is 0.1～5% (quality percentage composition), silicious sesquioxane is 0.5-20% (a quality percentage composition), poly butylene succinate 99.4%～72% (quality percentage composition).
3. poly butylene succinate according to claim 1/silicious sesquioxane composition is characterized in that silicious sesquioxane comprises clathrasil sesquioxyalkane or incomplete clathrasil sesquioxyalkane.
4. poly butylene succinate according to claim 1/silicious sesquioxane composition; it is characterized in that chainextender Shi bisoxazoline compounds, epoxy compounds, vulcabond, N, the two lactan of N '-carbonyl, the two lactam compounds of two acyl group, anhydride compounds.
5. poly butylene succinate according to claim 1/silicious sesquioxane composition, preferred chainextender Shi bisoxazoline compounds, epoxy compounds, the two lactam compounds of two acyl group.
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| CN2009101438900A CN101906241A (en) | 2009-06-02 | 2009-06-02 | Polydiethylene glycol sebacate/silsesquioxane composition |
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| CN2009101438900A CN101906241A (en) | 2009-06-02 | 2009-06-02 | Polydiethylene glycol sebacate/silsesquioxane composition |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106566209A (en) * | 2016-10-21 | 2017-04-19 | 上海航天设备制造总厂 | Preparing method of sulfonation octaphenyl multi-face low polysilsesquioxane/polysuccinic acid butanediol ester |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008019338A (en) * | 2006-07-12 | 2008-01-31 | Asahi Kasei Chemicals Corp | Stainproof matte film or sheet |
| CN101319034A (en) * | 2008-07-18 | 2008-12-10 | 中国科学院长春应用化学研究所 | Method for preparing crosslinked poly-succinic butanediol ester |
-
2009
- 2009-06-02 CN CN2009101438900A patent/CN101906241A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008019338A (en) * | 2006-07-12 | 2008-01-31 | Asahi Kasei Chemicals Corp | Stainproof matte film or sheet |
| CN101319034A (en) * | 2008-07-18 | 2008-12-10 | 中国科学院长春应用化学研究所 | Method for preparing crosslinked poly-succinic butanediol ester |
Non-Patent Citations (1)
| Title |
|---|
| TAKENORI SAKUMA，ET AL: ""Thermal and Dynamic Mechanical Properties of Organic-Inorganic Hybrid Composites of Itaconate-Containing Poly（butylene succinate）and Methacrylate-Substituted Polysilsesquioxane"", 《JOURNAL OF APPLIED POLYMER SCIENCE》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106566209A (en) * | 2016-10-21 | 2017-04-19 | 上海航天设备制造总厂 | Preparing method of sulfonation octaphenyl multi-face low polysilsesquioxane/polysuccinic acid butanediol ester |
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Application publication date: 20101208 |