CN115011081A - Glass fiber reinforced PET composition with rapid crystallization and preparation method thereof - Google Patents
Glass fiber reinforced PET composition with rapid crystallization and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
- C08J5/08—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials glass fibres
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- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/08—Copolymers of ethene
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- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/34—Silicon-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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Abstract
The invention discloses a glass fiber reinforced PET composition with rapid crystallization, which comprises the following raw materials in part by weight of 100: 5-75 parts of PET resin; 0-20 parts of PET-PEG block copolymer; 20-45 parts of glass fiber; 0.3-2 parts of a crystallization promoter; 0.5-3 parts of a nucleating agent; 2-5 parts of a toughening agent; 0.1-1.0 part of other auxiliary agents; the glass fiber is selected from alkali-free glass fiber, and the diameter of the glass fiber is 8-15 mu m; the invention provides a preparation method of a glass fiber reinforced PET composition with rapid crystallization, and the prepared glass fiber reinforced PET material has good physical and mechanical properties and impact toughness, high heat-resistant temperature and short molding period, and can be used for injection molding of relevant parts in electronic and electric industries, automobile industries and the like.
Description
Technical Field
The invention relates to the field of modification of PET (polyethylene terephthalate) materials, in particular to a glass fiber reinforced PET composition with rapid crystallization and a preparation method thereof.
Background
The PET has good comprehensive performance, excellent physical and mechanical properties in a wider temperature range, high long-term use temperature of 120 ℃, excellent electrical insulation, good electrical performance even at high temperature and high frequency, and good creep resistance, fatigue resistance, friction resistance and dimensional stability. The modified PET has higher processing and impact properties, can obviously improve the heat resistance, modulus, toughness, dimensional stability and flame retardance of the PET by reinforcing, flame-retardant modifying and alloying modifying the PET, and is widely applied to the fields of electronics, electrics, automobiles and household appliances. In the field of household appliances, the modified PET material can be applied to household appliance shells, oven handles, electromagnetic heating plates of electric cookers and the like.
Because the PET material has the problem that the crystallization speed is slow, the crystallinity is low, even add glass fiber can't accelerate the crystallization of material yet, this just leads to the PET material cycle of moulding plastics extremely long, simultaneously glass fiber reinforced PET material's heat distortion temperature because the crystallinity of PET is low also can not obtain very big degree promotion. In order to improve the crystallization property of the PET material, the crystallization of the PET is improved to a certain extent by adding a nucleating agent or compounding the nucleating agent and a crystallization promoter in the traditional path, although the problem of slow crystallization speed of the PET can be improved to a greater extent, compared with the PBT material, the modified PET material has the defect of longer injection molding period; on the other hand, the nucleating agent and the crystallization promoter can induce the molecular chain of the PET material to degrade, thereby causing the problem that the PET material is fragile after being modified.
Disclosure of Invention
Aiming at the technical problems, the invention provides the glass fiber reinforced PET composition with rapid crystallization and the preparation method thereof, and the prepared PET material has short injection molding period and higher impact toughness.
The specific technical scheme is as follows:
the glass fiber reinforced PET composition with rapid crystallization comprises the following raw materials in parts by weight of 100:
25-75 parts of PET resin;
0-20 parts of PET-PEG block copolymer;
20-45 parts of glass fiber;
0.3-2 parts of a crystallization promoter;
0.5-3 parts of a nucleating agent;
2-5 parts of a toughening agent;
0.1-1.0 part of other auxiliary agents;
the glass fiber is selected from alkali-free glass fiber, and the diameter of the glass fiber is 8-15 mu m;
preferably, the PET resin is a polymer without isophthalic acid (IPA), the intrinsic viscosity is preferably 0.6-1.0 dL/g, and the melting point of the material is more than or equal to 250 ℃. The molecular chain of the PET material is damaged by isophthalic acid (IPA) contained in the molecular chain, and the crystallization performance of the PET material is further reduced.
Preferably, the PET-PEG block copolymer is a block copolymer with PEG molecular weight of 2000-4000 and PEG mass content of 8-15%. PEG is introduced into the PET polymer chain segment, so that the chain flexibility of the polymer molecular chain is greatly increased, and the crystallization capacity of the polymer is improved; on the other hand, the long soft segment of PEG can also improve the notch impact toughness of the modified polymer to a certain extent.
Preferably, the molecular weight of PEG is preferably 2000-4000, the mass content of PEG in the PET-PEG block copolymer is preferably 8-15%, the main consideration is that the quantity of the soft chain segment is too small, and the improvement on the crystallization property of PET is limited; however, too high proportion of the soft segment also affects the molecular chain regularity of the PET material, the crystallization ability of the material is still reduced, and too high proportion of the soft segment, the mechanical strength of the material and the heat distortion temperature are also affected.
Preferably, the crystallization promoter is one or two of PEG-4-dilaurate, PEG 400-diethyl hexanol and tribenzyl allyl ether hexanol. The crystallization promoter is mostly micromolecular liquid, and mainly enters a PET molecular chain to unfreeze a chain segment of the PET molecular chain, so that the moving capability of the PET chain segment is improved, the crystallization of PET is facilitated, and the crystallization of PET is more complete.
Preferably, the nucleating agent is a mixture of chemical alkali metal salt and talcum powder, and the ratio is 0.5: 1-2: 1. The talc powder is preferably of a type having more than 3000 meshes, and a larger mesh is more favorable for heterogeneous nucleation.
Preferably, the chemical alkali metal salt is at least one of sodium montanate, ethylene methacrylic acid ionomer (Surlyn), and vinyl acrylic acid ionomer (Aclyn).
Preferably, the toughening agent is at least one of ethylene-acrylate-glycidyl methacrylate, ethylene-octene-glycidyl methacrylate, and ethylene-octene-g-maleic anhydride.
Preferably, the other auxiliaries include antioxidants and lubricants.
The antioxidant is selected from a compound consisting of antioxidant 1010 and antioxidant 168 according to the weight ratio of 1: 1;
preferably, the lubricant is selected from at least one of calcium stearate, ethylene bis stearamide and silicone powder.
The invention also discloses a preparation method of the glass fiber reinforced PET composition with rapid crystallization, which comprises the following steps:
1) uniformly mixing PET and PET-PEG resin raw materials with a crystallization promoter, and then adding powder except glass fibers to continuously mix to obtain a mixed material;
2) feeding the mixed material through a main feeding port of a double-screw extruder, adding a reinforcing component from a side feeding port of the double-screw extruder, and performing extrusion, granulation and drying to obtain the rapidly-crystallized glass fiber reinforced PET composition, wherein the temperature of each temperature zone of the double-screw extruder from feeding to extrusion discharging is set as follows: a first area: 220-250 ℃ and two to nine zones: 270-220 ℃ and die head: at 260 ℃.
Compared with the prior art, the invention has the following advantages:
the invention provides a glass fiber reinforced PET composition with rapid crystallization, which adopts a PET-PEG segmented copolymer to improve the molecular chain flexibility of a PET polymer, thereby improving the crystallization performance of a polymer material. On the other hand, the long soft segment of PEG can also improve the notch impact toughness of the modified polymer to a certain extent. Compared with the traditional glass fiber reinforced PET material modified by adding a nucleating agent or compounding the nucleating agent and a crystallization accelerator, the modified glass fiber reinforced PET material disclosed by the invention is faster in crystallization, and has a shorter molding injection molding period and higher notch impact toughness.
Detailed Description
In each embodiment of the invention, the following brands of raw materials are specifically selected:
the PET resin selects medium petrochemical characterized chemical fiber FG600 grade, and the intrinsic viscosity is 0.68 dL/g; and the PET resin containing isophthalic acid (IPA) is selected as three-chamber PET 318.
The PBT resin selects medium petrochemical characterized chemical fiber L1075, and the intrinsic viscosity is 0.75 dL/g.
PET-PEG self-preparation: mixing PTA and EG according to a certain proportion, adopting antimony acetate as a catalyst, carrying out esterification reaction at the temperature of 250 +/-10 ℃, then adding PEG into a reaction product BHET for polycondensation reaction, adopting antimony trioxide as a catalyst, and finally preparing the PET-PEG block copolymer at the reaction temperature of 280 +/-10 ℃.
The glass fiber is alkali-free chopped glass fiber ECS303-3-H produced by Chongqing International composite materials GmbH, and is prepared by chopping long fiber processed by silane coupling agent and special impregnating compound, wherein the length of the glass fiber is 3.0mm, and the diameter of the glass fiber is 13 μm.
The crystallization accelerator is PX520 or Tegmer809 (Hallstar) in the chemical industry of the three-synthesis.
The nucleating agent is a compound of 10000 meshes of talcum powder 3CA and Surlyn8920 from IMERYS company, and the ratio of the talcum powder to the Surlyn is 1: 1.
The toughening agent is PTW of DuPont or BF-E of Sumitomo.
The antioxidant is a compound of antioxidant 1010 and antioxidant 168, and the weight ratio of the antioxidant to the antioxidant is 1: 1.
The lubricant is a compound of calcium stearate and silicone powder, and the weight ratio is 1: 2.
The present invention is specifically described below by way of examples, but the technical scope of the present invention is not limited to these examples. In the present invention, unless otherwise specified, parts are parts by weight.
Examples 1 to 4 and comparative examples 1 to 4
Embodiments 1 to 4 relate to a glass fiber reinforced PET composition with rapid crystallization, wherein the composite material comprises the following components in percentage by weight as shown in table 1:
the preparation method of the comparative examples 1 to 4 is the same as that of the examples, and the raw material components and the proportions are also shown in the following table 1:
TABLE 1
| Material | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| PET FG600 | 63.4 | 58.4 | 53.4 | 43.4 | 0 | 64.2 | 49.2 | 0 |
| PET 318 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 43.4 |
| PBT | 0 | 0 | 0 | 0 | 66.2 | 0 | 0 | 0 |
| PET-PEG | 0 | 5 | 10 | 20 | 0 | 0 | 15 | 20 |
| Glass fiber | 30 | 30 | 30 | 30 | 30 | 30 | 30 | 30 |
| Crystallization accelerator | 0.8 | 0.8 | 0.8 | 0.8 | 0 | 0 | 0 | 0.8 |
| Nucleating agent | 2 | 2 | 2 | 2 | 0 | 2 | 2 | 2 |
| Toughening agent | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 |
| Antioxidant agent | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
| Lubricant agent | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
The preparation method of the embodiment 1-4 is as follows: uniformly mixing PET and PET-PEG resin raw materials with a crystallization promoter, and then adding powder except glass fibers to continuously mix to obtain a mixed material; and then feeding the mixed material through a main feeding port of a double-screw extruder, adding a reinforcing component from a side feeding port of the double-screw extruder, and carrying out extrusion, granulation and drying to obtain the glass fiber reinforced PET composition with rapid crystallization.
The temperature of each temperature zone from feeding to extruding and discharging of the double-screw extruder is set as follows: a first area: 245 ℃ and a second zone: 270 ℃ and three zones: 270 ℃ and four zones: 250 ℃ and five regions: 230 ℃ and six zones: 230 ℃ and seven regions: 220 ℃ and eight regions: 220 ℃ and nine zones: 220 ℃ and die head: and the screw rotating speed of the double-screw extruder is 350-450 rpm at 260 ℃.
The test method comprises the following steps:
physical and mechanical properties: the tensile property test refers to GB/T1040.2-2006 standard, and the tensile rate is 5 mm/min; the bending property test refers to the GB/T9341-2008 standard, and the bending speed is 2 mm/min; the impact performance test refers to the GB/T1043.1-2008 standard; the heat distortion temperature (1.80MPa) is referred to GB/T1634.2-2004 standard.
Evaluation of molding cycle of the material: and (3) performing injection molding on the prepared material on an injection molding machine (the injection molding temperature is 275 ℃, 270 ℃ and 250 ℃) to obtain a conventional physical mechanical tensile sample strip, adjusting the mold temperature to 90 ℃, adjusting the cooling time until normal and stable injection molding can be performed, and counting the average injection molding period of 30 molds.
The cold crystallization peak of the material was obtained by DSC curve.
The properties of the products prepared in the examples and comparative examples are shown in Table 2 below.
TABLE 2
| Material properties | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Tensile strength Mpa | 158 | 153 | 147 | 138 | 132 | 115 | 132 | 146 |
| Flexural strength Mpa | 252 | 245 | 238 | 210 | 214 | 158 | 203 | 202 |
| Impact strength KJ/m of simply supported beam gap 2 | 9 | 11 | 13 | 15 | 9 | 8 | 10 | 16 |
| Thermal deformationThe temperature is 1.80MPa | 189 | 216 | 228 | 205 | 202 | 101 | 194 | 178 |
| Cold crystallization Peak deg.C | 103.2 | / | / | / | / | 124.8 | 114.5 | 118.3 |
| Molding cycle s | 17.4 | 15.8 | 15.3 | 16.3 | 14.8 | 26.9 | 19.6 | 22.8 |
As can be seen from the above table, the invention preferably selects proper PET and PET-PEG resin, crystallization accelerator, nucleating agent, toughening agent and the like, and obtains a glass fiber reinforced PET composition with rapid crystallization; the modified PET material has excellent physical mechanical property and heat resistance. Particularly, with the increase of the adding proportion of the PET-PEG, the impact performance of the material is improved, and meanwhile, the cold crystallization peak of the PET material disappears, so that the crystallization performance of the PET material is improved by adding the PET-PEG, and the molding period of the material is also greatly improved; meanwhile, as the content of PET-PEG is increased, the tensile strength of the material is gradually reduced, which may be related to the increase of the chain flexibility of the polymer due to the introduction of PEG groups on the molecular chain of the polymer. As can be seen by comparing examples 2-3 with comparative examples 1-2, the molding cycle of the material is obviously shortened after the PET-PEG is added into the modified glass fiber reinforced PET, and is basically close to that of the PBT material. As can be seen from the comparison of the example 1 and the comparative examples 2 to 3, the crystallization promoter and the PET-PEG can better improve the crystallization performance of the PET material, and after the two substances are added, the crystallization performance of the PET material is improved to a certain extent, the thermal deformation temperature is obviously increased, and the material molding injection molding period is obviously reduced. Comparative example 4 using a PET resin containing isophthalic acid, the heat distortion temperature and molding cycle were inferior to those of example 4, and it was found that isophthalic acid had a large influence on the nucleation effect of PET crystals.
Claims (8)
1. The glass fiber reinforced PET composition with rapid crystallization is characterized by comprising the following raw materials in parts by weight of 100:
25-75 parts of PET resin;
0-20 parts of PET-PEG block copolymer;
20-45 parts of glass fiber;
0.3-2 parts of a crystallization promoter;
0.5-3 parts of a nucleating agent;
2-5 parts of a toughening agent;
0.1-1.0 part of other auxiliary agents;
the glass fiber is selected from alkali-free glass fiber, and the diameter of the glass fiber is 8-15 mu m.
2. The fast-crystallizing glass fiber reinforced PET composition as claimed in claim 1, wherein the PET resin is selected from polymers without isophthalic acid (IPA), the intrinsic viscosity is preferably 0.6-1.0 dL/g, and the melting point of the material is not less than 250 ℃.
3. The fast-crystallizing glass fiber reinforced PET composition as claimed in claim 1, wherein the PET-PEG block copolymer is preferably a block copolymer with PEG molecular weight of 2000-4000 and PEG mass content of 8-15%.
4. The fast-crystallizing glass fiber reinforced PET composition as claimed in claim 1, wherein the crystallization promoter is one or two selected from PEG-4-dilaurate, PEG 400-diethylhexanol, tribenzylidesopropyl ether-bis-hexanol.
5. The fast-crystallizing glass fiber reinforced PET composition as claimed in claim 1, wherein the nucleating agent is a mixture of alkali metal salt and talc powder in a ratio of 0.5:1 to 2: 1;
the chemical alkali metal salt is at least one of sodium montanate, ethylene methacrylic acid ionomer (Surlyn) and vinyl acrylic acid ionomer (Aclyn).
6. The fast crystallizing glass fiber reinforced PET composition of claim 1, wherein the toughening agent is at least one of ethylene-acrylate-glycidyl methacrylate, ethylene-octene-glycidyl methacrylate, and ethylene-octene-g-maleic anhydride.
7. The fast crystallizing glass fiber reinforced PET composition of claim 1 wherein the other additives include antioxidants and lubricants;
the antioxidant is selected from a compound consisting of antioxidant 1010 and antioxidant 168 according to the weight ratio of 1: 1;
the lubricant is at least one selected from calcium stearate, ethylene bis stearamide and silicone powder.
8. A method for preparing the glass fiber reinforced PET composition with rapid crystallization rate according to any one of claims 1 to 7, which comprises the following steps:
1) uniformly mixing PET and PET-PEG resin raw materials with a crystallization promoter, and then adding powder except glass fibers to continuously mix to obtain a mixed material;
2) feeding the mixed material through a main feeding port of a double-screw extruder, adding a reinforcing component from a side feeding port of the double-screw extruder, extruding, granulating and drying to obtain the rapidly-crystallized glass fiber reinforced PET composition, wherein the temperature of each temperature zone from feeding to extruding and discharging of the double-screw extruder is set as follows: a first area: 220-250 ℃ and two to nine zones: 270-220 ℃ and die head: at 260 ℃.
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| CN116396591A (en) * | 2023-03-30 | 2023-07-07 | 中山市祺瑞达工程塑料实业有限公司 | Preparation method of reinforced PET material with low linear thermal expansion coefficient and anisotropy thereof and product thereof |
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