CN113604014A - High-weather-resistance high-rigidity glass fiber reinforced PBT (polybutylene terephthalate) -PET (polyethylene terephthalate) alloy modified material - Google Patents
High-weather-resistance high-rigidity glass fiber reinforced PBT (polybutylene terephthalate) -PET (polyethylene terephthalate) alloy modified material Download PDFInfo
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- 239000003365 glass fiber Substances 0.000 title claims abstract description 91
- 239000000463 material Substances 0.000 title claims abstract description 81
- 239000000956 alloy Substances 0.000 title claims abstract description 76
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 72
- 229920001707 polybutylene terephthalate Polymers 0.000 title description 83
- 229920000139 polyethylene terephthalate Polymers 0.000 title description 83
- 239000005020 polyethylene terephthalate Substances 0.000 title description 83
- -1 polybutylene terephthalate Polymers 0.000 title description 7
- 239000002131 composite material Substances 0.000 claims abstract description 94
- 239000000835 fiber Substances 0.000 claims abstract description 55
- 239000003607 modifier Substances 0.000 claims abstract description 37
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 37
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 36
- 239000011521 glass Substances 0.000 claims abstract description 28
- 239000003112 inhibitor Substances 0.000 claims abstract description 26
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 22
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000011324 bead Substances 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 16
- 239000004952 Polyamide Substances 0.000 claims abstract description 14
- 229920002647 polyamide Polymers 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims description 26
- 150000002148 esters Chemical group 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 24
- 238000009210 therapy by ultrasound Methods 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 18
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 15
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 15
- 239000000498 cooling water Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 229920005575 poly(amic acid) Polymers 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 11
- 239000011325 microbead Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 4
- 239000005357 flat glass Substances 0.000 claims description 4
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 4
- 235000010234 sodium benzoate Nutrition 0.000 claims description 4
- 239000004299 sodium benzoate Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000004642 Polyimide Substances 0.000 abstract description 11
- 229920001721 polyimide Polymers 0.000 abstract description 11
- 230000032683 aging Effects 0.000 abstract description 8
- 238000005452 bending Methods 0.000 abstract description 6
- 238000004140 cleaning Methods 0.000 abstract description 3
- 125000004185 ester group Chemical group 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 5
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- 208000012886 Vertigo Diseases 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 229920006351 engineering plastic Polymers 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/046—Reinforcing macromolecular compounds with loose or coherent fibrous material with synthetic macromolecular fibrous material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
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- C08J5/047—Reinforcing macromolecular compounds with loose or coherent fibrous material with mixed fibrous material
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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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- C—CHEMISTRY; METALLURGY
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- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2479/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C08K3/22—Oxides; Hydroxides of metals
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Abstract
The invention discloses a high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material, and particularly relates to the technical field of PBT/PET alloy materials, which comprises the following steps: PBT slice, PET slice, glass fiber, ester exchange inhibitor and composite modifier. The invention can effectively improve the aging resistance, tensile strength, bending strength and bending modulus of the PBT and PET alloy modified material, can effectively ensure that the alloy modified material is used outdoors for a long time, and has better applicability; electrostatic spinning and imidization treatment are carried out to prepare the nano silicon carbide/polyimide composite fiber, and the nano titanium dioxide can be compounded into the hollow glass beads and the nano silicon carbide/polyamide acid composite fiber, so that the aging resistance and the self-cleaning performance of the composite modified fiber can be effectively enhanced; the nano silicon carbide/polyamide acid composite fiber can be loaded outside the hollow glass bead, so that the structural strength and stability of the PBT and PET alloy modified material are further enhanced.
Description
Technical Field
The invention relates to the technical field of PBT/PET alloy materials, in particular to a high-weather-resistance high-rigidity glass fiber reinforced PBT and PET alloy modified material.
Background
Polyethylene terephthalate (PET) and polybutylene terephthalate (PBT) are polymers with excellent comprehensive performance and low cost, and have wide application in the field of engineering plastics. At present, the alloy modified material prepared by using blending extrusion equipment has become the modification trend of PBT/PET and is widely applied. Meanwhile, the glass fiber is used for reinforcing in the PBT/PET, so that the performance of the alloy material can be improved. The PET/PBT alloy (polyethylene terephthalate/polybutylene terephthalate) is an engineering plastic with excellent comprehensive performance, has the characteristics of high temperature resistance, moisture resistance, chemical corrosion resistance, good electrical insulation performance, good elasticity and the like, can keep good mechanical properties in a wider temperature range, has wide application in national economy and high and new technology industries, and is an indispensable novel material. However, the greatest defects of PET/PBT alloy are high notch sensitivity, low notch impact strength, low thermal deformation temperature and large shrinkage rate, thereby greatly limiting the application of the PET/PBT alloy. Therefore, the PET/PBT alloy needs to be subjected to reinforcing, toughening and modifying.
The existing PBT and PET alloy material has poor weather resistance, is not suitable for being used outdoors for a long time and is easy to damage.
Disclosure of Invention
In order to overcome the above defects in the prior art, embodiments of the present invention provide a high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material.
A high-weather-resistance high-rigidity glass fiber reinforced PBT and PET alloy modified material comprises the following components in percentage by weight: 54.60-55.80% of PBT slices, 9.70-10.50% of PET slices, 23.80-24.60% of glass fibers, 0.30-0.50% of ester exchange inhibitor and the balance of composite modifier.
Further, the composite modifier comprises the following components in percentage by weight: 5.80-6.60% of nano silicon carbide, 14.90-15.50% of polyamide acid, 8.60-9.60% of nano titanium dioxide, 30.60-31.20% of hollow glass beads, 1.60-2.20% of sodium dodecyl benzene sulfonate and the balance of deionized water.
Further, the paint comprises the following components in percentage by weight: 54.60% of PBT slice, 9.70% of PET slice, 23.80% of glass fiber, 0.30% of ester exchange inhibitor and 11.60% of composite modifier; the composite modifier comprises the following components in percentage by weight: 5.80 percent of nano silicon carbide, 14.90 percent of polyamic acid, 8.60 percent of nano titanium dioxide, 30.60 percent of hollow glass micro-beads, 1.60 percent of sodium dodecyl benzene sulfonate and 38.50 percent of deionized water.
Further, the paint comprises the following components in percentage by weight: 55.80 percent of PBT slice, 10.50 percent of PET slice, 24.60 percent of glass fiber, 0.50 percent of ester exchange inhibitor and 8.60 percent of composite modifier; the composite modifier comprises the following components in percentage by weight: 6.60 percent of nano silicon carbide, 15.50 percent of polyamic acid, 9.60 percent of nano titanium dioxide, 31.20 percent of hollow glass micro-beads, 2.20 percent of sodium dodecyl benzene sulfonate and 34.90 percent of deionized water.
Further, the paint comprises the following components in percentage by weight: 55.20 percent of PBT slice, 10.10 percent of PET slice, 24.20 percent of glass fiber, 0.40 percent of ester exchange inhibitor and 10.10 percent of composite modifier; the composite modifier comprises the following components in percentage by weight: 6.20 percent of nano silicon carbide, 15.20 percent of polyamic acid, 9.10 percent of nano titanium dioxide, 30.90 percent of hollow glass micro-beads, 1.90 percent of sodium dodecyl benzene sulfonate and 36.70 percent of deionized water.
Further, the ester exchange inhibitor is one or two of sodium benzoate and disodium hydrogen phosphate, the viscosity of the PBT slice is 0.9-1.1, the water content is 0.25-0.5%, and the content of terminal shrinking group is less than or equal to 20 mol/t; the viscosity of the PET slice is 0.7-0.9, the water content is 0.25-0.5%, and the end shrinking base content is 30 +/-5 mol/t; the glass fiber is one or two of flat glass fiber or short glass fiber, and the diameter of the glass fiber is 10-13 mu m.
The invention also provides a preparation method of the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material, which comprises the following specific preparation steps:
the method comprises the following steps: weighing the PBT slice, the PET slice, the glass fiber, the ester exchange inhibitor and the composite modifier in parts by weight;
step two: mixing the composite modifier in the step one, heating to 70-80 ℃, and carrying out ultrasonic treatment for 20-30 minutes to obtain a mixture A;
step three: performing electrostatic spinning on the mixture A prepared in the step two to obtain composite fibers, and performing thermal imidization treatment on the composite modified fibers to obtain composite modified fibers;
step four: blending the PBT slice, the PET slice, the ester exchange inhibitor and the two-thirds weight part composite modified fiber prepared in the step three to obtain a mixture B;
step five: blending the glass fiber obtained in the step one and the residual composite modified fiber obtained in the step three to obtain a mixture C;
step five: putting the mixture B prepared in the fourth step into a double-screw extruder, and adding the mixture C prepared in the fifth step into the double-screw extruder from a side feed;
step six: after the extruder discharges materials, the materials enter a cooling water tank for cooling, then enter a granulator for granulating, and enter a homogenizing bin after being screened by a vibrating screen, so that the high-weather-resistance and high-rigidity glass fiber reinforced PBT and PET alloy modified material is prepared.
Further, in the second step, the ultrasonic treatment frequency is 23-27 KHz, and the ultrasonic treatment power is 1200-1800W; in the third step, in the electrostatic spinning process, 14-18 KV high voltage is applied, the distance between a capillary nozzle of the injector and a grounded receiving device is 13-15 cm, and the thermal imidization treatment temperature is 200-300 ℃; in step five, the twin screw extruder temperature is set to a zone: 240-260 ℃, the temperature of the second zone is 240-260 ℃, the temperature of the third zone is 240-250 ℃, the temperature of the fourth zone is 235-245 ℃, the temperature of the fifth zone is 225-235 ℃, the temperature of the sixth zone is 225-235 ℃, the temperature of the seventh zone is 225-235 ℃, the temperature of the eighth zone is 225-235 ℃, and the temperature of the ninth zone is 230-240 ℃; in the sixth step, the temperature of the cooling water tank is 24-26 ℃, and the rotating speed of the granulator is 800-1100 r/min.
Further, in the second step, the ultrasonic treatment frequency is 23KHz, and the ultrasonic treatment power is 1200W; in the third step, in the electrostatic spinning process, 14KV high voltage is applied, the distance between a capillary nozzle of the injector and a grounded receiving device is 13cm, and the thermal imidization treatment temperature is 200 ℃; in step five, the twin screw extruder temperature is set to a zone: 240 ℃, 240 ℃ of the temperature of the second zone, 240 ℃ of the temperature of the third zone, 235 ℃ of the temperature of the fourth zone, 225 ℃ of the temperature of the fifth zone, 225 ℃ of the temperature of the sixth zone, 225 ℃ of the temperature of the seventh zone, 225 ℃ of the temperature of the eighth zone and 230 ℃ of the temperature of the ninth zone; in the sixth step, the temperature of the cooling water tank is 24 ℃, and the rotating speed of the granulator is 800 r/min.
Further, in the second step, the ultrasonic treatment frequency is 25KHz, and the ultrasonic treatment power is 1500W; in the third step, 16KV high voltage is applied in the electrostatic spinning process, the distance between a capillary nozzle of the injector and a grounded receiving device is 14cm, and the thermal imidization treatment temperature is 250 ℃; in step five, the twin screw extruder temperature is set to a zone: 250 ℃, 250 ℃ of the temperature of the second zone, 245 ℃ of the temperature of the third zone, 240 ℃ of the temperature of the fourth zone, 230 ℃ of the temperature of the fifth zone, 230 ℃ of the temperature of the sixth zone, 230 ℃ of the temperature of the seventh zone, 230 ℃ of the temperature of the eighth zone and 235 ℃ of the temperature of the ninth zone; in the sixth step, the temperature of the cooling water tank is 25 ℃, and the rotating speed of the granulator is 900 r/min.
The invention has the technical effects and advantages that:
1. the high-weather-resistance high-rigidity glass fiber reinforced PBT and PET alloy modified material prepared by the raw material formula can effectively improve the aging resistance, tensile strength, bending strength and bending modulus of the PBT and PET alloy modified material, can effectively ensure that the PBT and PET alloy modified material is used outdoors for a long time, and has better applicability; the nano silicon carbide and the polyamide acid in the formula are blended to prepare spinning solution, then electrostatic spinning is carried out to prepare nano silicon carbide/polyamide acid composite fiber, then imidization treatment is carried out to obtain the nano silicon carbide/polyimide composite fiber, and meanwhile, in the process of electrostatic spinning, the nano titanium dioxide can be compounded into the hollow glass beads and the nano silicon carbide/polyamide acid composite fiber, so that the aging resistance and the self-cleaning performance of the composite modified fiber can be effectively enhanced; the hollow glass beads are used as a supporting framework, the nano silicon carbide/polyamide acid composite fiber can be loaded to the outside of the hollow glass beads in the synthesis process, and the composite modified fiber based on the hollow glass beads can be quickly combined with the glass fiber in the main material, so that the structural strength and the stability of the PBT and PET alloy modified material are further enhanced;
2. in the process of preparing the high-weather-resistance high-rigidity glass fiber reinforced PBT and PET alloy modified material, in the second step, the composite modification is subjected to mixed heating and ultrasonic treatment, so that the composite effect of the raw materials in the composite modifier can be effectively enhanced, the contact and combination effect of the raw materials is better, and the rapid reaction of the raw materials is ensured; in the third step, the mixture A is subjected to electrostatic spinning treatment and then imidization treatment, so that raw materials can be effectively subjected to composite treatment to synthesize nano silicon carbide/polyimide composite fibers, nano titanium dioxide is compounded into the nano silicon carbide/polyimide composite fibers and hollow glass beads, and the nano silicon carbide/polyimide composite fibers are supported by the hollow glass beads; in the fourth step, part of the composite modified fibers are blended with other raw materials, and in the fifth step, the rest composite modified fibers and the glass fibers are blended, so that the distribution uniformity and stability of the composite modified fibers in the PBT and PET alloy modified material can be effectively enhanced.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material, which comprises the following components in percentage by weight: 54.60% of PBT slice, 9.70% of PET slice, 23.80% of glass fiber, 0.30% of ester exchange inhibitor and 11.60% of composite modifier; the composite modifier comprises the following components in percentage by weight: 5.80 percent of nano silicon carbide, 14.90 percent of polyamic acid, 8.60 percent of nano titanium dioxide, 30.60 percent of hollow glass micro-beads, 1.60 percent of sodium dodecyl benzene sulfonate and 38.50 percent of deionized water;
the ester exchange inhibitor is one or two of sodium benzoate or disodium hydrogen phosphate, the viscosity of the PBT slice is 0.9, the water content is 0.25%, and the end shrinking group content is less than or equal to 20 mol/t; the viscosity of the PET slice is 0.7, the water content is 0.25%, and the end-shrinking base content is 30 +/-5 mol/t; the glass fiber is one or two of flat glass fiber or chopped glass fiber, and the diameter of the glass fiber is 10 mu m;
the invention also provides a preparation method of the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material, which comprises the following specific preparation steps:
the method comprises the following steps: weighing the PBT slice, the PET slice, the glass fiber, the ester exchange inhibitor and the composite modifier in parts by weight;
step two: mixing the composite modifier in the step one, heating to 70 ℃, and carrying out ultrasonic treatment for 20 minutes to obtain a mixture A;
step three: performing electrostatic spinning on the mixture A prepared in the step two to obtain composite fibers, and performing thermal imidization treatment on the composite modified fibers to obtain composite modified fibers;
step four: blending the PBT slice, the PET slice, the ester exchange inhibitor and the two-thirds weight part composite modified fiber prepared in the step three to obtain a mixture B;
step five: blending the glass fiber obtained in the step one and the residual composite modified fiber obtained in the step three to obtain a mixture C;
step five: putting the mixture B prepared in the fourth step into a double-screw extruder, and adding the mixture C prepared in the fifth step into the double-screw extruder from a side feed;
step six: after the extruder discharges materials, the materials enter a cooling water tank for cooling, then enter a granulator for granulating, and enter a homogenizing bin after being screened by a vibrating screen, so that the high-weather-resistance and high-rigidity glass fiber reinforced PBT and PET alloy modified material is prepared.
In the second step, the ultrasonic treatment frequency is 23KHz, and the ultrasonic treatment power is 1200W; in the third step, in the electrostatic spinning process, 14KV high voltage is applied, the distance between a capillary nozzle of the injector and a grounded receiving device is 13cm, and the thermal imidization treatment temperature is 200 ℃; in step five, the twin screw extruder temperature is set to a zone: 240 ℃, 240 ℃ of the temperature of the second zone, 240 ℃ of the temperature of the third zone, 235 ℃ of the temperature of the fourth zone, 225 ℃ of the temperature of the fifth zone, 225 ℃ of the temperature of the sixth zone, 225 ℃ of the temperature of the seventh zone, 225 ℃ of the temperature of the eighth zone and 230 ℃ of the temperature of the ninth zone; in the sixth step, the temperature of the cooling water tank is 24 ℃, and the rotating speed of the granulator is 800 r/min.
Example 2:
different from the embodiment 1, the material comprises the following components in percentage by weight: 55.80 percent of PBT slice, 10.50 percent of PET slice, 24.60 percent of glass fiber, 0.50 percent of ester exchange inhibitor and 8.60 percent of composite modifier; the composite modifier comprises the following components in percentage by weight: 6.60 percent of nano silicon carbide, 15.50 percent of polyamic acid, 9.60 percent of nano titanium dioxide, 31.20 percent of hollow glass micro-beads, 2.20 percent of sodium dodecyl benzene sulfonate and 34.90 percent of deionized water.
Example 3:
different from the examples 1-2, the material comprises the following components in percentage by weight: 55.20 percent of PBT slice, 10.10 percent of PET slice, 24.20 percent of glass fiber, 0.40 percent of ester exchange inhibitor and 10.10 percent of composite modifier; the composite modifier comprises the following components in percentage by weight: 6.20 percent of nano silicon carbide, 15.20 percent of polyamic acid, 9.10 percent of nano titanium dioxide, 30.90 percent of hollow glass micro-beads, 1.90 percent of sodium dodecyl benzene sulfonate and 36.70 percent of deionized water.
Taking the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material prepared in the above examples 1-3, the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of the first control group, the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of the second control group, the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of the third control group, the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of the fourth control group, and the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of the fifth control group, respectively, the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of the first control group has no nano silicon carbide compared with the examples, the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of the second control group has no polyamide acid compared with the examples, and the high weather-resistant high-rigidity reinforced PBT and PET alloy modified material of the third control group has no nano titanium dioxide compared with the examples, compared with the examples, the high-weather-resistance high-rigidity glass fiber reinforced PBT and PET alloy modified material of the control group IV does not contain hollow glass beads, compared with the examples, the high-weather-resistance high-rigidity glass fiber reinforced PBT and PET alloy modified material of the control group V does not contain sodium dodecyl benzene sulfonate, the high-weather-resistance high-rigidity glass fiber reinforced PBT and PET alloy modified material prepared in the three examples and the high-weather-resistance high-rigidity glass fiber reinforced PBT and PET alloy modified material of the five control groups are respectively tested by eight groups, and every 30 samples are taken as one group for testing; the test results are shown in table one:
table one:
as can be seen from the table I, when the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material comprises the following raw materials in proportion: comprises the following components in percentage by weight: 55.20 percent of PBT slice, 10.10 percent of PET slice, 24.20 percent of glass fiber, 0.40 percent of ester exchange inhibitor and 10.10 percent of composite modifier; the composite modifier comprises the following components in percentage by weight: when the nano silicon carbide is 6.20%, the polyamide acid is 15.20%, the nano titanium dioxide is 9.10%, the hollow glass bead is 30.90%, the sodium dodecyl benzene sulfonate is 1.90%, and the deionized water is 36.70%, the aging resistance, the tensile strength, the bending strength and the bending modulus of the high-weather-resistance high-rigidity glass fiber reinforced PBT and PET alloy modified material can be effectively improved, the long-term outdoor use of the PBT and PET alloy modified material can be effectively ensured, and the applicability is better; embodiment 3 is a preferred embodiment of the present invention, the nano silicon carbide and the polyamic acid in the formula are blended to prepare a spinning solution, then electrostatic spinning is performed to prepare a nano silicon carbide/polyamic acid composite fiber, and then imidization treatment is performed to obtain a nano silicon carbide/polyimide composite fiber, wherein the nano silicon carbide/polyimide composite fiber has the properties of silicon carbide and polyimide, so that the high strength, wear resistance, high and low temperature resistance, corrosion resistance, acid and alkali resistance and aging resistance of the PBT and PET alloy modified material can be effectively improved; meanwhile, in the electrostatic spinning process, the nano titanium dioxide can be compounded into the hollow glass beads and the nano silicon carbide/polyamide acid composite fibers in the synthesis process of the nano silicon carbide/polyamide acid composite fibers, so that the aging resistance and the self-cleaning performance of the composite modified fibers can be effectively enhanced; the hollow glass beads are used as a supporting framework, the nano silicon carbide/polyamide acid composite fiber can be loaded to the outside of the hollow glass beads in the synthesis process, and the composite modified fiber based on the hollow glass beads can be quickly combined with the glass fiber in the main material, so that the structural strength and the stability of the PBT and PET alloy modified material are further enhanced; the sodium dodecyl benzene sulfonate is used in the electrostatic spinning solution, so that the heat resistance and the flame retardant property of the nano silicon carbide/polyamide acid composite fiber can be effectively enhanced, and the heat resistance and the flame retardant property of the PBT and PET alloy modified material are further improved.
Example 4:
the invention provides a high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material, which comprises the following components in percentage by weight: 55.20 percent of PBT slice, 10.10 percent of PET slice, 24.20 percent of glass fiber, 0.40 percent of ester exchange inhibitor and 10.10 percent of composite modifier; the composite modifier comprises the following components in percentage by weight: 6.20 percent of nano silicon carbide, 15.20 percent of polyamic acid, 9.10 percent of nano titanium dioxide, 30.90 percent of hollow glass microsphere, 1.90 percent of sodium dodecyl benzene sulfonate and 36.70 percent of deionized water;
the ester exchange inhibitor is one or two of sodium benzoate or disodium hydrogen phosphate, the viscosity of the PBT slice is 1.0, the water content is 0.35 percent, and the end shrinking group content is less than or equal to 20 mol/t; the viscosity of the PET slice is 0.8, the water content is 0.35%, and the end-shrinking base content is 30 +/-5 mol/t; the glass fiber is one or two of flat glass fiber or chopped glass fiber, and the diameter of the glass fiber is 12 mu m;
the invention also provides a preparation method of the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material, which comprises the following specific preparation steps:
the method comprises the following steps: weighing the PBT slice, the PET slice, the glass fiber, the ester exchange inhibitor and the composite modifier in parts by weight;
step two: mixing the composite modifier in the step one, heating to 75 ℃, and carrying out ultrasonic treatment for 25 minutes to obtain a mixture A;
step three: performing electrostatic spinning on the mixture A prepared in the step two to obtain composite fibers, and performing thermal imidization treatment on the composite modified fibers to obtain composite modified fibers;
step four: blending the PBT slice, the PET slice, the ester exchange inhibitor and the two-thirds weight part composite modified fiber prepared in the step three to obtain a mixture B;
step five: blending the glass fiber obtained in the step one and the residual composite modified fiber obtained in the step three to obtain a mixture C;
step five: putting the mixture B prepared in the fourth step into a double-screw extruder, and adding the mixture C prepared in the fifth step into the double-screw extruder from a side feed;
step six: after the extruder discharges materials, the materials enter a cooling water tank for cooling, then enter a granulator for granulating, and enter a homogenizing bin after being screened by a vibrating screen, so that the high-weather-resistance and high-rigidity glass fiber reinforced PBT and PET alloy modified material is prepared.
In the second step, the ultrasonic treatment frequency is 23KHz, and the ultrasonic treatment power is 1200W; in the third step, in the electrostatic spinning process, 14KV high voltage is applied, the distance between a capillary nozzle of the injector and a grounded receiving device is 13cm, and the thermal imidization treatment temperature is 200 ℃; in step five, the twin screw extruder temperature is set to a zone: 240 ℃, 240 ℃ of the temperature of the second zone, 240 ℃ of the temperature of the third zone, 235 ℃ of the temperature of the fourth zone, 225 ℃ of the temperature of the fifth zone, 225 ℃ of the temperature of the sixth zone, 225 ℃ of the temperature of the seventh zone, 225 ℃ of the temperature of the eighth zone and 230 ℃ of the temperature of the ninth zone; in the sixth step, the temperature of the cooling water tank is 24 ℃, and the rotating speed of the granulator is 800 r/min.
Example 5:
different from the embodiment 4, in the second step, the ultrasonic processing frequency is 27KHz, and the ultrasonic processing power is 1800W; in the third step, in the electrostatic spinning process, 18KV high voltage is applied, the distance between a capillary nozzle of the injector and a grounded receiving device is 15cm, and the thermal imidization treatment temperature is 300 ℃; in step five, the twin screw extruder temperature is set to a zone: 260 ℃, 260 ℃ of the temperature of the second zone, 250 ℃ of the temperature of the third zone, 245 ℃ of the temperature of the fourth zone, 235 ℃ of the temperature of the fifth zone, 235 ℃ of the temperature of the sixth zone, 235 ℃ of the temperature of the seventh zone, 235 ℃ of the temperature of the eighth zone and 240 ℃ of the temperature of the ninth zone; in the sixth step, the temperature of the cooling water tank is 26 ℃, and the rotating speed of the granulator is 1100 r/min.
Example 6:
different from the embodiments 4-5, in the second step, the ultrasonic treatment frequency is 25KHz, and the ultrasonic treatment power is 1500W; in the third step, 16KV high voltage is applied in the electrostatic spinning process, the distance between a capillary nozzle of the injector and a grounded receiving device is 14cm, and the thermal imidization treatment temperature is 250 ℃; in step five, the twin screw extruder temperature is set to a zone: 250 ℃, 250 ℃ of the temperature of the second zone, 245 ℃ of the temperature of the third zone, 240 ℃ of the temperature of the fourth zone, 230 ℃ of the temperature of the fifth zone, 230 ℃ of the temperature of the sixth zone, 230 ℃ of the temperature of the seventh zone, 230 ℃ of the temperature of the eighth zone and 235 ℃ of the temperature of the ninth zone; in the sixth step, the temperature of the cooling water tank is 25 ℃, and the rotating speed of the granulator is 900 r/min.
Taking the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material prepared in the above examples 4-6, the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of the sixth control group, the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of the seventh control group, the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of the eighth control group, and the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of the ninth control group, respectively, the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of the sixth control group has no operation in step two compared with the examples, the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of the seventh control group has no operation in step three compared with the examples, the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of the eighth control group has no operation in step four compared with the examples, compared with the examples, the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of the control group nine does not have the operation in the step five, the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material prepared in the three examples and the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of the four control groups are respectively tested in seven groups, every 30 samples are taken as one group, and the test results are shown in the table two:
table two:
as can be seen from table two, example 6 is a preferred embodiment of the present invention; in the second step, the composite modification is subjected to mixing heating and 25KHz ultrasonic treatment for 25 minutes, so that the composite effect of the raw materials in the composite modifier can be effectively enhanced, the contact and combination effect of the raw materials is better, and the rapid reaction of the raw materials is ensured; in the third step, the mixture A is subjected to electrostatic spinning treatment and then imidization treatment, so that the raw materials can be effectively subjected to composite treatment to synthesize nano silicon carbide/polyimide composite fibers, and meanwhile, nano titanium dioxide is compounded into the nano silicon carbide/polyimide composite fibers and hollow glass beads, and the hollow glass beads support the nano silicon carbide/polyimide composite fibers, so that the high strength, wear resistance, high and low temperature resistance, corrosion resistance, acid and alkali resistance and aging resistance of the PBT and PET alloy modified material can be effectively enhanced; in the fourth step, part of the composite modified fibers are blended with other raw materials, and in the fifth step, the rest of the composite modified fibers and the glass fibers are blended, so that the distribution uniformity and stability of the composite modified fibers in the PBT and PET alloy modified material can be effectively enhanced, and the overall structural performance of the PBT and PET alloy modified material is further ensured.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The high-weather-resistance high-rigidity glass fiber reinforced PBT and PET alloy modified material is characterized in that: comprises the following components in percentage by weight: 54.60-55.80% of PBT slices, 9.70-10.50% of PET slices, 23.80-24.60% of glass fibers, 0.30-0.50% of ester exchange inhibitor and the balance of composite modifier.
2. The high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of claim 1, which is characterized in that: the composite modifier comprises the following components in percentage by weight: 5.80-6.60% of nano silicon carbide, 14.90-15.50% of polyamide acid, 8.60-9.60% of nano titanium dioxide, 30.60-31.20% of hollow glass beads, 1.60-2.20% of sodium dodecyl benzene sulfonate and the balance of deionized water.
3. The high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of claim 2, which is characterized in that: comprises the following components in percentage by weight: 54.60% of PBT slice, 9.70% of PET slice, 23.80% of glass fiber, 0.30% of ester exchange inhibitor and 11.60% of composite modifier; the composite modifier comprises the following components in percentage by weight: 5.80 percent of nano silicon carbide, 14.90 percent of polyamic acid, 8.60 percent of nano titanium dioxide, 30.60 percent of hollow glass micro-beads, 1.60 percent of sodium dodecyl benzene sulfonate and 38.50 percent of deionized water.
4. The high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of claim 2, which is characterized in that: comprises the following components in percentage by weight: 55.80 percent of PBT slice, 10.50 percent of PET slice, 24.60 percent of glass fiber, 0.50 percent of ester exchange inhibitor and 8.60 percent of composite modifier; the composite modifier comprises the following components in percentage by weight: 6.60 percent of nano silicon carbide, 15.50 percent of polyamic acid, 9.60 percent of nano titanium dioxide, 31.20 percent of hollow glass micro-beads, 2.20 percent of sodium dodecyl benzene sulfonate and 34.90 percent of deionized water.
5. The high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of claim 2, which is characterized in that: comprises the following components in percentage by weight: 55.20 percent of PBT slice, 10.10 percent of PET slice, 24.20 percent of glass fiber, 0.40 percent of ester exchange inhibitor and 10.10 percent of composite modifier; the composite modifier comprises the following components in percentage by weight: 6.20 percent of nano silicon carbide, 15.20 percent of polyamic acid, 9.10 percent of nano titanium dioxide, 30.90 percent of hollow glass micro-beads, 1.90 percent of sodium dodecyl benzene sulfonate and 36.70 percent of deionized water.
6. The high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material of claim 2, which is characterized in that: the ester exchange inhibitor is one or two of sodium benzoate or disodium hydrogen phosphate, the viscosity of the PBT slice is 0.9-1.1, the water content is 0.25-0.5%, and the end shrinking group content is less than or equal to 20 mol/t; the viscosity of the PET slice is 0.7-0.9, the water content is 0.25-0.5%, and the end shrinking base content is 30 +/-5 mol/t; the glass fiber is one or two of flat glass fiber or short glass fiber, and the diameter of the glass fiber is 10-13 mu m.
7. The preparation method of the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material according to any one of claims 1 to 6, characterized by comprising the following steps: the preparation method comprises the following specific steps:
the method comprises the following steps: weighing the PBT slice, the PET slice, the glass fiber, the ester exchange inhibitor and the composite modifier in parts by weight;
step two: mixing the composite modifier in the step one, heating to 70-80 ℃, and carrying out ultrasonic treatment for 20-30 minutes to obtain a mixture A;
step three: performing electrostatic spinning on the mixture A prepared in the step two to obtain composite fibers, and performing thermal imidization treatment on the composite modified fibers to obtain composite modified fibers;
step four: blending the PBT slice, the PET slice, the ester exchange inhibitor and the two-thirds weight part composite modified fiber prepared in the step three to obtain a mixture B;
step five: blending the glass fiber obtained in the step one and the residual composite modified fiber obtained in the step three to obtain a mixture C;
step five: putting the mixture B prepared in the fourth step into a double-screw extruder, and adding the mixture C prepared in the fifth step into the double-screw extruder from a side feed;
step six: after the extruder discharges materials, the materials enter a cooling water tank for cooling, then enter a granulator for granulating, and enter a homogenizing bin after being screened by a vibrating screen, so that the high-weather-resistance and high-rigidity glass fiber reinforced PBT and PET alloy modified material is prepared.
8. The preparation method of the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material according to claim 7, characterized by comprising the following steps: in the second step, the ultrasonic treatment frequency is 23-27 KHz, and the ultrasonic treatment power is 1200-1800W; in the third step, in the electrostatic spinning process, 14-18 KV high voltage is applied, the distance between a capillary nozzle of the injector and a grounded receiving device is 13-15 cm, and the thermal imidization treatment temperature is 200-300 ℃; in step five, the twin screw extruder temperature is set to a zone: 240-260 ℃, the temperature of the second zone is 240-260 ℃, the temperature of the third zone is 240-250 ℃, the temperature of the fourth zone is 235-245 ℃, the temperature of the fifth zone is 225-235 ℃, the temperature of the sixth zone is 225-235 ℃, the temperature of the seventh zone is 225-235 ℃, the temperature of the eighth zone is 225-235 ℃, and the temperature of the ninth zone is 230-240 ℃; in the sixth step, the temperature of the cooling water tank is 24-26 ℃, and the rotating speed of the granulator is 800-1100 r/min.
9. The preparation method of the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material according to claim 8, characterized by comprising the following steps: in the second step, the ultrasonic treatment frequency is 23KHz, and the ultrasonic treatment power is 1200W; in the third step, in the electrostatic spinning process, 14KV high voltage is applied, the distance between a capillary nozzle of the injector and a grounded receiving device is 13cm, and the thermal imidization treatment temperature is 200 ℃; in step five, the twin screw extruder temperature is set to a zone: 240 ℃, 240 ℃ of the temperature of the second zone, 240 ℃ of the temperature of the third zone, 235 ℃ of the temperature of the fourth zone, 225 ℃ of the temperature of the fifth zone, 225 ℃ of the temperature of the sixth zone, 225 ℃ of the temperature of the seventh zone, 225 ℃ of the temperature of the eighth zone and 230 ℃ of the temperature of the ninth zone; in the sixth step, the temperature of the cooling water tank is 24 ℃, and the rotating speed of the granulator is 800 r/min.
10. The preparation method of the high weather-resistant high-rigidity glass fiber reinforced PBT and PET alloy modified material according to claim 8, characterized by comprising the following steps: in the second step, the ultrasonic treatment frequency is 25KHz, and the ultrasonic treatment power is 1500W; in the third step, 16KV high voltage is applied in the electrostatic spinning process, the distance between a capillary nozzle of the injector and a grounded receiving device is 14cm, and the thermal imidization treatment temperature is 250 ℃; in step five, the twin screw extruder temperature is set to a zone: 250 ℃, 250 ℃ of the temperature of the second zone, 245 ℃ of the temperature of the third zone, 240 ℃ of the temperature of the fourth zone, 230 ℃ of the temperature of the fifth zone, 230 ℃ of the temperature of the sixth zone, 230 ℃ of the temperature of the seventh zone, 230 ℃ of the temperature of the eighth zone and 235 ℃ of the temperature of the ninth zone; in the sixth step, the temperature of the cooling water tank is 25 ℃, and the rotating speed of the granulator is 900 r/min.
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