CN113956496A - Preparation method of novel two-dimensional nylon 6 antioxidant - Google Patents

Preparation method of novel two-dimensional nylon 6 antioxidant Download PDF

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Publication number
CN113956496A
CN113956496A CN202111176638.7A CN202111176638A CN113956496A CN 113956496 A CN113956496 A CN 113956496A CN 202111176638 A CN202111176638 A CN 202111176638A CN 113956496 A CN113956496 A CN 113956496A
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China
Prior art keywords
antioxidant
novel
nylon
dimensional
preparation
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Pending
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CN202111176638.7A
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Chinese (zh)
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林福华
王波
卫英慧
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Taiyuan University of Science and Technology
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Taiyuan University of Science and Technology
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Priority to CN202111176638.7A priority Critical patent/CN113956496A/en
Publication of CN113956496A publication Critical patent/CN113956496A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G83/00Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
    • C08G83/008Supramolecular polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/02Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/24Crystallisation aids

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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)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to the technical field of nylon 6 antioxidants, and particularly relates to a preparation method of a novel two-dimensional nylon 6 antioxidant. Mixing trimesic acid with Cu (NO)3)•3H2And O is reacted, and the two-dimensional nylon 6 antioxidant taking copper ions as central atoms is obtained through separation and purification. The antioxidant can greatly improve the oxidation resistance and mechanical property of the nylon 6 after aging.

Description

Preparation method of novel two-dimensional nylon 6 antioxidant
Technical Field
The invention relates to the technical field of polymer antioxidants, in particular to a preparation method of a novel two-dimensional nylon 6 antioxidant.
Background
Nylon 6(PA6) is one of the most commonly used engineering plastics, has good chemical resistance and processing fluidity, has a regular structure, good mechanical strength, crystallinity and wear resistance, is lower in price compared with other engineering plastics, and is widely applied to the fields of packaging, electronics, transportation and the like. . However, the PA6 product has serious aging degradation phenomena under the action of heat and oxygen, such as yellowing and brittleness, reduction of mechanical properties of materials and the like, and the processing and the service life of the product are greatly influenced. Therefore, only by modifying the thermal oxygen stability of PA6, it has the required properties for different fields.
Disclosure of Invention
The invention aims to provide a preparation method of a novel two-dimensional nylon 6 antioxidant, and the scheme is thatUsing trimesic acid with Cu (NO)3)·3H2And O is reacted, and the two-dimensional nylon 6 antioxidant taking copper ions as central atoms is obtained through separation and purification. . Solves the technical problem of severe aging degradation of PA6 products under the action of heat and oxygen.
The invention aims to provide a preparation method of a novel two-dimensional nylon 6 antioxidant, which comprises the following preparation processes:
a certain amount of trimesic acid (H)3BTC) is dissolved in alcohol solution and stirred until the BTC is completely dissolved; weighing Cu (NO)3)·3H2Dissolving O in deionized water, and stirring until the O is completely dissolved; and uniformly mixing the two solutions, transferring the mixed solution into a stainless steel reaction kettle, reacting for a certain time at a certain temperature, naturally cooling to room temperature, carrying out suction filtration, washing with distilled water and absolute ethyl alcohol for three times respectively, drying a sample, and then placing the dried sample in a vacuum drying oven for activation for 12 hours.
Further, the temperature condition of the synthesis reaction is 120-140 ℃.
Further, the time length of the combination reaction is 12-24 h. The above time ensures H3BTC and Cu (NO)3) ·3H2O is sufficiently bound.
Further, the alcohol solution is ethanol.
Further, the crude product after the reaction is finished is obtained after being filtered, washed, activated and dried.
The principle and the advantages of the scheme are as follows: in this scheme trimesic acid is used with Cu (NO)3)·3H2O is reacted, and the antioxidant is obtained through separation and purification, and Cu1+、Cu2+The regeneration can be continued through the oxidation-reduction reaction and the reaction of capturing free radicals, and the high antioxidant activity is always kept in the reaction process. The two-dimensional nanostructure of the composite material has good compatibility with a PA6 matrix, and can be composited with PA6 on a nanometer scale. In addition, the Cu-MOF nano particles can play a heterogeneous nucleation role in a PA6 matrix, so that the material has better mechanical properties.
Drawings
FIG. 1 is a graph comparing aging times of the present invention.
Detailed Description
The following is further detailed by way of specific embodiments:
example 1:
weighing 1.050g of trimesic acid (H)3BTC) is dissolved in 20mL of ethanol and stirred until the BTC is completely dissolved; 2.186g Cu (NO) are weighed out3)·3H2Dissolving O in 20mL of deionized water, and stirring until the O is completely dissolved; mixing the two solutions, stirring for 30min until the two solutions are uniformly mixed, transferring the mixture into a 50mL stainless steel reaction kettle, reacting for 24h at 120 ℃, naturally cooling to room temperature after complete reaction, performing suction filtration, washing with distilled water and absolute ethyl alcohol for three times respectively, drying a sample, and then placing the sample in a 150 ℃ vacuum drying oven for activation for 12 h.
Mixing the sample and PA6 in a double-screw extruder according to the proportion of 1:10000, extruding, granulating and injection molding to obtain a composite material standard sample strip, aging by adopting a xenon arc lamp with the lamp tube of 340nm according to the method of GB/T7141-2008, and simulating factors such as outdoor ultraviolet light, humidity, rainfall, visible light, temperature and the like. Accelerated aging is respectively carried out on the composite material for different times, and the performance of the composite material is measured by using a thermal weight loss analyzer, a universal tensile machine and an impact testing machine. The specific data are shown in fig. 1.
Comparative example 1:
PA6 is mixed, extruded, granulated and injection-molded into a composite material standard sample strip in a double-screw extruder, and a xenon arc lamp is adopted for aging according to the method of GB/T7141-2008, the lamp tube is 340nm, and factors such as outdoor ultraviolet light, humidity, rainfall, visible light, temperature and the like are simulated. Accelerated aging was performed on PA6 for different times, and its performance was measured using a thermogravimetric analyzer, a universal tensile machine, and an impact tester. The specific data are shown in fig. 1.
The foregoing is merely an example of the present invention and common general knowledge in the art of designing and/or characterizing particular aspects and/or features is not described in any greater detail herein. It should be noted that, for those skilled in the art, without departing from the technical solution of the present invention, several variations and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.

Claims (4)

1. A preparation method of a novel two-dimensional nylon 6 antioxidant is characterized by comprising the following steps: mixing trimesic acid with Cu (NO)3)•3H2And O, reacting, separating and purifying to obtain a crude antioxidant product, filtering and washing the crude antioxidant product, activating, and drying to obtain the novel two-dimensional nylon 6 antioxidant.
2. The method for preparing the novel two-dimensional nylon 6 antioxidant as claimed in claim 1, wherein the method comprises the following steps: the trimesic acid and Cu (NO)3)•3H2The reaction temperature condition of O is 120-140 ℃.
3. The method for preparing the novel two-dimensional nylon 6 antioxidant as claimed in claim 1, wherein the method comprises the following steps: the trimesic acid and Cu (NO)3)•3H2The reaction time of O is 12-24 h.
4. The method for preparing the novel two-dimensional nylon 6 antioxidant as claimed in claim 1, wherein the method comprises the following steps: dissolving the trimesic acid in an alcohol solution, and then mixing with Cu (NO)3)•3H2And O is reacted.
CN202111176638.7A 2021-10-09 2021-10-09 Preparation method of novel two-dimensional nylon 6 antioxidant Pending CN113956496A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111176638.7A CN113956496A (en) 2021-10-09 2021-10-09 Preparation method of novel two-dimensional nylon 6 antioxidant

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111176638.7A CN113956496A (en) 2021-10-09 2021-10-09 Preparation method of novel two-dimensional nylon 6 antioxidant

Publications (1)

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CN113956496A true CN113956496A (en) 2022-01-21

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CN202111176638.7A Pending CN113956496A (en) 2021-10-09 2021-10-09 Preparation method of novel two-dimensional nylon 6 antioxidant

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116102739A (en) * 2023-02-02 2023-05-12 华东理工大学 Copper-based multifunctional auxiliary agent for nylon and preparation method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116102739A (en) * 2023-02-02 2023-05-12 华东理工大学 Copper-based multifunctional auxiliary agent for nylon and preparation method and application thereof
CN116102739B (en) * 2023-02-02 2024-05-14 华东理工大学 Copper-based multifunctional auxiliary agent for nylon and preparation method and application thereof

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