CN116285257A - Preparation method of high-temperature-resistant super-tough modified PBT-PET composite material - Google Patents
Preparation method of high-temperature-resistant super-tough modified PBT-PET composite material Download PDFInfo
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- CN116285257A CN116285257A CN202310563846.5A CN202310563846A CN116285257A CN 116285257 A CN116285257 A CN 116285257A CN 202310563846 A CN202310563846 A CN 202310563846A CN 116285257 A CN116285257 A CN 116285257A
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- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000013067 intermediate product Substances 0.000 claims abstract description 36
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 20
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 238000012545 processing Methods 0.000 claims abstract description 13
- 238000000465 moulding Methods 0.000 claims abstract description 7
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 10
- -1 alkyl carboxylic acid Chemical class 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 230000001476 alcoholic effect Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 5
- 239000000047 product Substances 0.000 abstract description 5
- 239000000377 silicon dioxide Substances 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 3
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 3
- 238000001125 extrusion Methods 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000001816 cooling Methods 0.000 description 8
- KZTYYGOKRVBIMI-UHFFFAOYSA-N diphenyl sulfone Chemical compound C=1C=CC=CC=1S(=O)(=O)C1=CC=CC=C1 KZTYYGOKRVBIMI-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 238000007599 discharging Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000001376 precipitating effect Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 4
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229940005605 valeric acid Drugs 0.000 description 2
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000002464 physical blending Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000010626 work up procedure Methods 0.000 description 1
Classifications
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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
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- 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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
Abstract
The invention relates to a preparation method of a high-temperature-resistant super-tough modified PBT-PET composite material, which comprises the following steps: s1, blending PBT, PET and hexamethylenediamine and reacting to obtain an intermediate product 1; s2, grafting the hydroxylated silicon dioxide with an alkyl carboxylic acid part to obtain an intermediate product 2; s3, blending the intermediate products 1 and 2, feeding the mixture into an extruder for processing, and extruding and molding the mixture. The invention mainly carries out segment modification on the composite material, and carries out melt extrusion after being physically blended with silicon dioxide particles containing hydroxyl and alkyl chains, thus obtaining the high-temperature-resistant PBT-PET composite material with uniform phase state. After the composite material is placed at high temperature for a long time, the composite material shows good mechanical properties, and is at the same level as the initial state, so that the product has good application prospect and excellent heat resistance.
Description
Technical Field
The invention relates to the technical field of modified composite materials, in particular to a preparation method of a high-temperature-resistant super-tough modified PBT-PET composite material.
Background
PBT and PET are cheap and widely used aromatic polyesters, are important thermoplastic polyesters, have excellent physical properties, chemical properties, dimensional stability, transparency and recyclability, and can be widely applied to the fields of magnetic recording, photosensitive materials, electronic, electric insulation, industrial films, package decoration, screen protection, optical mirror surface protection and the like.
The main advantages are as follows: (1) The high-temperature heat-resistant alloy has excellent stability, and can continuously maintain stable performance in a high-temperature environment; (2) The glass has low haze and high light transmittance, small surface finish and small thickness tolerance; (3) The film has excellent mechanical strength and chemical property after film formation; (4) It also has degradability and is an environment-friendly material.
In the prior art, patents such as CN114163790A, CN109572128A, CN114702794A and the like disclose heat-resistant PET materials or films, have the effects of high heat resistance, flame retardance and the like, and are suitable for being used as materials in high-temperature operation areas.
However, the improvement of the high temperature resistance of PBT and PET is still a difficult problem in the industry at present. How to ensure that the material does not generate thermal deformation, embrittlement and other phenomena in a long-term high-temperature environment, and keep good mechanical properties is always a hot spot for people to chase.
In view of the foregoing, there is a need to develop a new technical solution to solve the problems in the prior art.
Disclosure of Invention
Based on the method, the invention develops a preparation method of the high-temperature-resistant super-tough modified PBT-PET composite material. The main technical scheme is that the PBT-PET composite material is modified, and an amino chain segment is introduced to form an intermediate product 1, so that the heat resistance is improved to a certain extent compared with the original alkoxy chain segment; secondly, silicon dioxide particles containing hydroxyl and alkyl chains, namely an intermediate product 2, are introduced, the intermediate product 1 and the intermediate product 2 are uniformly blended in an extruder, and the hydroxyl and amino groups on the intermediate product 1 are easy to form intermolecular hydrogen bonds, so that intermolecular acting force is reinforced, the rigidity and crystallinity of the molecular chains are enhanced, and the heat resistance of the product is further improved. The alkyl chain segment on the intermediate product 2 has flexibility, and the defect of insufficient flexibility on the intermediate product 1 can be overcome, so that the flexibility of the product is increased to a certain extent, and the toughness is not obviously lost.
The invention aims to provide a preparation method of a high-temperature-resistant super-tough modified PBT-PET composite material, which comprises the following steps:
s1, blending PBT, PET and hexamethylenediamine and reacting to obtain an intermediate product 1;
s2, grafting the hydroxylated silicon dioxide with an alkyl carboxylic acid part to obtain an intermediate product 2;
s3, blending the intermediate products 1 and 2, feeding the mixture into an extruder for processing, and extruding and molding the mixture.
Further, in step S1, the reaction conditions are: the reaction temperature is 200-250 ℃ and the reaction time is 10-15 h in the autoclave.
Further, in step S2, the reaction conditions are: mixing the hydroxylated silica with an alkyl carboxylic acid in an alcoholic solvent, sonicating, and then filtering.
Further, the molar ratio of the PBT, the PET and the hexamethylenediamine blend is as follows: 1:1:5-1:3:15.
Further, the molar ratio of the hydroxylated silica to the alkyl carboxylic acid is 1:0.3 to 1:0.1.
Further, in step S3, PEN is also added.
Further, in step S3, the temperature of the extruder processing is 280 to 290 ℃.
Further, the alkyl carboxylic acid is selected from alkyl carboxylic acids having an alkyl length of C4 to C8.
Further, the extruder is a twin screw extruder.
Further, the mass ratio of the intermediate product 1 to the intermediate product 2 is 1:0.1-1:0.05.
The invention has the following beneficial effects:
the invention discloses a preparation method of a blend based on a PBT-PET composite material, which is mainly used for segment modification of the composite material, and is used for carrying out physical blending with silicon dioxide particles containing hydroxyl groups and alkyl chains and then carrying out melt extrusion to obtain the high-temperature-resistant PBT-PET composite material with uniform phase. After the composite material is placed at high temperature for a long time, the composite material shows good mechanical properties, and is at the same level as the initial state, so that the product has good application prospect and excellent heat resistance.
Detailed Description
In order to more clearly illustrate the technical solution of the present invention, the following examples are set forth. The starting materials, reactions and workup procedures used in the examples are those commonly practiced in the market and known to those skilled in the art unless otherwise indicated.
PEN, PBT and PET in the embodiments of the invention are purchased from Basoff.
The hydroxylated silica of the present invention was purchased from eastern sea county rich mineral products limited.
The extruder in the embodiment of the invention adopts a double-screw extruder.
Example 1
A preparation method of a high-temperature-resistant super-tough modified PBT-PET composite material comprises the following steps:
s1, blending PBT, PET and hexamethylenediamine (1:1:5, n/n/n) with enough diphenyl sulfone, adding the mixture into a pressure kettle provided with a cooling and static device and a stirrer under the protection of nitrogen, heating to 230 ℃, reacting 10 and h, and then cooling and discharging to obtain an intermediate product 1;
s2, blending hydroxylated silicon dioxide and caproic acid (1:5, m/m), dispersing 10 h by using ethanol as a solvent under the ultrasonic condition at 70 ℃, and then filtering and precipitating to obtain an intermediate product 2;
s3, blending the intermediate product 1, the intermediate product 2 and PEN (1:0.07:0.3, m/m/m), adding the blend into a double-screw extruder for processing, setting the processing temperature of the extruder to be 282-285 ℃, and extruding and molding.
Example 2
A preparation method of a high-temperature-resistant super-tough modified PBT-PET composite material comprises the following steps:
s1, blending PBT, PET and hexamethylenediamine (1:3:8, n/n/n) with enough diphenyl sulfone, adding the mixture into a pressure kettle provided with a cooling and static device and a stirrer under the protection of nitrogen, heating to 230 ℃, reacting 10 and h, and then cooling and discharging to obtain an intermediate product 1;
s2, blending hydroxylated silicon dioxide and butyric acid (1:5, m/m), dispersing 10 h by using ethanol as a solvent under the ultrasonic condition at 70 ℃, and then filtering and precipitating to obtain an intermediate product 2;
s3, blending the intermediate product 1, the intermediate product 2 and PEN (1:0.1:0.3, m/m/m), adding the blend into a double-screw extruder for processing, setting the processing temperature of the extruder to be 282-285 ℃, and extruding and molding.
Example 3
A preparation method of a high-temperature-resistant super-tough modified PBT-PET composite material comprises the following steps:
s1, blending PBT, PET and hexamethylenediamine (1:2:6, n/n/n) with enough diphenyl sulfone, adding the mixture into a pressure kettle provided with a cooling device and a stirrer under the protection of nitrogen, heating to 240 ℃, reacting 10 and h, and then cooling and discharging to obtain an intermediate product 1;
s2, blending hydroxylated silicon dioxide and valeric acid (1:5, m/m), taking ethanol as a solvent, dispersing 10 h under the ultrasonic condition at 70 ℃, and then filtering and precipitating to obtain an intermediate product 2;
s3, blending the intermediate product 1, the intermediate product 2 and PEN (1:0.05:0.2, m/m/m), adding the blend into a double-screw extruder for processing, setting the processing temperature of the extruder to be 282-285 ℃, and extruding and molding.
Example 4
A preparation method of a high-temperature-resistant super-tough modified PBT-PET composite material comprises the following steps:
s1, blending PBT, PET and hexamethylenediamine (1:2:5, n/n/n) with enough diphenyl sulfone, adding the mixture into a pressure kettle provided with a cooling device and a stirrer under the protection of nitrogen, heating to 240 ℃, reacting 10 and h, and then cooling and discharging to obtain an intermediate product 1;
s2, blending hydroxylated silicon dioxide and valeric acid (1:6, m/m), taking ethanol as a solvent, dispersing 10 h under the ultrasonic condition at 70 ℃, and then filtering and precipitating to obtain an intermediate product 2;
s3, blending the intermediate product 1, the intermediate product 2 and PEN (1:0.05:0.1, m/m/m), adding the blend into a double-screw extruder for processing, setting the processing temperature of the extruder to be 282-285 ℃, and extruding and molding.
Comparative example 1
A method for preparing a composite material, this comparative example 1 differs from example 1 in that: in step S2, the raw material hydroxylated silicon dioxide is placed in a muffle furnace and heated at 800 ℃ to remove most of hydroxyl groups. The silica was then substituted for intermediate 2 in equal mass, the other ingredients and preparation method being the same as in example 1.
Comparative example 2
A method for preparing a composite material, this comparative example 2 differs from example 1 in that: in step S2, the intermediate 2 was replaced with hydroxylated silica in equal mass, and the other components and preparation method were the same as in example 1.
Test case
The testing method comprises the following steps:
performance test comparisons were made on the PBT composite samples prepared in example 1 and comparative examples 1-2. The sample extruded from the extruder is longitudinally stretched at 120 ℃ with the stretching ratio of 4; and stretching transversely at 140 ℃ with a stretching ratio of 2; finally, the film is formed into a film with the thickness of 40-50 mu m by heat setting at 230 ℃. Then the films are respectively placed at normal temperature, and the mechanical properties of the films are tested; the samples were then placed in an environment of 85 ℃ at 14 d and their relevant parameters were then tested.
Wherein, the MD tensile strength is vertical tensile strength, and a tensile testing machine (the brand is AG-LN10KN of the testing equipment of the Zhuhai city safety regulations); MD heat shrinkage is vertical heat shrinkage, and is measured by a heat shrinkage tester (brand name: dongguan Boleid Instrument Co., ltd.).
The test results are shown in Table 1.
TABLE 1 Performance test results
According to Table 1, the capabilities of the materials in example 1 are significantly better than those in comparative examples 1-2, and the fact that the materials have strong intermolecular forces among the components in the technical scheme of the invention proves that the mechanical properties of the materials are not obviously reduced even if the materials are placed for a long time at high temperature.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (7)
1. The preparation method of the high-temperature-resistant super-tough modified PBT-PET composite material is characterized by comprising the following steps of:
s1, blending PBT, PET and hexamethylenediamine and reacting to obtain an intermediate product 1;
s2, grafting the hydroxylated silicon dioxide with an alkyl carboxylic acid part to obtain an intermediate product 2;
s3, blending the intermediate products 1 and 2, feeding the mixture into an extruder for processing, and extruding and molding;
the molar ratio of the PBT to the PET to the hexamethylenediamine blend is as follows: 1:1:5-1:3:15;
the mass ratio of the hydroxylated silicon dioxide to the alkyl carboxylic acid is 1:5-1:6;
the mass ratio of the intermediate product 1 to the intermediate product 2 is 1:0.1-1:0.05.
2. The method for preparing the high temperature resistant super tough modified PBT-PET composite material according to claim 1, wherein in the step S1, the reaction conditions are as follows: the reaction temperature is 200-250 ℃ and the reaction time is 10-15 h in the autoclave.
3. The method for preparing the high temperature resistant super tough modified PBT-PET composite material according to claim 1, wherein in the step S2, the reaction conditions are as follows: mixing the hydroxylated silica with an alkyl carboxylic acid in an alcoholic solvent, sonicating, and then filtering.
4. The method for preparing a high temperature resistant super tough modified PBT-PET composite material according to claim 1, wherein PEN is further added in step S3.
5. The method for preparing a high temperature resistant super tough modified PBT-PET composite according to claim 1, wherein in step S3, the extruder processing temperature is 280-290 ℃.
6. The method for preparing the high temperature resistant super tough modified PBT-PET composite material according to claim 1, wherein the alkyl carboxylic acid is selected from alkyl carboxylic acids with alkyl length of C4-C8.
7. The method for preparing the high temperature resistant super tough modified PBT-PET composite material according to claim 1, wherein the extruder is a twin screw extruder.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310563846.5A CN116285257B (en) | 2023-05-18 | 2023-05-18 | Preparation method of high-temperature-resistant super-tough modified PBT-PET composite material |
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| CN202310563846.5A CN116285257B (en) | 2023-05-18 | 2023-05-18 | Preparation method of high-temperature-resistant super-tough modified PBT-PET composite material |
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| CN116285257B CN116285257B (en) | 2023-07-18 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116622227A (en) * | 2023-07-24 | 2023-08-22 | 广东永鑫华新型材料有限公司 | Preparation method of glass fiber reinforced nylon material with low water absorption |
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| CN1305511A (en) * | 1998-06-15 | 2001-07-25 | 伊斯曼化学公司 | High barrier polyester/phenylenedi (oxyacetic acid) polyester blends |
| CN102660019A (en) * | 2012-05-09 | 2012-09-12 | 金发科技股份有限公司 | High temperature-resistant nylon/ polybutylece terephthalate (PBT)/polyethylene terephthalate (PET) copolymer, and preparation method and application thereof |
| CN102660020A (en) * | 2012-05-09 | 2012-09-12 | 金发科技股份有限公司 | High-temperature resistant nylon/PEN/PBT/PET copolymer and preparation method thereof |
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- 2023-05-18 CN CN202310563846.5A patent/CN116285257B/en active Active
Patent Citations (4)
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|---|---|---|---|---|
| CN1305511A (en) * | 1998-06-15 | 2001-07-25 | 伊斯曼化学公司 | High barrier polyester/phenylenedi (oxyacetic acid) polyester blends |
| CN1312837A (en) * | 1998-06-15 | 2001-09-12 | 伊斯曼化学公司 | Polyester/phenylenedic (oxyacetic acid) copolyester blends having improved barrier to gas permeation |
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Non-Patent Citations (2)
| Title |
|---|
| LIANA R. AZIZOVA ET AL: "Thermal and hydrolytic stability of grafted ester groups of carboxylic acids on the silica surface", 《J THERM ANAL CALORIM》, vol. 122, pages 517 - 523, XP035553327, DOI: 10.1007/s10973-015-4828-1 * |
| 周天等: "电容膜用新型PEN-PET共聚酯的研制", 《聚酯工业》, vol. 20, no. 1, pages 16 - 20 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116622227A (en) * | 2023-07-24 | 2023-08-22 | 广东永鑫华新型材料有限公司 | Preparation method of glass fiber reinforced nylon material with low water absorption |
| CN116622227B (en) * | 2023-07-24 | 2023-09-15 | 广东永鑫华新型材料有限公司 | Preparation method of glass fiber reinforced nylon material with low water absorption |
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