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Block ionomer water-phase self-assembled nano capsule and preparation method thereof

A nanocapsule, ionomer technology, applied in microcapsule preparation, microsphere preparation, antifouling/underwater coatings, etc. The effect of big application prospects

Inactive Publication Date: 2013-10-30
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, the commonly used preparation methods of nanocapsules mainly include emulsion polymerization, interfacial and in-situ polymerization, etc.; however, emulsion polymerization requires a large amount of surfactant, which remains in the product and is difficult to remove, and the performance of nanocapsules is therefore affected. great influence

Method used

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  • Block ionomer water-phase self-assembled nano capsule and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Control the temperature of the constant temperature water bath at 50°C, first dissolve 4.9g of dimethylolpropionic acid in 7.4g of N-methyl-2-pyrrolidone to prepare a solution, and then mix the solution with 52g of 400 Add polyethylene glycol in the reactor, start the stirrer;

[0026] (2) Add 22g of isophorone diisocyanate dropwise to the above reaction kettle, after 30 minutes of continuous dripping, then raise the temperature to 80°C, add dibutyltin dilaurate, react for 3.5h, then cool down to 30°C, Add 3g of triethylamine, neutralize and react for 10 minutes to obtain block ionomer, the hydroxyl content of block ionomer is 2.8%;

[0027] (3) Add 9.17g of the above-generated block ionomer and 9.17g of N,N-dimethylformamide into the reactor, add 5g of hexamethylene diisocyanate biuret dropwise, and react for 29 minutes;

[0028] (4) Dissolve 7.30g of 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one in 3g of xylene, and add dropwise to the reacted product in step (3) f...

Embodiment 2

[0032] (1) Control the temperature of the constant temperature water bath to 70°C, first dissolve 6.4g of dimethylolpropionic acid in 9.6g of N-methyl-2-pyrrolidone to prepare a solution, and then mix the solution with 126g of 2000 molecular weight Add polyethylene glycol in the reactor, start the stirrer;

[0033] (2) Add 6g of isophorone diisocyanate dropwise to the above reaction kettle, after 36 minutes of continuous dripping, then raise the temperature to 80°C, add dibutyltin dilaurate, react for 4.5h, then cool down to 40°C, Add 4.8g of triethylamine, neutralize and react for 10 minutes to obtain a block ionomer, the hydroxyl content of the block ionomer is 2%;

[0034] (3) Add 5.06g of the above-generated block ionomer and 5.06g of N,N-dimethylformamide into the reactor, add 5g of hexamethylene diisocyanate biuret dropwise, and react for 31 minutes;

[0035] (4) Dissolve 5.19g of 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one in 2g of xylene, and add dropwise to the react...

Embodiment 3

[0039] (1) Control the temperature of the constant temperature water bath to 60°C, first dissolve 3.9g of dimethylolpropionic acid in 5.9g of N-methyl-2-pyrrolidone to prepare a solution, and then mix the solution with 74g of a molecular weight of 1000 Add polyethylene glycol in the reactor, start the stirrer;

[0040] (2) Add 6g of isophorone diisocyanate dropwise to the above reaction kettle, after 30 minutes of continuous dripping, then raise the temperature to 80°C, add dibutyltin dilaurate, react for 4 hours, then cool down to 40°C, add 2.4g of triethylamine, neutralized for 10min to obtain block ionomer;

[0041] (3) Add 6.07g of the above-generated block ionomer and 6.07g of N,N-dimethylformamide into the reactor, add 6.01g of hexamethylene diisocyanate biuret dropwise, and react for 24 minutes;

[0042] (4) Dissolve 8.30g of 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one in 4g of xylene, and add dropwise to the reacted product in step (3) for 35min continuous dripping; ...

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Abstract

The invention discloses a block ionomer water-phase self-assembled nano capsule and a preparation method thereof. The preparation method comprises the following steps: dissolving 3.9-6.4g of dimethylolpropionic acid in 5.9-9.6g of N-methyl-2-pyrrolidone to prepare a solution; adding the solution and 52-126g of polyethylene glycol into a reaction kettle, and dropwisely adding 6-22g of isophorone diisocyanate, thus obtaining a block ionomer; adding 5.06-9.17g of block ionomer and 5.06-9.17g of N,N-dimethyl formamide into the reaction kettle, and dropwisely adding 5-6.01g of hexamethylene diisocyanate biuret; and dropwisely adding 4.87-8.30g of 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one into 2-4g of dimethyl benzene solution, adding water, carrying out shear dispersion, standing, defoaming, and discharging to obtain the required 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one nano capsule.

Description

technical field [0001] The invention relates to the field of nanocapsules, in particular to a block ionomer water-phase self-assembled nanocapsule and a preparation method thereof. Background technique [0002] 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one, its structural formula is as follows: [0003] [0004] This is a new type of environment-friendly high-efficiency broad-spectrum organic antifouling agent. Its development and application are of great significance to the protection of the marine ecological environment and the promotion of the sustainable development of the marine economy. It was awarded the US President's Green Chemistry Challenge Award in 1996. This type of antifouling agent has been widely used. However, the biggest problem is that it will be released from the coating at a relatively fast and uncontrolled rate, resulting in a functional maintenance time of the coating that cannot meet the application requirements. [0005] Nanocapsule, also known a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/14C08G18/79C08G18/75C08G18/66C08G18/48C08G18/34C09D175/12C09D175/08C09D5/16
Inventor 胡剑青朱海军涂伟萍王锋
Owner SOUTH CHINA UNIV OF TECH