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Method for producing polythene/POSS modified tough clay nano composite material

A technology of nanocomposite materials and polyethylene, which is applied in the field of preparation of polyethylene/POSS modified clay nanocomposites, can solve the problems of poor mechanical properties of composite materials, high temperature resistance, material processing and adverse effects on performance, etc., to achieve The preparation method is simple, avoiding thermal instability, thermal stability and the effect of improving the dynamic mechanical storage modulus

Inactive Publication Date: 2008-05-07
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The organic modifier usually used is an amine salt with a long alkane group. Since this type of amine salt is an organic small molecule, it cannot withstand high temperature, so it will have a negative impact on the processing and performance of the material.
Shah RK et al. reported in Polymer, 47 (11), 4075-4084, 2006 to prepare low-density polyethylene (LDPE) / organic amine modified clay nanocomposites at different temperatures by melt blending method, and found that with With the increase of melt blending temperature, the degradation of organic amines is intensified, and the mechanical properties of the obtained composites gradually deteriorate

Method used

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  • Method for producing polythene/POSS modified tough clay nano composite material
  • Method for producing polythene/POSS modified tough clay nano composite material
  • Method for producing polythene/POSS modified tough clay nano composite material

Examples

Experimental program
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Effect test

Embodiment 1

[0031] (1) Preparation of acenaphthyldiimine ligand

[0032] 3.0 g of 4,4-methylene-bis(2,6-diisopropylaniline) and 0.54 g of acenaphthoquinone were dissolved in 50 ml of toluene solution, 2 ml of formic acid was added as a catalyst, and the mixture was refluxed for 14 hours. During the reflux process, a water separator was used to remove the moisture generated during the reaction. After the reflux was completed, the temperature of the solution was lowered to room temperature, and the solvent was evaporated in vacuo. The resulting crude product was purified by column (silica gel, ethyl acetate:petroleum ether=1:9) to obtain 1.2 g of N,N'-bis[4-(4-amino-3,5-diisopropylbenzyl )-2,6-diisopropylphenyl] acenaphthylenediimine ligand L, yellow powder. Ligand L 1 H-NMR (500MHz, CDCl 3 ) results: 7.89(d, 2H), 7.37(t, 2H), 7.01(s, 4H), 6.87(s, 4H), 6.74(s, 2H), 3.84(d, 4H), 3.53(s, 4H ), 2.19(s, 12H), 2.06(s, 12H); ligand L 13 C-NMR (500MHz, CDCl 3 )结果:161.016,145.358,140.787,137...

Embodiment 2

[0045] The other conditions of this embodiment are the same as in Example 1: the polymerization reaction time in step (6) is 80min. Under the above polymerization conditions, the branching degree, melting point, crystallinity and molecular weight of the obtained polyethylene are shown in Table 1. The POSS modified clay content is 6.2%. The thermal decomposition temperature of polyethylene / POSS modified clay nanocomposites is shown in Table 2. When 50% thermal weight loss is used as a comparison point, the degradation temperature of polyethylene composites is 471.9 ° C, which is higher than that of pure Polyethylene is 56.0°C higher. The storage modulus of polyethylene / POSS modified clay nanocomposites is shown in Table 3. At 20°C, the storage modulus of polyethylene composites is 989% higher than that of pure polyethylene.

Embodiment 3

[0049] The other conditions of this embodiment are the same as in Example 1: the polymerization reaction time in step (6) is 45min. Under the above polymerization conditions, the branching degree, melting point, crystallinity and molecular weight of the obtained polyethylene are shown in Table 1. The POSS modified clay content is 9.8%. The thermal decomposition temperature of polyethylene / POSS modified clay nanocomposites is shown in Table 2. When 50% thermal weight loss is used as a comparison point, the degradation temperature of polyethylene composites is 477.8 ° C, which is higher than that of pure Polyethylene is 61.9°C higher. The storage modulus of polyethylene / POSS modified clay nanocomposites is shown in Table 3. At 20°C, the storage modulus of polyethylene composites is 1226% higher than that of pure polyethylene.

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Abstract

The invention provides a preparation method of a polyethylene / POSS modified clay nanocomposite material. In the method, the layered inorganic clay is firstly modified with POSS with amino groups, and then the POSS modified clay is treated with alkyl aluminum and then N, N'-bis(2,6-diisopropylphenyl) acenaphthylenediimide (ArN=C(An)-C(An)=NAr, An=acenaphthene, Ar=2,6-( The i-Pr)2C6H3) nickel complex is used as a supported catalyst, and diethylaluminum chloride is used as a cocatalyst, and the supported catalyst is used to catalyze ethylene polymerization in situ in a non-polar solvent to prepare a polyethylene / POSS modified clay nanocomposite. The invention uses POSS to modify the inorganic clay, which avoids the disadvantage of thermal instability, and at the same time makes N, N'-bis(2,6-diisopropylphenyl)acenaphthyldiimide (ArN=C(An )-C(An)=NAr, An=acenaphthene, Ar=2,6-(i-Pr)2C6H3) Nickel complexes can be effectively fixed between the clay sheets, which is beneficial to the clay sheets in the ethylene polymerization process in the stripping. Compared with pure polyethylene, the heat stability and dynamic mechanical storage modulus of the polyethylene / POSS modified clay nanocomposite prepared by the invention are greatly improved.

Description

technical field [0001] The invention belongs to the field of polyethylene / clay nanocomposite materials, in particular to a preparation method of polyethylene / POSS (multifaceted oligomerized silsesquioxane) modified clay nanocomposite materials. Background technique [0002] The use of exfoliated layered clays as nanoreinforcement agents for polyethylene has been a research hotspot for many years. Studies have shown that the preparation of polyethylene / clay nanocomposites by in-situ polymerization is an effective method among various methods. In the preparation of polyethylene / clay nanocomposites by in-situ polymerization, there are two key factors that need attention: (1) The catalyst should be effectively loaded between the clay sheets during the loading process to facilitate the formation of clay sheets during ethylene polymerization. Peeling off, Jin YH et al. reported in Macromolecular Rapid Communications, 23, 135-140, 2002, the use of ammonium salts with hydroxyl grou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L23/06C08K3/34C08F110/02C08F4/70
Inventor 张黎明何富安江洪流
Owner SUN YAT SEN UNIV
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