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Preparation method for macromolecular adsorbent precursor diblock copolymer

A technology of block copolymer and adsorbent, which is applied in the field of preparation of diblock copolymer as precursor of polymer adsorbent, can solve the problems of widening distribution, uncontrollable reaction, explosion and so on.

Inactive Publication Date: 2017-07-07
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the precursor is usually synthesized by solution polymerization, the heat is not easily discharged during the reaction process, and it is easy to cause detonation, resulting in larger molecular weight, wider distribution, and uncontrollable reaction.

Method used

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  • Preparation method for macromolecular adsorbent precursor diblock copolymer
  • Preparation method for macromolecular adsorbent precursor diblock copolymer

Examples

Experimental program
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Effect test

Embodiment 1

[0025] With methyl acrylate (MA) as the first monomer, add 0.05 parts of MA, according to the degree of polymerization n(MA): n(BDMAT)=30, the amount of BDMAT added is 0.0017 parts, azobisisobutyronitrile (AIBN) As an initiator, 1,4-dioxane is used as a solvent, and is added to a round bottom flask, wherein the ratio of the amount of BDMAT to AIBN is controlled at 2:1, and the calculated AIBN added is 0.00085 parts, and the rotor is added to stir Make it completely dissolved, and after passing nitrogen gas for 30 minutes, stir and react in an oil bath at 70°C for 5 hours. After the reaction is completed, quickly put it in an ice bath to cool to terminate the reaction. The yellow liquid obtained after the reaction is precipitated twice in distilled water. To remove the solvent 1,4-dioxane and unreacted monomers, and finally vacuum dry to obtain a yellow viscous liquid polymethylacrylate PMA containing a carboxyl group at one end and a trisulfide bond at the other end 30 -SC(S))...

Embodiment 2

[0028]With methyl acrylate (MA) as the first monomer, add 0.05 parts of MA, according to the degree of polymerization n(MA): n(BDMAT)=30, the amount of BDMAT added is 0.0017 parts, azobisisobutyronitrile (AIBN) As an initiator, 1,4-dioxane is used as a solvent, and it is added to a round bottom flask, wherein the ratio of the amount of BDMAT to AIBN is controlled at 3:1, and the rotor is added to stir to make it all dissolve, and nitrogen gas is introduced for 30 minutes Finally, stir the reaction in an oil bath at 70°C for 5 hours. After the reaction is completed, quickly place it in an ice bath to cool to terminate the reaction. The yellow liquid obtained after the reaction is precipitated twice in distilled water to remove the solvent 1,4-dioxine Hexacyclic and unreacted monomers, and finally vacuum-dried to obtain a yellow viscous liquid polymethylacrylate PMA containing a carboxyl group at one end and a trisulfide bond at the other end 30 -SC(S))S.

[0029] Adopt the met...

Embodiment 3

[0031] With methyl acrylate (MA) as the first monomer, add 0.05 parts of MA, according to the degree of polymerization n(MA): n(BDMAT)=30, the amount of BDMAT added is 0.0017 parts, azobisisobutyronitrile (AIBN) As an initiator, 1,4-dioxane is used as a solvent, and it is added to a round bottom flask, wherein the ratio of the amount of BDMAT to AIBN is controlled at 4:1, and the rotor is added to stir to make it all dissolve, and nitrogen gas is introduced for 30 minutes Finally, stir the reaction in an oil bath at 70°C for 5 hours. After the reaction is completed, quickly place it in an ice bath to cool to terminate the reaction. The yellow liquid obtained after the reaction is precipitated twice in distilled water to remove the solvent 1,4-dioxine Hexacyclic and unreacted monomers, and finally vacuum-dried to obtain a yellow viscous liquid polymethylacrylate PMA containing a carboxyl group at one end and a trisulfide bond at the other end 30 -SC(S))S.

[0032] Adopt the me...

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Abstract

The invention relates to a preparation method for a macromolecular adsorbent precursor diblock copolymer. A macromolecular chain transfer agent PMA is compounded according to a RAFT polymerizing method which comprises the following steps: taking methyl acrylate as a first monomer, trithiocarbonate as a chain transfer agent, azodiisobutyronitrile as an initiator and 1,4-dioxane or N,N-dimethyl formamide as a solvent, thereby acquiring yellow viscous liquid polymethyl acrylate with carboxyl at one end and trithio sulfatide at the other end, and then taking N-isopropyl acrylamide as a second monomer for compounding polymethyl acrylate as the macromolecular chain transfer agent, thereby acquiring a diblock copolymer PMA-b-PNIPAM. According to the invention, RAFT polymerization is utilized to compound hydrophilic PMA as the chain transfer agent for the next stage reaction by using trithio ester with higher chain transfer constant as an active / controllable polymerized chain transfer agent. The diblock copolymer PMA-b-PNIPAM at different block ratio is compounded in the manner of changing the design for different degrees of polymerization.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a preparation method of a diblock copolymer as a precursor of a polymer adsorbent. Background technique [0002] Heavy metal pollutants have the characteristics of long residual time, easy accumulation, refractory degradation and wide sources, which have attracted the attention of many scientific researchers in recent years. The methods for treating heavy metal wastewater can be divided into three categories: chemical treatment, physical and chemical treatment, and biological treatment. In the chemical treatment method, heavy metal polymer adsorbent is a research hotspot. Heavy metal polymer adsorbent contains a large number of adsorption groups and has strong adsorption capacity. It can also introduce specific functional adsorption groups through molecular design to select heavy metal ions. Non-toxic adsorption, which is conducive to the recovery of high-purity heavy metal ions...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F220/14C08F220/54C08F2/38B01J20/26B01J20/30
CPCC08F293/005B01J20/264C08F2/38C08F220/14C08F220/54
Inventor 黄定海柳盼盼李纳川宋丽
Owner TIANJIN UNIV
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