CN105482384A - High-formability PET (polyethylene terephthalate) engineering plastic and preparation method thereof - Google Patents
High-formability PET (polyethylene terephthalate) engineering plastic and preparation method thereof Download PDFInfo
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- CN105482384A CN105482384A CN201511009635.9A CN201511009635A CN105482384A CN 105482384 A CN105482384 A CN 105482384A CN 201511009635 A CN201511009635 A CN 201511009635A CN 105482384 A CN105482384 A CN 105482384A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention provides a high-formability PET (polyethylene terephthalate) engineering plastic and a preparation method thereof. The PET engineering plastic is mainly prepared from the following raw materials: 30-60 parts of PET resin, 5-35 parts of PCT (polycaprolactam) resin, 20-45 parts of glass fiber, 0.3-1.5 parts of antioxidant, 0.2-0.5 part of nucleator, 2-10 parts of toughener and 0.3-1 part of ester exchange inhibitor. The PET engineering plastic has the advantages of stable dimension and high formability, and can quickly form. The product can not easily generate cracks, and has favorable shock strength and chemical resistance. Meanwhile, the shrinkage, warpage and hydroscopicity of the product are lowered.
Description
Technical field
The present invention relates to engineering plastics technical field, PET engineering plastics particularly relating to a kind of easy-formation and preparation method thereof.
Background technology
The widespread use of plastics plays a very important role electric and electronic industrial expansion.Plastics have excellent electrical insulation capability, and the feature such as quality is light, physicochemical property stable, easy-formation processing, cost are low, are widely used as the case material of electric/electronic device and components and parts, coating material, substrate material, dielectric insulation layer material etc.In addition, in recent years along with the development of science and technology, there is plastics and the matrix material thereof of the functions such as conduction, magnetic conduction, electromagnetic shielding, also the electric and electronic material that some are traditional is replaced just gradually, widen the range of application of plastics in electric and electronic industry further, and create huge economic and social benefit.
To various different electrical and electronic product, specifically should consider from aspects such as the service requirements of product, forming process and economy and select suitable material.As the plastics that electrical and electronic product insulating material uses, electrical insulation properties (volume specific resistance, surface resistivity) and the dielectric properties (specific inductivity, dielectric loss angular factor, dielectric strength) of material mainly should be considered.Insulation engineering plastics must have high resistivity, high dielectric strength, low-k, low dielectric loss angle tangent.Various plastics are due to the difference of structure, and electrical property has very big-difference.Except electrical property, also should consider the mechanical property (intensity, modulus, elongation, hardness, wear resistance, resistance to tearing, resistance to flexing, fatigue resistance) of material, thermotolerance, ageing resistance, lower temperature resistance, radiation resistance (resistance to electron rays, gamma-rays, neutron ray), flame retardant resistance, chemical stability (erosion resistance, organic solvent resistance, wet fastness), cementability, foreign matter content etc.
When engineering plastics are for making various electric elements, for ensureing the trouble-free service of electrical equipment, require that engineering plastics have good thermotolerance.PET (polyethylene terephthalate) is important member in linear thermoplastic's polyester family.It is transparent, glossiness is high, have good weathering resistance and chemical stability, good rigidly, and thermotolerance is high, can keep excellent mechanical property in wide temperature range.PET can adopt various moulding process to be processed into goods.But because in PET main chain, oxyethyl group segment is short, its phenyl ring be connected is higher to its steric effect, and in PET crystallisation process, relate to the configuration inversion of main chain quaternary carbon atom, this process need be higher with energy, make the crystallisation process of PET resin slow, cause the problems such as injection mould temperature higher (more than 80 DEG C), molding cycle long, the easy sticking to mould of goods further, the application in engineering plastics is limited, is mainly used in fiber, bottle material and film at present.Although the basic property of PET resin is good, but there is the problems such as melt strength difference, crystallization velocity be slow, show as in PET resin melt process and very easily occur melt " trickling phenomenon ", after there is the PET resin cooling of " trickling phenomenon ", material property is low, is difficult to use as engineering plastics.Modification difficult point when PET resin is applied as engineering plastics and key improve its crystallization rate and crystallization degree, improve melt strength simultaneously, control the melt viscosity stability in preparation and fabrication process, the PET engineering plastics dimensional stability of preparation is poor, produce be full of cracks and slowly shaping, resistance to impact shock and chemical resistance poor, meanwhile, the shrinking percentage of goods, warpage and rate of moisture absorption are all higher.
Summary of the invention
In view of this, one aspect of the present invention provides a kind of PET engineering plastics of easy-formation, this PET engineering plastics dimensional stabilizing, easy-formation and can rapid shaping, goods not easily produce be full of cracks, have good resistance to impact shock and chemical resistance, meanwhile, the shrinking percentage of goods, warpage and rate of moisture absorption is reduced.
The present invention is by the following technical solutions:
PET engineering plastics for easy-formation, by mass parts, are prepared from primarily of following raw material:
PCT is poly-poly terephthalic acid 1,4-cyclohexanedimethanoester ester, PCT resin is a kind of thermoplastics of high temperature resistant, semicrystalline, not only there is the advantage of the polyester materials such as water-intake rate is lower, good stability of the dimension, resistance to chemical reagents are excellent, but also there is the good transparency and gamma ray resistant, be the thermoplastic polyester that current thermotolerance is the highest.PCT temperature limit is between 130 DEG C ~ 150 DEG C, and deflection temperature is 243 DEG C ~ 260 DEG C, the wave soldering fishplate bar during the PBT of resistance to thermal level can be replaced to produce as printed circuit board (PCB) and Reflow Soldering fishplate bar.But it is because PCT also has good toughness, thermostability, workability, chemical resistant properties and agent of low hygroscopicity, in humid conditions, very little on the impact of the mechanical property of PCT, dimensional stability and processing characteristics.PCT resin and PET resin belong to thermoplastic polyester series, and the two consistency is good; Promoter action is played in high workability and the crystallization of fast crystallization rate to PET resin of PCT resin; The second-order transition temperature (89 DEG C) of PCT resin, fusing point (280 ~ 295 DEG C) are all higher than PET resin (254 DEG C ~ 265 DEG C), processing temperature when modified PET resin is higher, high processing temperature makes system viscosity reduce, be conducive to the crystallization of acceleration PET resin simultaneously, improve the degree of crystallinity of PET thus improve and the melt strength of stabilising system, far away higher than nucleator and nucleation accelerating agent, there is not micro-nucleator or nucleation accelerating agent and be difficult to that dispersion in PET melt is difficult, problem pockety in the addition of PCT resin of the present invention; Be conducive to the adding of PCT resin improving the thermotolerance of goods, chemical proofing, dimensional stability and dielectricity, reduce the shrinking percentage of goods, warpage and water absorbability simultaneously.
Wherein, by mass parts, described raw material also comprises fire retardant 12 ~ 15 parts and lubricant 0.5 ~ 1.5 part;
Preferably, described raw material also comprises PBT resin 5 ~ 10 parts.
PBT is polybutylene terephthalate, PBT resin is similar with PET resin chemical structure, the butoxy kindliness contained in PBT molecular backbone chain is high, make PBT resin crystallization velocity fast, fluidity of molten is good, can improve melt strength and the crystallization rate of PBT resin, be used alone PBT resin modified PET resin, but after PBT resin modified PET resin, the thermotolerance of material, rigidity all significantly decline.
Wherein, by mass parts, be prepared from primarily of following raw material:
Wherein, the intrinsic viscosity of described PCT resin is 0.65 ~ 0.9, is preferably 0.72 ~ 0.85;
Preferably, described PCT resin is the binary polycondensate of terephthalic acid and Isosorbide-5-Nitrae-cyclohexanediol, or terephthalic acid, ethylene glycol, Isosorbide-5-Nitrae-cyclohexanediol terploycondensate;
Preferably, in described terploycondensate the mol ratio of Isosorbide-5-Nitrae cyclohexanediol and ethylene glycol for being not less than 2:1;
Preferably, the content of described PCT resin is no more than 40% of resin total amount.
The resistance to impact shock of improved product of the PCT resin of the terploycondensate composition of terephthalic acid, ethylene glycol, Isosorbide-5-Nitrae-cyclohexanediol, chemical resistance and mobility, dimensional stability, low-shrinkage, does not produce be full of cracks, rapid shaping, easy-formation; Ray and oxyethane can be used to carry out disinfection; Terephthalic acid, Isosorbide-5-Nitrae-cyclohexanediol binary co-condensation polymer composition PCT resin can further improve fluidity of molten, crystallization velocity and degree of crystallinity.
Wherein, described glass fibre is macrofiber and/or chopped strand, is preferably the chopped strand of 3 ~ 7mm;
Preferably, described glass fibre is through silane coupling agent process;
Preferably, the fiber diameter of described glass fibre is 5 ~ 15 μm, is preferably 9 ~ 13 μm.
The average fiber length of the glass fibre in the present invention in composition particle remains on 20 μm ~ 500 μm (after mixing), preferably 40 μm ~ 350 μm, and preferably 60 μm ~ 280 μm further.The fiber diameter of glass fibre is preferably 5 ~ 15 μm, preferably 9 ~ 15 μm.In the present invention, fiber diameter is weight average Fibre diameter.
Wherein, described oxidation inhibitor is that Hinered phenols antioxidant and phosphite ester kind antioxidant carry out composite mixture in 1:1 ~ 4 in mass ratio, and preferred mass is than 1:1.5 ~ 2;
Preferably, the preferred polynary hindered phenol such as 1010,1790 and 3114 of described Hinered phenols antioxidant, phosphite ester kind antioxidant preferably containing whorled phosphorous acid ester, such as 626,627, P-EPQ etc.
Preferably, described phosphite ester kind antioxidant structural formula is such as formula shown in I, and in formula I, R ' is alkyl and/or aryl, is preferably C1 ~ C25 alkyl and/or C6 ~ C12 aryl.
Formula I
Wherein, described fire retardant is brominated flame-retardant, halogen-free flame retardants, the mixture of a kind of in bromo-phosphorus-phosphorus-nitrogen coordinated fire-retardant agent or inorganic combustion inhibitor or at least two kinds, be preferably decabromodiphynly oxide, TDE, brominated epoxy resin, brominated polystyrene resin, P-N flame retardant, red phosphorus, antimonous oxide, the mixture of a kind of in zinc borate or magnesium hydroxide or at least two kinds, preferred brominated epoxy resin and/or brominated polystyrene resin further, further be preferably brominated flame-retardant and inorganic combustion inhibitor in mass ratio for 3-4:1 carries out composite mixture.
Wherein, described toughner is the mixture of a kind of in styrene analog thermoplastic elastomer, anhydride modified styrene analog thermoplastic elastomer, ethylene-acrylate copolymer, ethylene-methyl acrylate-glyceryl methacrylate ternary atactic copolymer or ethylene-acrylate-maleic anhydride tercopolymer random copolymers or at least two kinds; Such as 35BA40, EBA3107,3427,3108,34035AX8900, AX8840, PTW, 4700, SEBS1901, SEBS1652, SEBS1654.
Preferably, described ester exchange inhibitor is phosphoric acid salt and/or phosphorous acid esters; Such as ESC-PGP, TPP, NaH
2pO
4.
Preferably, described ester exchange inhibitor content is 0.5 ~ 3% of PET resin and PCT resin total mass.
Wherein, the P250 of nucleator Brueggemann.
The present invention provides a kind of method preparing above-mentioned PET engineering plastics on the other hand, in preparation process, melt viscosity and melt strength are stablized, material crystalline speed significantly improves, crystallization degree is perfect, overcome " trickling " drawback common in general PET resin processing, improve Drawing abillity and product properties, the PET engineering plastics made have good resistance to impact shock and chemical resistance, dimensional stability, easy-formation and can rapid shaping, goods not easily produce be full of cracks, meanwhile, reduce the shrinking percentage of goods, warpage and moisture absorption.
Prepare a method for above-mentioned PET engineering plastics, comprise the following steps:
(1) PET resin, PCT resin, optionally PBT resin, oxidation inhibitor, nucleator, toughner, optionally lubricant and ester exchange inhibitor are mixed by formula ratio, obtain mixture;
(2) described mixture and glass fibre are put in forcing machine by formula ratio, add optionally fire retardant during melt blending, and carry out extruding pelletization, obtained PET engineering plastics.
Wherein, in step (2), the Heating temperature of described forcing machine is as follows: 160 ~ 220 DEG C, a district, 210 ~ 240 DEG C, 2nd district, 230 ~ 270 DEG C, 3rd district, 230 ~ 280 DEG C, 4th district, 230 ~ 270 DEG C, 5th district, 230 ~ 270 DEG C, 6th district and head 240 ~ 270 DEG C.
Compared with prior art, beneficial effect of the present invention: PCT resin and PET resin belong to thermoplastic polyester series, the two consistency is good, in PET engineering plastics preparation process of the present invention, promoter action is played in the high workability of PCT resin and the crystallization of fast crystallization rate to PET resin, the second-order transition temperature (89 DEG C) of PCT resin, fusing point (280 ~ 295 DEG C) is all higher than PET resin (254 DEG C ~ 265 DEG C), processing temperature when modified PET resin is higher, high processing temperature makes system viscosity reduce, be conducive to the crystallization accelerating PET resin simultaneously, improve the degree of crystallinity of PET thus improve and the melt strength of stabilising system, the addition of PCT resin is far away higher than nucleator and nucleation accelerating agent, there is not micro-nucleator or nucleation accelerating agent, to be difficult to dispersion in PET melt difficult, problem pockety, melt viscosity of the present invention and melt strength are stablized, material crystalline speed significantly improves, crystallization degree is perfect, overcome " trickling " drawback common in general PET resin processing, improve Drawing abillity and product properties, the PET engineering plastics dimensional stabilizing made, easy-formation and can rapid shaping, goods not easily produce be full of cracks, there is good resistance to impact shock and chemical resistance, simultaneously, reduce the shrinking percentage of goods, warpage and rate of moisture absorption.
Embodiment
Further illustrate technical scheme of the present invention respectively below in conjunction with the embodiments.
Embodiment 1: the PET engineering plastics of the present embodiment, by mass parts, comprises following component:
PET resin, PCT resin, oxidation inhibitor, nucleator, toughner, lubricant and ester exchange inhibitor are mixed by formula ratio, obtains mixture;
(2) described mixture and glass fibre are put in forcing machine by formula ratio, add fire retardant by formula ratio during melt blending, and carry out extruding pelletization, obtained PET engineering plastics.
Wherein, the Heating temperature of forcing machine is as follows: 160 ~ 220 DEG C, a district, 210 ~ 240 DEG C, 2nd district, 230 ~ 270 DEG C, 3rd district, 230 ~ 280 DEG C, 4th district, 230 ~ 270 DEG C, 5th district, 230 ~ 270 DEG C, 6th district and head 240 ~ 270 DEG C.
According to the preparation method of embodiment 1, the PET engineering plastics of preparation embodiment 2 ~ 4 and comparative example 1 ~ 4, its component (by mass parts) is as shown in table 1:
Table 1
Performance test: the PET engineering plastics prepared in embodiment 1 ~ 4 and comparative example 1 ~ 3 are carried out test result as following table according to testing standard:
Table 2
Embodiment 1: compared with comparative example 1, is added with PCT resin in embodiment 1, thermotolerance, the rigidity of obtained PET engineering plastics significantly improve, and product surface warpage, rate of moisture absorption, contractibility obviously reduce, and CTI is high, and electrical property is excellent; Compared with the civilian example 2 of contrast, ester exchange inhibitor is added with in embodiment 1, prevent PET/PCT resin excessively carry out in melt-processed process transesterification reaction impact even destroy the crystallization velocity of PET and PCT and percent crystallization in massecuite so that cause product properties significantly to decline functional, obtained PET resin excellent performance.
Embodiment 2: compared with embodiment 1, embodiment 2 carries out further optimization process to each component concentration, contributes to the performance improving PET engineering plastics further, and thermotolerance and the rigidity of goods improve further, and rate of moisture absorption and shrinking percentage are reduced further; PBT resin modified PET resin is used alone in comparative example 4, but the thermotolerance of material, rigidity all significantly decline after PBT resin modified PET resin, compared with comparative example 4, embodiment 2 uses PCT resin to replace PBT resin, be conducive to the thermotolerance of raising goods, chemical proofing, dimensional stability and dielectricity, reduce the shrinking percentage of goods, warpage and water absorbability simultaneously;
Embodiment 3: compared with embodiment 2, the component of the oxidation inhibitor in embodiment 3, fire retardant and toughner and proportioning thereof are carried out further preferably, make the over-all properties of PET engineering plastics more excellent;
Embodiment 4: compared with contrast literary composition 2, on PCT basis, add PBT resin in embodiment 4 more jointly modification is carried out to PET resin, found that the thermotolerance of PET engineering plastics, chemical proofing, dimensional stability and dielectricity are further enhanced, reduce the shrinking percentage of goods, warpage and water absorbability simultaneously further, overcome the problem that the independent modified PET resin of PBT resin causes thermotolerance and rigidity all significantly to decline.
It should be noted that and understand, when not departing from the spirit and scope of accompanying claim the present invention for required protection, various amendment and improvement can be made to the present invention of foregoing detailed description.Therefore, the scope of claimed technical scheme is not by the restriction of given any specific exemplary teachings.
Applicant states, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, namely do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (10)
1. PET engineering plastics for easy-formation, is characterized in that, by mass parts, are prepared from primarily of following raw material:
2. PET engineering plastics according to claim 1, is characterized in that, by mass parts, described raw material also comprises fire retardant 12 ~ 15 parts, lubricant 0.5 ~ 1.5 part and PBT resin 5 ~ 10 parts.
3. PET engineering plastics according to claim 1 and 2, is characterized in that, by mass parts, are prepared from primarily of following raw material:
4. according to the PET engineering plastics one of claims 1 to 3 Suo Shu, it is characterized in that, the intrinsic viscosity of described PCT resin is 0.65 ~ 0.9, is preferably 0.72 ~ 0.85;
Preferably, described PCT resin is the binary polycondensate of terephthalic acid and Isosorbide-5-Nitrae-cyclohexanediol, or phthalic acid, ethylene glycol, Isosorbide-5-Nitrae-cyclohexanediol terploycondensate;
Preferably, in described terploycondensate the mol ratio of Isosorbide-5-Nitrae cyclohexanediol and ethylene glycol for being not less than 2:1;
Preferably, the content of described PCT resin is no more than 40% of resin total amount.
5. according to the PET engineering plastics one of Claims 1-4 Suo Shu, it is characterized in that, described glass fibre is macrofiber and/or chopped strand, is preferably the chopped strand of 3 ~ 7mm;
Preferably, described glass fibre is through silane coupling agent process;
Preferably, the fiber diameter of described glass fibre is 5 ~ 15 μm, is preferably 9 ~ 13 μm.
6. according to the PET engineering plastics one of claim 1 to 5 Suo Shu, it is characterized in that, described oxidation inhibitor is that Hinered phenols antioxidant and phosphite ester kind antioxidant carry out composite mixture in 1:1 ~ 4 in mass ratio, is preferably mass ratio 1:1.5 ~ 2;
Preferably, described Hinered phenols antioxidant is polynary Hinered phenols antioxidant, and described phosphite ester kind antioxidant is for containing whorled phosphite ester kind antioxidant;
Preferably, described phosphite ester kind antioxidant structural formula is such as formula shown in I, and in formula I, R ' is alkyl and/or aryl, is preferably C1 ~ C25 alkyl and/or C6 ~ C12 aryl;
7. according to the PET engineering plastics one of claim 1 to 6 Suo Shu, it is characterized in that, described fire retardant is brominated flame-retardant, halogen-free flame retardants, the mixture of a kind of in bromo-phosphorus-phosphorus-nitrogen coordinated fire-retardant agent or inorganic combustion inhibitor or at least two kinds, be preferably decabromodiphynly oxide, TDE, brominated epoxy resin, brominated polystyrene resin, P-N flame retardant, red phosphorus, antimonous oxide, the mixture of a kind of in zinc borate or magnesium hydroxide or at least two kinds, preferred brominated epoxy resin and/or brominated polystyrene resin further, further be preferably brominated flame-retardant and inorganic combustion inhibitor in mass ratio for 3-4:1 carries out composite mixture.
8. according to the PET engineering plastics one of claim 1 to 7 Suo Shu, it is characterized in that, described toughner is the mixture of a kind of in styrene analog thermoplastic elastomer, anhydride modified styrene analog thermoplastic elastomer, ethylene-acrylate copolymer, ethylene-methyl acrylate-glyceryl methacrylate ternary atactic copolymer or ethylene-acrylate-maleic anhydride tercopolymer random copolymers or at least two kinds;
Preferably, described ester exchange inhibitor is phosphoric acid salt and/or phosphorous acid esters;
Preferably, described ester exchange inhibitor content is 0.5 ~ 3% of PET resin and PCT resin total mass.
9. prepare a method for the described PET engineering plastics of one of claim 1 ~ 8, it is characterized in that, comprise the following steps:
(1) PET resin, PCT resin, optionally PBT resin, oxidation inhibitor, nucleator, toughner, optionally lubricant and ester exchange inhibitor are mixed by formula ratio, obtain mixture;
(2) described mixture and glass fibre are put in forcing machine, during melt blending and the fire retardant added optionally, and carry out extruding pelletization, obtained PET engineering plastics.
10. preparation method according to claim 9, it is characterized in that, in step (2), the Heating temperature of described forcing machine is as follows: 160 ~ 220 DEG C, a district, 210 ~ 240 DEG C, 2nd district, 230 ~ 270 DEG C, 3rd district, 230 ~ 280 DEG C, 4th district, 230 ~ 270 DEG C, 5th district, 230 ~ 270 DEG C, 6th district and head 240 ~ 270 DEG C.
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CN106755617A (en) * | 2017-01-12 | 2017-05-31 | 东莞市天熠皮业科技股份有限公司 | A kind of utilization scrap leather material is processed into the production technology of the matte cladding with silky handle |
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Application publication date: 20160413 |