Preparation method for perylene bisimide polyurethane liquid crystal non-covalent modified graphene

A perylene imide polyurethane, non-covalent modification technology, applied in dyeing polymer organic compound treatment, fibrous filler, etc., to achieve the effect of simple synthesis process, wide source of raw materials, and less environmental pollution

Active Publication Date: 2014-09-24
绍兴盖诺超菱润滑材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the above studies, graphene oxide was grafted and modified with liquid crystals, and peryleneimide polyurethane liquid crystal non-covalently modified graphene was prepared with perylene anhydride as a raw material, and there is no literature report so far.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Add 0.5 grams of perylene anhydride to 30 milliliters of N-methylpyrrolidone, then add 0.13 grams of zinc acetate and heat up to 160°C, then stir to dissolve and add 0.268 grams of diglycolamine, react at constant temperature for 12 hours, and wait for the reaction to complete Finally, pour the obtained reaction liquid into absolute ethanol to precipitate the material, filter, and vacuum-dry to obtain the hydroxyl-terminated perylene imide.

[0022] (2) Dissolve 0.25 g of the hydroxyl-terminated perylene imide prepared in step (1) in 20 ml of N,N-dimethylformamide, then add 0.093 g of hexamethylene diisocyanate and 0.02 g of catalyst dilaurel diisobutyltin acid, in N 2 Under protection, heat up to 60°C and react for 6 hours, then add 0.11 g of polyethylene glycol-200, heat up to 90°C and continue to react for 8 hours. After the reaction, pour the obtained reaction solution into distilled water to precipitate and discharge the material, filter, and vacuum dry , Pery...

Embodiment 2

[0027] (1) Add 0.8 grams of perylene anhydride to 32 milliliters of N-methylpyrrolidone, then add 0.2 grams of zinc acetate and heat up to 160 ° C, then stir and dissolve and add 0.429 grams of diglycolamine, react at constant temperature for 12 hours, and wait for the reaction to complete Finally, pour the obtained reaction liquid into absolute ethanol to precipitate the material, filter, and vacuum-dry to obtain the hydroxyl-terminated perylene imide.

[0028] (2) Dissolve 0.4 g of the hydroxyl-terminated perylene imide prepared in step (1) in 32 ml of N,N-dimethylformamide, then add 0.148 g of hexamethylene diisocyanate and 0.04 g of catalyst dilaurel diisobutyltin acid, in N 2 Under protection, raise the temperature to 60°C for 6 hours, then add 0.176 g of polyethylene glycol-200, raise the temperature to 92°C and continue the reaction for 8 hours. After the reaction, pour the obtained reaction solution into distilled water to precipitate the material, filter, and vacuum d...

Embodiment 3

[0033] (1) Add 1 gram of perylene anhydride to 40 milliliters of N-methylpyrrolidone, then add 0.25 grams of zinc acetate and heat up to 160°C, then stir to dissolve and add 0.536 grams of diglycolamine, react at constant temperature for 12 hours, and wait for the reaction to complete Finally, pour the obtained reaction liquid into absolute ethanol to precipitate the material, filter, and vacuum-dry to obtain the hydroxyl-terminated perylene imide.

[0034] (2) Dissolve 0.5 g of the hydroxyl-terminated perylene imide prepared in step (1) in 40 ml of N,N-dimethylformamide, then add 0.185 g of hexamethylene diisocyanate and 0.05 g of catalyst dilaurel diisobutyltin acid, in N 2Under protection, heat up to 63°C and react for 6 hours, then add 0.22 g of polyethylene glycol-200, heat up to 94°C and continue to react for 8 hours. After the reaction, pour the obtained reaction solution into distilled water to precipitate, filter, and vacuum dry , Perylene imide polyurethane liquid c...

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Abstract

The invention discloses a preparation method for perylene bisimide polyurethane liquid crystal non-covalent modified graphene. The preparation method comprises the following steps: adding perylene and zinc acetate into N-methyl pyrrolidone, stirring and heating to 150-160 DEG C, adding diglycolamine, reacting for 12 hours, pouring into absolute ethyl alcohol for precipitating and discharging, filtering, and drying in vacuum to obtain hydroxyl-terminated perylene bisimide; taking and dissolving the hydroxyl-terminated perylene bisimide into N, N-dimethyl formamide, adding hexamethylene diisocyanate and a catalyst, heating to 60-65 DEG C and reacting for 6 hours under protection of N2, adding polyethylene glycol, heating to 90-95 DEG C and reacting for 8 hours, pouring reaction liquid into distilled water for precipitating and discharging, filtering, and drying in vacuum to obtain perylene bisimide polyurethane liquid crystals; and taking and dissolving the perylene bisimide polyurethane liquid crystals into chloroform, adding graphene, ultrasonically treating for 2-3 hours, carrying out suction filtration, washing by chloroform, and drying in vacuum to obtain the perylene bisimide polyurethane liquid crystal non-covalent modified graphene. The method disclosed by the invention has the advantages of being wide in material source, simple in process, low in price, small in pollution and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer material modification, in particular to a method for preparing peryleneimide polyurethane liquid crystal non-covalently modified graphene. Background technique [0002] Epoxy resin (EP) has excellent properties such as chemical corrosion resistance, electrical insulation, strong adhesion, good stability and small shrinkage, and it is low in cost, and has the advantages of flexible formula composition and processing methods, etc. It is widely used in the fields of adhesives, coatings, potting materials, structural materials and fiber-reinforced composite materials, and is one of the most widely used matrix resins in polymer-based composite materials. However, due to the high crosslinking density and large internal stress of the cured epoxy resin, there are disadvantages such as brittleness, poor fatigue resistance, and low heat resistance. Certain restrictions. Therefore, the use of graphene, liq...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/46C09C3/10C08G18/73C08G18/48C08G18/38
Inventor 陆绍荣曾岑肖仙娥潘露露虞锦洪徐旭
Owner 绍兴盖诺超菱润滑材料有限公司
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