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Preparation method of polyurethane RAFT (reversible addition fragmentation chain transfer) reagent

A technology of polyurethane and reagents, which is applied in the field of preparation of polyurethane RAFT reagents, can solve the problems of complex process, low yield, and inability to produce on a large scale, and achieve the effect of simple process and convenient purification

Active Publication Date: 2018-05-11
SHANGRAO NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The position of the trithioester group of the above-mentioned polyurethane RAFT reagent is mostly based on the main chain, and the position of the trithioester group of the polyurethane RAFT reagent described in CN105199050A is on the side chain, but it is prepared from dibasic alcohol containing trithioester , the raw material needs to be prepared and purified separately, and the yield is not high, the process is complicated, and it cannot be produced on a large scale

Method used

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  • Preparation method of polyurethane RAFT (reversible addition fragmentation chain transfer) reagent
  • Preparation method of polyurethane RAFT (reversible addition fragmentation chain transfer) reagent
  • Preparation method of polyurethane RAFT (reversible addition fragmentation chain transfer) reagent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Step 1, add 8.91g (0.04mol) isophorone diisocyanate, 3.08g (0.028mol) 3-chloro-1,2-propanediol, 1.48g (0.01mol) dimethylol butyric acid, 0.04g (6.33×10 -5 mol) dibutyltin dilaurate, 5.00 mL of anhydrous acetone, stirred and reacted at 80°C for 6 hours, added 0.52 g (0.004 mol) of n-octanol and reacted for 2 hours, the reaction was completed, and set aside.

[0029] Step 2, the reaction kettle is placed on an ice bath, 5.67g (0.028mol) of dodecyl mercaptan is added thereto, under magnetic stirring, 3.73g of 30wt% NaOH aqueous solution is slowly added dropwise to the flask, and after 15min, under stirring Add acetone 5.00mL, after fully dissolved, add 2.13g (0.028mol) CS 2 , continue to stir the reaction for 1h. Then add the polyurethane prepared in step 1, stir and react at 30°C for 12 hours, the product is precipitated in 250mL volume ratio of 1:1 methanol / water, after the precipitate is dried at room temperature, it is placed in a vacuum drying oven at 90°C and dried...

Embodiment 2

[0031] Step 1. Add 8.91g (0.04mol) isophorone diisocyanate, 7.33g (0.028mol) 2,2-dibromomethyl-1,3-propanediol, 1.48g (0.01mol) dihydroxy Methylbutyric acid, 0.04g (6.33×10 -5 mol) dibutyltin dilaurate, 5.00 mL of anhydrous acetone, stirred and reacted at 80°C for 6 hours, added 0.52 g (0.004 mol) of n-octanol and reacted for 2 hours, the reaction was completed, and set aside.

[0032] Step 2, the reaction kettle is placed on an ice bath, 5.67g (0.028mol) of dodecyl mercaptan is added thereto, under magnetic stirring, 3.73g of 30wt% NaOH aqueous solution is slowly added dropwise to the flask, and after 15min, under stirring Add acetone 5.00mL, after fully dissolved, add 2.13g (0.028mol) CS 2 , continue to stir the reaction for 1h. Then add the polyurethane prepared in step 1, stir and react at 30°C for 12 hours, the product is precipitated in 250mL volume ratio of 1:1 methanol / water, after the precipitate is dried at room temperature, it is placed in a vacuum drying oven at ...

Embodiment 3

[0034] Step 1. Add 6.73g (0.04mol) hexamethylene diisocyanate, 3.08g (0.028mol) 3-chloro-1,2-propanediol, 1.07g (0.008mol) dimethylol propionic acid, 0.05g (7.92×10 -5 mol) dibutyltin dilaurate, 5.00mL of anhydrous acetone, stirred and reacted at 85°C for 8h, added 1.04g (0.008mol) of n-octanol and reacted for 2h, the reaction was completed and set aside.

[0035] Step 2, the reaction kettle is placed on an ice bath, 5.67g (0.028mol) of dodecyl mercaptan is added thereto, and under magnetic stirring, 3.73g of 30wt% NaOH aqueous solution is slowly added dropwise to the flask, and after 15min, under stirring Add acetone 5.00mL, after fully dissolved, add 2.13g (0.028mol) CS 2, continue to stir the reaction for 1h. Then add the polyurethane prepared in step 1, stir and react at 50°C for 6 hours, the product is precipitated in 250mL volume ratio of 2:1 methanol / water, after the precipitate is dried at room temperature, it is placed in a vacuum drying oven at 90°C and dried overn...

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Abstract

The invention relates to a preparation method of a polyurethane RAFT (reversible addition fragmentation chain transfer) reagent. The preparation method comprises steps as follows: diisocyanate, halogen-containing dihydricalcohol and a hydrophilic chain-extending agent are dissolved in a solvent and subjected to a reaction under the action of a catalyst, a polyurethane prepolymer is obtained, n-octanol is used for blocking, and functional polyurethane is obtained; lauryl mercaptan, carbon disulfide and sodium hydroxide as raw materials react, sodium lauryl sulfate is obtained, functional polyurethane is added, the mixture is stirred to react for a couple of hours while heated, precipitation is performed in methanol / water, and the polyurethane RAFT reagent is obtained. The method is simple in synthesis, facilitates purification and can be used for preparing a grafted copolymer.

Description

technical field [0001] The invention belongs to the field of macromolecular materials, and in particular relates to a preparation method of polyurethane RAFT reagent, a polymer containing trithioester functional group used for reversible addition-fragmentation chain transfer polymerization. Background technique [0002] In 1956, Szwarc proposed the concept of active polymerization. The characteristics of this polymerization are no termination, no transfer, and the initiation rate is much greater than the growth rate. Even if the polymerization reaction is terminated, the polymer chain remains active, and new monomers continue to be added, and the polymerization reaction is complete. keep going. In 1998, Rizzardo et al first proposed the reversible addition-fragmentation chain transfer (RAFT) living free radical polymerization, which is characterized by the reversible chain transfer reaction between the growing free radical and the special chain transfer agent, so as to reali...

Claims

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Application Information

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IPC IPC(8): C08G18/83C08G18/75C08G18/32C08G18/34C08G18/73C08F283/00
CPCC08F283/006C08G18/348C08G18/3808C08G18/381C08G18/73C08G18/755C08G18/834C08F2438/03
Inventor 郑劼廖承莉王珊
Owner SHANGRAO NORMAL UNIV
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