CN105153654A - Fiber-reinforced polyester composition and preparation method thereof - Google Patents
Fiber-reinforced polyester composition and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a fiber-reinforced polyester composition and a preparation method thereof, belonging to the technical field of materials. POSS (polyhedral oligomeric silsesquioxane) with active epoxy side group is used as a chain extender and rigid particle toughener to respectively modify and reinforce PET (polyethylene terephthalate). According to the fiber-reinforced polyester composition, the mass rate of reinforcing fibers is 15-50%; and the modifying base at least comprises the following components in parts by mass: 100 parts of polyester resin and 0.8-3 parts of POSS. The POSS is selected from one of [(R1SiO1.5)8]Sigma8 and [(RSiO1.5)4(RSiO1.0OH)3]Sigma7. The preparation method of the fiber-reinforced polyester composition adopts a double screw extruder melting compounding technique, and the reinforcing fibers are introduced from a side feed port. The fiber-reinforced polyester composition provided by the invention has the advantages of high strength, favorable toughness, high crystallization hardening rate and short intramode cooling time, and is especially suitable for high-speed injection molding of fabricated products.
Description
Technical field
The invention belongs to field of material technology, relate to polymer modification technology, particularly the design of fiber reinforcement engineering plastics and processing technology.
Background technology
Polyethylene terephthalate (PET) engineering plastics are one of most active research and development focuses of the non-fine Application Areas of PET in the world today, especially in recent years, PET engineering plastics constantly increase with its excellent performance, lower production cost and higher cost performance proportion in without industry engineering plastics, and current PET engineering plastics are widely used in the aspects such as various load bearing equipment, automobile, household electrical appliance and furniture.
Adopt fiber-reinforced modified PET to be the important modified measures that PET applies as engineering plastics, fiber reinforcement greatly can improve the intensity of PET, toughness, heat-drawn wire and processing technology.But adopt the blended method that obtains of twin-screw extrusion to prepare enhancing modified PET, because the high temperature of extrusion and high speed shear effect are easy to the degraded, the chain scission that cause PET molecular chain, cause the reduction of material property, comprise intensity and reduce (dying down) and toughness reduction (becoming fragile), so chain extension thickening, the reconstruction molecular weight in the PET course of processing, be the important measures improving PET engineering plastics performance.
Polyhedral oligomeric silsesquioxane (POSS) is a kind of organic-inorganic materials, and it is the space cagelike structure that the inorganic nano core be made up of silicone atom is formed with peripheral organic group, and size arrives several nano level 1.The specific hybrid inorganic-organic structure of POSS, it is made both to have had the stability of inorganic materials, have and possess the natural good consistency with organic polymer material, POSS class nano material has much special character, as high temperature resistant, rub resistance, fire-retardant, high structural stability, low dielectric, high strength etc.POSS and the polymer with active lateral group are easy to chemical reaction occurs, and can be used as the nanometer strengthener of polymer materials, Rigid Particles Toughened agent and chainextender.Epoxy group(ing) POSS is adopted to carry out modification as reactive chain extenders to REINFORCED PET, the active epoxy group PET molecular chain of epoxy-functional POSS periphery reacts, between different PET molecular chain, play the effect of chain extension-crosslinking, improve the viscosity of resin matrix, thus can improve the intensity of material.Rigidity POSS nanoparticulate dispersed in the base in addition, when being subject to shock action, can playing the effect absorbing striking energy, thus can improve the toughness of material by causing crazing at periphery.
Ou Yuxiang etc. are at document " the chemical modification POSS for polymer nanocomposites " (chemistry circular, 6,2009) mention in, single active group POSS modified PET material can be adopted, improve PET Young's modulus, but the single active group POSS adopted does not have the effect of chain extension thickening, the effect improving Reinforced PET Composite over-all properties can not be played.
Liu Wei mentions in its Master's thesis " preparation and property of POSS/PET matrix material ", blending method is adopted to prepare POSS/PET matrix material, POSS can play the effect of heterogeneous nucleation to PET, affect PET crystal habit, but its POSS kind adopted does not have the effect of chain extension thickening yet.
Summary of the invention
PET engineering plastic composition that the object of the present invention is to provide a kind of high-strength and high ductility and preparation method thereof.The object of the present invention is achieved like this, adopts POSS with active epoxy side base as chainextender and Rigid Particles Toughened agent, inorganic or organic fibre conduct
toughener, respectively modification and enhancing are carried out to PET, are aided with conven-tional adjuvants, obtain the PET engineering plastic composition that intensity and toughness significantly improve.
The fiber reinforced polyester composition that the present invention relates to, the mass ratio of fortifying fibre is between 15 ~ 50%, and the quality of material composition of modified matrix at least comprises:
100 parts, vibrin,
POSS0.8 ~ 3 part,
Wherein, described vibrin is the ethylene glycol terephthalate (PET) of limiting viscosity 0.78 ~ 0.875dl/g; Described POSS is selected from ［ (R
1siO
1.5)
8?
∑ 8, ［ (RSiO
1.5)
4(RSiO
1.0oH)
3?
∑ 7pOSS in one, wherein: R is selected from the one in alkyl, aryl; R
1be selected from the one in epoxy alkyl, epoxy cycloalkyl; ∑ # represents the Siliciumatom number in POSS molecule, and # is that 8 to represent POSS molecule be complete cagelike structure, and # is the 7 imperfect cagelike structures representing that POSS molecule is unfilled corner.
The fiber reinforced polyester composition that the present invention relates to, the mass ratio of fortifying fibre is between 15 ~ 50%, and the quality of material of modified matrix consists of:
100 parts, vibrin,
POSS0.8 ~ 3 part,
Compatilizer 2 ~ 7.5 parts,
Crystallization promoter 1.5 ~ 4.5 parts,
Crystallization nucleating agent 0.5 ~ 3 part;
Wherein, described compatilizer is acrylic acid esters co-polymer, and described crystallization promoter is the one in polyoxyethylene glycol or polyether ester, and described crystallization nucleating agent is one in talcum powder, Phenylsulfonic acid calcium, ionic polymer or its mixed system.
The fiber reinforced polyester composition that the present invention relates to, described vibrin is.
The fiber reinforced polyester composition that the present invention relates to, the mass ratio of vibrin and POSS is between 100:1.5 ~ 2.5.
The fiber reinforced polyester composition that the present invention relates to, described compatilizer is selected from one in ethylene-methacrylic acid copolymer EMA, ethylene-butyl acrylate copolymer EBA, ethylene-methyl acrylate-glyceryl methacrylate multipolymer EMA-GMA or its mixed system.
The fiber reinforced polyester composition that the present invention relates to, the mass ratio of vibrin and compatilizer is between 100:3 ~ 5.
The fiber reinforced polyester composition that the present invention relates to, the mass ratio of vibrin and crystallization promoter is between 100:2 ~ 3.5.
The fiber reinforced polyester composition that the present invention relates to, the mass ratio of vibrin and crystallization nucleating agent is between 100:0.75 ~ 2.5.
The fiber reinforced polyester composition that the present invention relates to, wherein fortifying fibre is selected from glass fibre, carbon fiber or aramid fiber.
The fiber reinforced polyester composition that the present invention relates to, reinforced fiber content is between 30 ~ 40wt%.
The preparation method of the fiber reinforced polyester composition that the present invention relates to, adopt twin screw extruder melting mixing technique, side spout introduces fortifying fibre, it is characterized in that: screw rod and head temperature are: 240 DEG C ~ 270 DEG C, screw speed 400 ~ 480r/min.
The fiber reinforced polyester composition that the present invention relates to, POSS is simultaneously as chainextender and Rigid Particles Toughened collection, play a part to rebuild molecular weight in extrusion process, the REINFORCED PET engineering plastics of preparation, intensity is high, good toughness, and crystal hardened speed is high, in mould, cooling time is short, is specially adapted to high speed injection motding fabricated product.
Embodiment
Below in conjunction with specific embodiment, the technical scheme that the present invention proposes is further described, but not as the restriction to technical scheme.
Comparative example
By 100 parts of PET resin (HY-C01, viscosity 0.875dl/g), 5 parts of EMA-GMA, 0.75 part of talcum powder, after 2 parts of polyoxyethylene glycol (PEG-400) mix, processing is extruded with CTE35 equidirectional parallel double-screw extruder, glass fibre (14-2000-988A) introduced by side feeding, screw rod 9 district and head temperature are set as: 240, 245, 250, 255, 255, 245, 245, 245, 240, 250, screw speed is 400r/min, controlling fibre content is 30%, the tensile strength of matrix material is 115MPa, flexural strength is 150MPa, modulus in flexure is 7250MPa, Izod notched impact strength is 10KJ/m
2, heat-drawn wire is 239 DEG C (0.45MPa).
Embodiment 1
By 100 parts of PET resin (CB-608S, viscosity 0.865dl/g), 0.8 part of POSS (［ (γ-epoxypropoxy-SiO
1.5)
8?
∑ 8), after 5 parts of EMA-GMA, 0.75 part of talcum powder, 2 parts of polyoxyethylene glycol (PEG-400) mix, processing is extruded with CTE35 equidirectional parallel double-screw extruder, glass fibre (14-2000-988A) introduced by side feeding, and screw rod 9 district and head temperature are set as: 240, and 245,250,255,255,245,245,245,240,250, screw speed is 400r/min, controlling fibre content is 30%, and the tensile strength of matrix material is 125MPa, and flexural strength is 179MPa, modulus in flexure is 8390MPa, and Izod notched impact strength is 12KJ/m
2, heat-drawn wire is 243 DEG C (0.45MPa).
Embodiment 2
By 100 parts of PET resin (WP56151, viscosity 0.81dl/g), 1.5 parts of POSS (［ (γ-epoxypropoxy-SiO
1.5)
8?
∑ 8), 2 parts of EMA, 2.5 parts of ionic polymers (sarin 8920), after 1.5 parts of polyoxyethylene glycol (PEG-800) mix, processing is extruded with CTE35 equidirectional parallel double-screw extruder, glass fibre (ER-4300) introduced by side feeding, screw rod 9 district and head temperature are set as: 240, 265, 265, 260, 255, 245, 245, 245, 240, 255, screw speed is 450r/min, controlling fibre content is 29.5%, the tensile strength of matrix material is 133MPa, flexural strength is 195MPa, modulus in flexure is 8875MPa, Izod notched impact strength is 13KJ/m
2, heat-drawn wire is 244 DEG C (0.45MPa).
Embodiment 3
By 100 parts of PET resin (WP56151, viscosity 0.81dl/g), 1.9 parts of POSS (［ (1-(2,3 epoxy group(ing)-cyclohexyl)-ethyl-SiO
1.5)
8?
∑ 8), 2.45 part EBA, 2.3 parts of ionic polymers (sarin 8920), after 2.2 parts of polyoxyethylene glycol (PEG-800) mix, processing is extruded with CTE35 equidirectional parallel double-screw extruder, glass fibre (14-2000-988A) introduced by side feeding, screw rod 9 district and head temperature are set as: 240, 245, 250, 255, 255, 245, 245, 245, 240, 250, screw speed is 450r/min, controlling fibre content is 50%, the tensile strength of matrix material is 164MPa, flexural strength is 230MPa, modulus in flexure is 10155MPa, Izod notched impact strength is 15KJ/m
2, heat-drawn wire is 245 DEG C (0.45MPa).
Embodiment 4
By 100 parts of PET resin (WP56151, viscosity 0.81dl/g), 1.6 parts of POSS (［ (butyl-SiO
1.5)
4(SiO
1.0oH)
3?
∑ 7), 1.9 parts of EMA, 2.65 parts of ionic polymers (sarin 8920), after 2 parts of polyether esters (Uniplex510) mix, processing is extruded with CTE35 equidirectional parallel double-screw extruder, glass fibre (14-2000-988A) introduced by side feeding, screw rod 9 district and head temperature are set as: 240, 245, 250, 255, 255, 245, 245, 245, 240, 250, screw speed is 460r/min, controlling fibre content is 15%, the tensile strength of matrix material is 103MPa, flexural strength is 150MPa, modulus in flexure is 6560MPa, Izod notched impact strength is 9.5KJ/m
2, heat-drawn wire is 212 DEG C (0.45MPa).
Embodiment 5
By 100 parts of PET resin (HY-H01, viscosity 0.78dl/g), 2.3 parts of POSS (［ (γ-epoxypropoxy-SiO
1.5)
8?
∑ 8), after 2.8 parts of EBA, 0.5 part of Phenylsulfonic acid calcium (HK195), 4.5 parts of polyether esters (Tegmer809) mix, processing is extruded with CTE35 equidirectional parallel double-screw extruder, screw rod 9 district and head temperature are set as: 240,255,265,265,255,245,245,245,240,250, screw speed is 480r/min, and controlling fibre content is 24.8%, the tensile strength of matrix material is 135MPa, flexural strength is 200MPa, and modulus in flexure is 8570MPa, and Izod notched impact strength is 14KJ/m
2, heat-drawn wire is 243 DEG C (0.45MPa).
Embodiment 6
By 100 parts of PET resin (HY-H01, viscosity 0.78dl/g), 2.5 parts of POSS (［ (iso-octyl-SiO
1.5)
4(SiO
1.0oH)
3?
∑ 7), after 3 parts of EMA-GMA, 0.7 part of talcum powder, 4 parts of polyoxyethylene glycol (PEG400) mix, processing is extruded with CTE35 equidirectional parallel double-screw extruder, glass fibre (ECS-301HP) introduced by side feeding, and screw rod 9 district and head temperature are set as: 240, and 270,270,265,255,245,245,245,240,255, screw speed is 475r/min, controlling fibre content is 20%, and the tensile strength of matrix material is 110MPa, and flexural strength is 160MPa, modulus in flexure is 6895MPa, and Izod notched impact strength is 10KJ/m
2, heat-drawn wire is 225 DEG C (0.45MPa).
Embodiment 7
By 100 parts of PET resin (HY-C01, viscosity 0.875dl/g), 3 parts of POSS (［ (phenyl-SiO
1.5)
4(SiO
1.0oH)
3?
∑ 7), 7.5 parts of EMA-GMA, 1.5 parts of ionic polymers (sarin 8920), after 2.2 parts of polyether esters (Tegmer809) mix, processing is extruded with CTE35 equidirectional parallel double-screw extruder, glass fibre (ER-4300) introduced by side feeding, screw rod 9 district and head temperature are set as: 240, 265, 270, 265, 255, 245, 245, 245, 240, 250, screw speed is 470r/min, controlling fibre content is 32%, the tensile strength of matrix material is 119MPa, flexural strength is 185MPa, modulus in flexure is 7850MPa, Izod notched impact strength is 16KJ/m
2, heat-drawn wire is 242 DEG C (0.45MPa).
Embodiment 8
By 100 parts of PET resin (HY-C01, viscosity 0.875dl/g), 3 parts of POSS (［ (1-(2,3 epoxy group(ing)-cyclohexyl)-ethyl-SiO
1.5)
8?
∑ 8), 7 parts of EMA-GMA, 2 parts of ionic polymers (sarin 8940), after 2.2 parts of polyether esters (Tegmer809) mix, processing is extruded with CTE35 equidirectional parallel double-screw extruder, carbon fiber (T300-1000) introduced by side feeding, screw rod 9 district and head temperature are set as: 240, 255, 260, 265, 255, 245, 245, 245, 240, 250, screw speed is 440r/min, controlling fibre content is 44.7%, the tensile strength of matrix material is 155MPa, flexural strength is 220MPa, modulus in flexure is 9150MPa, Izod notched impact strength is 15KJ/m
2, heat-drawn wire is 245 DEG C (0.45MPa).
Embodiment 9
By 100 parts of PET resin (HY-C01, viscosity 0.875dl/g), 2.2 parts of POSS (［ (isobutyl--SiO
1.5)
4(SiO
1.0oH)
3?
∑ 7), 3.8 parts of EBA, 0.45 part of Phenylsulfonic acid calcium (HK195), 2.1 parts of ionic polymers (sarin 8920), after 3.5 parts of polyoxyethylene glycol (PEG-400) mix, processing is extruded with CTE35 equidirectional parallel double-screw extruder, screw rod 9 district and head temperature are set as: 240, 270, 270, 265, 255, 245, 245, 245, 240, 250, screw speed is 450r/min, extrusion temperature is set as 240 DEG C ~ 270 DEG C, controlling fibre content is 36%, the tensile strength of matrix material is 130MPa, flexural strength is 193MPa, modulus in flexure is 8860MPa, Izod notched impact strength is 14KJ/m
2, heat-drawn wire is 244 DEG C (0.45MPa).
Embodiment 10
By 100 parts of PET resin (HY-C01, viscosity 0.875dl/g), 2 parts of POSS (［ (isobutyl--SiO
1.5)
4(SiO
1.0oH)
3?
∑ 7), 4 parts of EBA, 0.5 part of Phenylsulfonic acid calcium (HK195), 2.2 parts of ionic polymers (sarin 8920), after 3.5 parts of polyoxyethylene glycol (PEG-400) mix, processing is extruded with CTE35 equidirectional parallel double-screw extruder, screw rod 9 district and head temperature are set as: 240, 270, 270, 265, 2260, 250, 245, 245, 240, 255, screw speed is 450r/min, extrusion temperature is set as 240 DEG C ~ 270 DEG C, controlling fibre content is 30%, the tensile strength of matrix material is 130MPa, flexural strength is 193MPa, modulus in flexure is 8860MPa, Izod notched impact strength is 14KJ/m
2, heat-drawn wire is 244 DEG C (0.45MPa).
Embodiment 11
By 100 parts of PET resin (HY-C01, viscosity 0.875dl/g), 2.3 parts of POSS (［ (isobutyl--SiO
1.5)
4(SiO
1.0oH)
3?
∑ 7), 3.9 parts of EMA, 1 part of talcum powder, 2 parts of ionic polymers (sarin 8940), after 3.5 parts of polyoxyethylene glycol (PEG-800) mix, processing is extruded with CTE35 equidirectional parallel double-screw extruder, aramid fiber (Twaron1488 introduced by side feeding, 3mm), screw rod 9 district and head temperature are set as: 240, 270, 265, 255, 255, 245, 245, 245, 240, 255, screw speed is 480r/min, controlling fibre content is 39.1%, the tensile strength of matrix material is 135MPa, flexural strength is 202MPa, modulus in flexure is 8950MPa, Izod notched impact strength is 13KJ/m
2, heat-drawn wire is 244 DEG C (0.45MPa).
Embodiment 12
By 100 parts of PET resin (CB-608S, viscosity 0.865dl/g), 1 part of POSS (［ (γ-epoxypropoxy-SiO
1.5)
8?
∑ 8), 2 parts of EMA, 1.3 parts of ionic polymers (sarin 8920), after 2.5 parts of polyether esters (Uniplex512) mix, processing is extruded with CTE35 equidirectional parallel double-screw extruder, glass fibre (14-2000-988A) introduced by side feeding, screw rod 9 district and head temperature are set as: 240, 260, 270, 265, 2060, 245, 245, 245, 240, 250, screw speed is 460r/min, controlling fibre content is 30%, the tensile strength of matrix material is 120MPa, flexural strength is 175MPa, modulus in flexure is 8567MPa, Izod notched impact strength is 11KJ/m
2, heat-drawn wire is 243 DEG C (0.45MPa).
Claims (9)
1. a fiber reinforced polyester composition, the mass ratio of fortifying fibre is between 15 ~ 50%, and the quality of material composition of modified matrix at least comprises:
100 parts, vibrin,
POSS0.8 ~ 3 part,
Wherein, described vibrin is the ethylene glycol terephthalate of limiting viscosity 0.78 ~ 0.875dl/g; Described POSS is selected from ［ (R
1siO
1.5)
8?
∑ 8, ［ (RSiO
1.5)
4(RSiO
1.0oH)
3?
∑ 7pOSS in one, wherein: R is selected from the one in alkyl, aryl; R
1be selected from the one in epoxy alkyl, epoxy cycloalkyl.
2. fiber reinforced polyester composition according to claim 1, the quality of material of modified matrix consists of:
100 parts, vibrin,
POSS0.8 ~ 3 part,
Compatilizer 2 ~ 7.5 parts,
Crystallization promoter 1.5 ~ 4.5 parts,
Crystallization nucleating agent 0.5 ~ 3 part;
Wherein, described compatilizer is acrylic acid esters co-polymer, and described crystallization promoter is the one in polyoxyethylene glycol or polyether ester, and described crystallization nucleating agent is one in talcum powder, Phenylsulfonic acid calcium, ionic polymer or or its mixed system.
3. the fiber reinforced polyester composition according to claim 1 or 2 any one, the mass ratio of vibrin and POSS is between 100:1.5 ~ 2.5.
4. fiber reinforced polyester composition according to claim 2, described acrylic acid esters co-polymer is selected from one in ethylene-methacrylic acid copolymer EMA, ethylene-butyl acrylate copolymer EBA, ethylene-methyl acrylate-glyceryl methacrylate multipolymer EMA-GMA or its mixed system.
5. fiber reinforced polyester composition according to claim 2, the mass ratio of vibrin and compatilizer is between 100:3 ~ 5.
6. fiber reinforced polyester composition according to claim 2, the mass ratio of vibrin and crystallization promoter is between 100:2 ~ 3.5.
7. fiber reinforced polyester composition according to claim 2, the mass ratio of vibrin and crystallization nucleating agent is between 100:0.75 ~ 2.5.
8. the fiber reinforced polyester composition according to claim 1 or 2 any one, reinforced fiber content is between 30 ~ 40wt%.
9. the preparation method of fiber reinforced polyester composition according to claim 8, adopt twin screw extruder melting mixing technique, side spout introduces fortifying fibre, it is characterized in that: screw rod and head temperature are: 240 DEG C ~ 270 DEG C, screw speed 400 ~ 480r/min.
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| CN105602210A (en) * | 2015-12-29 | 2016-05-25 | 江苏沃特特种材料制造有限公司 | Light liquid crystal polyester resin compound and preparation method thereof |
| 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 |
| CN111118661A (en) * | 2019-12-18 | 2020-05-08 | 晋江市远祥服装织造有限公司 | Biomass ultraviolet-proof fabric and preparation method and product thereof |
| CN111320846A (en) * | 2020-04-21 | 2020-06-23 | 广东圆融新材料有限公司 | Polyethylene terephthalate composition and preparation method thereof |
| CN111334037A (en) * | 2020-04-23 | 2020-06-26 | 广东中塑新材料有限公司 | PA1010 composite material and preparation method thereof |
| CN111334007A (en) * | 2020-04-21 | 2020-06-26 | 广东圆融新材料有限公司 | Reinforced polyethylene terephthalate composition and preparation method thereof |
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| CN105602210A (en) * | 2015-12-29 | 2016-05-25 | 江苏沃特特种材料制造有限公司 | Light liquid crystal polyester resin compound and preparation method thereof |
| 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 |
| CN111118661A (en) * | 2019-12-18 | 2020-05-08 | 晋江市远祥服装织造有限公司 | Biomass ultraviolet-proof fabric and preparation method and product thereof |
| CN111320846A (en) * | 2020-04-21 | 2020-06-23 | 广东圆融新材料有限公司 | Polyethylene terephthalate composition and preparation method thereof |
| CN111334007A (en) * | 2020-04-21 | 2020-06-26 | 广东圆融新材料有限公司 | Reinforced polyethylene terephthalate composition and preparation method thereof |
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Application publication date: 20151216 |