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Preparation method of triblock polymers with suspension nanometer zero-valent irons

A technology of nano-zero-valent iron and polymers, applied in chemical instruments and methods, and other chemical processes, to achieve the effects of improving reactivity and suspension performance, increasing yield, and reducing environmental pollution

Inactive Publication Date: 2012-10-03
INST OF HYDROGEOLOGY & ENVIRONMENTAL GEOLOGY CHINESE ACAD OF GEOLOGICAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0015] The invention provides a method for preparing polymethacrylic acid-polymethyl methacrylate-polystyrenesulfonic acid triblock polymers by an improved atom radical transfer method, so as to solve many defects in the existing production process. The process includes the following steps:

Method used

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  • Preparation method of triblock polymers with suspension nanometer zero-valent irons
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  • Preparation method of triblock polymers with suspension nanometer zero-valent irons

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Embodiment 1

[0032] Embodiment 1: as Figure 6Shown, the preparation method of polymethacrylic acid-polymethylmethacrylate-polystyrenesulfonic acid triblock polymer (PMAA-PMMA-PSS) comprises the following steps:

[0033] A. Synthesis of PtBMA-PMMA-PSt: Add 4.88g of anisole, 0.19g of chlorotoluenesulfonyl, 0.35g of pentamethyldivinyltriamine and 4.26g of tert-butyl methacrylate to the reactor and stir to dissolve , and then freeze with liquid nitrogen, vacuumize, and blow nitrogen to deoxygenate (repeat three times), then add 0.11g CuCl under nitrogen protection, and then keep the reaction system at 60°C and continue to react under nitrogen blowing. After 12 hours of reaction, 1.61 g of anisole and 1.51 g of methyl methacrylate were added, and the reaction system was kept at 30° C. and the reaction was carried out under continuous nitrogen flow. After reacting for 12 hours, 34.21 g of anisole and 31.25 g of styrene were added, and the reaction system was kept at 80° C. under continuous nit...

Embodiment 2

[0036] A. Synthesis of PtBMA-PMMA-PSt: Add 9.51g of anisole, 0.19g of chlorotoluenesulfonyl, 0.51g of pentamethyldivinyltriamine and 8.53g of tert-butyl methacrylate to the reactor and stir to dissolve , and then freeze with liquid nitrogen, vacuumize, and blow nitrogen to remove oxygen (repeat three times), then add 0.15g CuCl under nitrogen protection, and then keep the reaction system at 50°C and continue to react under nitrogen blowing. After reacting for 10 hours, 4.51 g of anisole and 4.01 g of methyl methacrylate were added, and the reaction system was kept at 250° C. and the reaction was carried out under continuous nitrogen flow. After reacting for 10 hours, 65.51 g of anisole and 62.49 g of styrene were added, and the reaction system was kept at 85° C. and the reaction was carried out under continuous nitrogen flow. After reacting for 60 hours, the reaction mixture was diluted with 1L tetrahydrofuran (THF), then the diluted solution was filtered through a neutral alu...

Embodiment 3

[0039] A. Synthesis of PtBMA-PMMA-PSt: Add 13.89g of anisole, 0.38g of chlorotoluenesulfonyl, 1.04g of pentamethyldivinyltriamine and 12.79g of tert-butyl methacrylate to the reactor and stir to dissolve , and then freeze with liquid nitrogen, vacuumize, and blow nitrogen to deoxygenate (repeat three times), then add 0.29g CuCl under nitrogen protection, and then keep the reaction system at 40°C and continue to react under nitrogen blowing. After reacting for 11 hours, 4.89 g of anisole and 4.01 g of methyl methacrylate were added, and the reaction system was kept at 35° C. and the reaction was carried out under continuous nitrogen flow. After reacting for 11 hours, 98.88 g of anisole and 93.74 g of styrene were added, and the reaction system was kept at 75° C. and the reaction was carried out under continuous nitrogen flow. After 40 hours of reaction, the reaction mixture was diluted with 1.5L tetrahydrofuran (THF), then the diluted solution was filtered in a neutral alumina ...

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Abstract

The invention discloses a preparation method of triblock polymers with suspension nanometer zero-valent irons. The preparation method comprises the steps of utilizing an atom transfer radical polymerization(ATRP) method to synthetize triblock polymers of poly(t-butyl methacrylate), polymethyl methacrylate and polrvinyl benzene, hydrolyzing the poly(t-butyl methacrylate) to prepare polymethacrylicacid using trifluoroacetic acid, and finally sulfonating the polrvinyl benzene to prepare polystyrolsulfon acid using sulfuric acid acetyl. The method improves the original three-step reaction into aone-step reaction in the synthetic process of the polymers, thereby reducing the operation steps, reducing the consumption of raw materials, improving reaction stability and improving the productivity of aimed compounds; and adding trifluoroacetic acid in a hydrolysis process, so that the hydrolysis process is thorough and the reactivity and the suspension property of products are improved. The experiment results show that the triblock polymers comprise functional groups in required target products, the molecular weight can reach about 100 thousand, and the stabilization time of suspension effects of nanometer zero-valent irons can reach more than two months.

Description

technical field [0001] The invention relates to a preparation method of a polymer, in particular to a preparation method of a three-block polymer used for suspending nanometer zero-valent iron. Background technique [0002] Nano zero-valent iron has strong reducibility. It can efficiently reduce and degrade chlorinated hydrocarbons such as trichlorethylene in water, and can also repair heavy metal pollutants in groundwater through adsorption and reduction. It is a very good groundwater remediation agent. Another advantage of nano zero-valent iron is that its particle size is small, and it can be injected into the formation by in-situ injection method, so as to realize the in-situ remediation of pollutants in groundwater. However, pure nano-zero-valent iron is easy to precipitate in water, so scientists from various countries have developed a variety of suspending agents to achieve its stable suspension. [0003] Among various nano-zero-valent iron suspending agents, polymet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F8/12C08F8/36C08F220/14C08F212/08B01J20/26B01J20/30
Inventor 韩占涛张威马丽莎王平
Owner INST OF HYDROGEOLOGY & ENVIRONMENTAL GEOLOGY CHINESE ACAD OF GEOLOGICAL SCI
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