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High-flame-retardant microsphere C60-PMMA composite material and preparation method thereof

A technology of C60-PMMA and composite materials, which is applied in the field of high flame-retardant microsphere C60-PMMA composite materials and its preparation, can solve the problems of easy combustion, poor impact resistance, poor thermal stability, etc., and achieve the purpose of inhibiting thermal degradation reactions, Remarkable flame retardant effect, effect of improving dispersion form

Inactive Publication Date: 2021-12-10
BINZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to its shortcomings such as brittleness and easy cracking, poor thermal stability, easy combustion, poor impact resistance, and prone to detonation in polymerization reactions, the wide application of PMMA is limited.

Method used

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  • High-flame-retardant microsphere C60-PMMA composite material and preparation method thereof
  • High-flame-retardant microsphere C60-PMMA composite material and preparation method thereof
  • High-flame-retardant microsphere C60-PMMA composite material and preparation method thereof

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preparation example Construction

[0026] A kind of highly flame-retardant microsphere C60-PMMA composite material and preparation method thereof, its synthesis process comprises the following steps:

[0027] (1) Preparation of dispersant: 1-2 parts of polyvinyl alcohol (PVA) and 90-100 parts of distilled water are put into a three-neck flask together, heated in a water bath to a temperature of 55-65°C, and the rotation speed is 300-350r / min. Stir continuously for 2 to 3 hours, and raise the temperature by 4 to 7°C every 2 to 3 hours until the PVA solution in the three-neck flask turns from milky white to transparent, then pour it into a beaker for later use.

[0028] (2) Preparation of PMMA microspheres: Pour 34 to 45 parts of distilled water into a three-necked flask, and drop 1 to 3 parts of 5% PVA solution. Stir for 5-10 minutes under the same conditions; then pour 10-15 parts of the MMA solution into a three-necked flask and heat up. Add 1% to 1.5% of the mass of MMA solution azobisisobutyronitrile (AIBN)...

Embodiment 1

[0041] Preparation of dispersant: put 5g of polyvinyl alcohol (PVA) and 95g of distilled water into a three-necked flask, heat it in a water bath to a temperature of 60°C, and stir continuously for 2.5h at a speed of 320r / min, and raise the temperature for 5 h every 2.5h. ℃ until the PVA solution in the three-necked flask turns from milky white to transparent to make a 5% PVA solution, which is poured into a beaker for subsequent use.

[0042] Preparation of PMMA microspheres: Pour 40g of distilled water into a three-necked flask, and drop into 2g of 5% PVA solution, adjust the rotation speed to 320r / min, and stir for 5min at a temperature of 40°C; then pour 12g of MMA solution into the three-necked flask Medium and warm up. Add 0.16g of azobisisobutyronitrile (AIBN) in 3 portions at 50°C, 60°C, and 70°C, then slowly raise the temperature to 78°C, and react for 30 minutes. Take out a small amount of beads and drop them into water without hardening, then finish the reaction fo...

Embodiment 2

[0047] Taking PMMA microspheres, C60 / PMMA microsphere sample 1, C60 / PMMA microsphere sample 2 and C60 / PMMA microsphere sample 3 as objects, the morphology and composition characterization, thermal performance evaluation and flame retardancy evaluation were carried out. The experimental results are shown in the table below:

[0048] (1) Scanning electron microscope analysis

[0049] PMMA and C60 / PMMA-1 observed under the scanning electron microscope such as figure 1 shown. From figure 1 It can be observed in (a) and 1 (b) that the prepared PMMA microspheres are uniformly spherical, and most of the surfaces are smooth, but some of them have small hole defects. The reason may be that the temperature of the material is too high during the polymerization process, which destroys the internal The chemical bond structure, the reaction stops before being completely combined into a spherical shape, resulting in local unevenness. From figure 1 (c), 1(d), it can be seen that the C60 / ...

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Abstract

The invention discloses a high-flame-retardant microsphere C60-PMMA composite material and a preparation method thereof. The preparation method comprises the following steps: firstly, continuously stirring and heating quantitative polyvinyl alcohol (PVA) and distilled water to prepare a dispersing agent; secondly, by taking azodiisobutyronitrile (AIBN) as a catalyst, sequentially adding a PVA solution and an MMA solution into distilled water at different temperatures and stirring rates to prepare PMMA microspheres; then, adding fullerene and sodium nitrate powder into quantitative concentrated sulfuric acid in sequence, slowly adding potassium permanganate to uniformly disperse, adding deionized water and hydrogen peroxide in sequence, and carrying out suction filtration by using a vacuum pump to finally obtain pretreated fullerene powder; and finally, preparing the high-flame-retardant microsphere C60 / PMMA composite material from the fullerene (C60) aqueous solution with different concentrations and methyl methacrylate (MMA) . The C60 is more uniformly dispersed in PMMA, the thermal stability is higher, the flame-retardant effect is obvious, and the safety performance is better.

Description

technical field [0001] The invention relates to the field of flame retardant technology, in particular to a high flame retardant microsphere C60-PMMA composite material and a preparation method thereof. Background technique [0002] Polymethyl methacrylate (PMMA) is an important general-purpose polymer, which is usually used as a glass because of its excellent properties such as high transparency, low cost, high mechanical strength, easy handling and processing, and chemical corrosion resistance. substitutes and are widely used in various fields. However, due to its shortcomings of brittleness, easy cracking, poor thermal stability, easy combustion, poor impact resistance, and prone to detonation in polymerization reactions, the wide application of PMMA is limited. In recent years, scholars at home and abroad have been optimizing and innovating the system of PMMA composite materials. Using nanomaterials as flame retardants to modify polymers can not only achieve a higher le...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/14B01J13/04C08F292/00C08F220/14
CPCB01J13/14B01J13/043C08F292/00C08F220/14
Inventor 胡莹莹许兰娟贾新磊张清涛申建军郭文杰李跃金李超
Owner BINZHOU UNIV