Closed isocyanate coupling agent and application thereof

A technology of blocking isocyanate and isocyanate, which is applied in the direction of fibrous fillers, compounds of group 4/14 elements of the periodic table, and dyed organosilicon compounds. Use requirements, lower physical and mechanical properties of nylon composite materials, etc., to achieve the effect of improving dispersion state, increasing molecular weight, and strong reactivity

Active Publication Date: 2014-05-28
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, as the amount of thermally conductive fillers increases, the physical and mechanical properties of nylon composites decrease; and because the inorganic surface is hydrophilic, it is difficult to wet and disperse in the nylon matrix, and there are hydroxyl groups on the surface, and the surface energy is relatively large. , fillers always tend to agglomerate, and coupling agents are commonly used to modify the surface of thermally conductive fillers
For example, Lin Xiaodan prepared thermally conductive and insulating nylon plastics by blending and extruding nylon 66 and large particle size MgO. KH-560 was used to modify the surface of MgO. When the amount of MgO added was 70%, the thermal conductivity of the composite material reached 1.90. W / (m K), but the tensile strength and bending strength are reduced to 41.4MPa and 70.61 MPa respectively, and the notched impact strength is also reduced to 3.3kJ / m 2 , the physical and mechanical properties of composite materials cannot meet the actual use needs of special fields

Method used

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  • Closed isocyanate coupling agent and application thereof
  • Closed isocyanate coupling agent and application thereof
  • Closed isocyanate coupling agent and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Weigh 15g of isocyanate propyltriethoxysilane, dilute it with 25ml of anhydrous toluene and add it into a 250ml three-necked flask, then weigh 6.3396g of methyl ethyl ketone oxime and dissolve it in 25ml of anhydrous toluene, transfer it to a constant pressure funnel, add methyl ethyl ketone dropwise Oxime, the dropwise addition process controls the reaction temperature not to exceed 40°C, and the dropwise addition time is 0.5h; after the dropwise addition is completed, keep the temperature for 0.5h, then rise to 80°C for 4h reaction, cool to room temperature, evaporate the solvent, and obtain methyl ethyl ketoxime blocked isocyanate propane base triethoxysilane coupling agent. Such as figure 1 , methyl ethyl ketoxime blocked isocyanate propyl triethoxysilane infrared data: wave number 2274cm -1 At -NCO characteristic absorption peak disappears, 1730cm -1 The carbonyl absorption peak in -NHCOO appears at 3351cm -1 Appeared -NH special absorption peak, 1382, 1443cm ...

Embodiment 2

[0038] Weigh 8g of isocyanate propyltrimethoxysilane, dilute it with 25ml of anhydrous toluene and add it into a 250ml three-necked flask, then weigh 3.7346g of methyl ethyl ketone oxime and dissolve it in 25ml of anhydrous toluene, transfer it to a constant pressure funnel, add methyl ethyl ketone oxime dropwise , the dropping process controls the reaction temperature not to exceed 40°C, and the dropping time is 0.6h; after the dropping is completed, the temperature is kept constant for 0.6h, then raised to 80°C for 5h, cooled to room temperature, and the solvent is evaporated to obtain methyl ethyl ketoxime blocked isocyanate coupling agent. Such as figure 2 , methyl ethyl ketoxime blocked isocyanate propyl trimethoxysilane infrared data: wave number 2274cm -1 At -NCO characteristic absorption peak disappears, 1731cm -1 The carbonyl absorption peak in -NHCOO appears at 3353cm -1 Appeared -NH special absorption peaks, 1377, 1442cm -1 Respectively -CH 3 and -CH 2 Curve...

Embodiment 3

[0043] Weigh 10g of isocyanate propyltriethoxysilane, dilute it with 25ml of anhydrous toluene and add it to a 250ml three-necked flask, then weigh 2.9550g of acetone oxime and dissolve it in 25ml of anhydrous toluene, transfer it to a constant pressure funnel, and add acetone dropwise Oxime, the dropwise addition process controls the reaction temperature not to exceed 40°C, and the dropwise addition time is 0.5h; after the dropwise addition, the temperature is kept at a constant temperature for 0.5h, and then raised to 80°C for 5h reaction, cooled to room temperature, and the solvent is evaporated to obtain acetone oxime blocked isocyanate. joint agent. Such as image 3 , acetone oxime blocked isocyanate propyltriethoxysilane infrared data: wave number 2274cm -1 At -NCO characteristic absorption peak disappears, 1730cm -1 The carbonyl absorption peak in -NHCOO appears at 3350cm -1 Appeared -NH special absorption peaks, 1383, 1447cm -1 Respectively -CH 3 and -CH 2 Curve...

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Abstract

The invention discloses a closed isocyanate coupling agent used for surface treatment for thermal conductive fillers and a thermal conductive insulating nylon composite material. When the coupling agent treats the thermal conductive fillers, a closed isocyanate group is not unblocked and generates a chemical bonding or physical adsorption action with the surfaces of the thermal conductive fillers. In the melting process, the isocyanate group can be unblocked and chemically reacts with amidogen or carboxyl on a nylon molecular chain end. The thermal conductive insulating nylon composite material comprises 100 parts of nylon, 25-40 parts of modified thermal conductive insulating filler, 5-25 parts of a flexibilizer and 1-10 parts of an addition agent. The materials are added into a high-speed mixing machine for mixing and then are extruded to obtain the thermal conductive insulating nylon composite material. The closed isocyanate coupling agent is used for a nylon substrate and can obviously improve the dispersity of the fillers in nylon. Meanwhile, the closed isocyanate coupling agent plays a role of chain extension, the thermal conductivity of the composite material achieves the operating requirement, the physical and mechanical properties cannot greatly decline, and actual use requirements are met.

Description

technical field [0001] The invention belongs to the field of resin-based heat-conducting composite materials, and specifically relates to a blocked isocyanate coupling agent and its application in processing heat-conducting and insulating fillers and in heat-conducting and insulating nylon composite materials. Background technique [0002] Nylon (polyamide) is a general term for thermoplastic resins containing repeated amide groups—[NHCO]—on the molecular main chain. It has a regular molecular structure and is an engineering plastic with high crystallinity and good comprehensive properties. It is widely used in electronics and electrical appliances. , automobiles, machinery and other fields. At present, with the high performance of electronic and electrical equipment, the miniaturization of automobiles, and the acceleration of the lightweight of mechanical equipment, the demand for nylon will increase. Especially when nylon is used as a structural material, high requirement...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C09C3/12C09C1/40C09C1/04C09C1/02C09C1/00C09C1/28C08L77/00C08L77/02C08L77/06C08K9/06C08K3/22C08K3/28C08K3/38C08K3/34
Inventor 徐卫兵孙芳周正发任凤梅马海红
Owner HEFEI UNIV OF TECH
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