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Dechlorinating agent as well as preparation method and application thereof

A chlorine removal agent and contact reaction technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problem of high chlorine content

Active Publication Date: 2022-04-26
智仑超纯环氧树脂(西安)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The application provides a chlorine removal agent and its preparation method and application. The chlorine removal agent has selectivity for chloride ions, can capture the chloride ions in epoxy resin, and can be recycled at the same time to save costs, so as to solve the traditional The problem of high chlorine content in the preparation process of epoxy resin

Method used

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  • Dechlorinating agent as well as preparation method and application thereof
  • Dechlorinating agent as well as preparation method and application thereof
  • Dechlorinating agent as well as preparation method and application thereof

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preparation example Construction

[0044] The second aspect of the present application provides a preparation method of a chlorine removal agent, and is prepared in the following manner:

[0045] Firstly, using triethynylamine and meta-azidobenzene as raw materials, using copper sulfate pentahydrate and sodium ascorbate as catalysts, the intermediate I was obtained through the click reaction of azide and alkyne, and then the intermediate I was obtained by the addition reaction of alkyne and carboxyl groups. The terminal double bond intermediate II is finally used to obtain the recyclable chlorine removal agent by self-polymerization of the intermediate II.

[0046] Please refer to the attached figure 1 , with figure 1 The synthesis and dechlorination mechanism diagram of the dechlorination agent provided for the embodiment of the application, such as figure 1 Shown, the preparation method of this chlorine removal agent may further comprise the steps:

[0047] 1) Add a mixed liquid of water and tert-butanol i...

Embodiment 1

[0052] Add 61.34g of mixed solvent (the mass ratio of water and tert-butanol is 1:1) into a three-necked flask equipped with a stirrer, and then add 9.96g of catalyst (the molar ratio of copper sulfate pentahydrate and sodium ascorbate is 1:2) , the temperature was raised to 60°C. Then 8.9g (0.1mol) of triethynylamine and 16g (0.1mol) of m-azidobenzene were dissolved in 20g of mixed solvent, and slowly added dropwise to the three-necked flask, the dropping time was kept at 5h, and the reaction was carried out for 10h, under the protection of argon throughout the process. . After the reaction was completed, it was cooled to room temperature, extracted with dichloromethane, separated to obtain an organic phase, dried with anhydrous sodium sulfate, filtered, and then rotary evaporated to remove the dichloromethane to obtain intermediate I.

[0053] Dissolve 24.9 (0.05mol) of intermediate I and 7.2 (0.1mol) of acrylic acid in 48.15g of acetone and place them in the reactor, add 0...

Embodiment 2

[0056] Add 140g mixed solvent (the mass ratio of water and tert-butanol is 1:1) in the there-necked flask equipped with stirrer, then add 13.34g catalyst (wherein the mol ratio of copper sulfate pentahydrate and sodium ascorbate is 1:2), The temperature increased to 65°C. Then 10.68g (0.12mol) of triethynylamine and 16g (0.1mol) of m-azidobenzene were dissolved in 20g of mixed solvent, and slowly added dropwise to the three-necked flask, the dropping time was kept at 6h, the reaction was 13h, and the whole process was protected by argon. . After the reaction was completed, it was cooled to room temperature, extracted with dichloromethane, separated to obtain an organic phase, dried with anhydrous sodium sulfate, filtered, and then rotary evaporated to remove the dichloromethane to obtain intermediate I.

[0057] Dissolve 24.9 (0.05mol) of intermediate I and 7.92 (0.11mol) of acrylic acid in 76.58g of acetone and place them in a reactor, add 1.64g of sodium hydroxide as a cata...

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Abstract

The invention provides a dechlorinating agent and a preparation method and application thereof.The preparation method comprises the steps that firstly, in a first organic solvent, in the atmosphere that copper sulfate pentahydrate and sodium ascorbate serve as catalysts and first protective gas, a mixed solution of triacetylene amine and m-azidobenzene is dropwise added into the first organic solvent, a first contact reaction is carried out, and a second contact reaction is carried out; a first product is obtained; then, extracting and separating the first product to obtain an organic phase of the first product; drying the organic phase, filtering, and performing rotary evaporation to obtain an intermediate I; further, in a second organic solvent, under the action of sodium hydroxide as a catalyst, performing a second contact reaction on a mixed solution of the intermediate I and acrylic acid, and performing rotary evaporation to obtain an intermediate II; and further, by taking water as a solvent, controlling the intermediate II and an ammonium persulfate aqueous solution to carry out a third contact reaction in the atmosphere of a second protective gas, and carrying out rotary evaporation to obtain the dechlorinating agent. The dechlorinating agent is applied to synthesis of epoxy resin.

Description

technical field [0001] The present application relates to the technical field of chlorine removal agents, in particular to a chlorine removal agent and its preparation method and application. Background technique [0002] Chlorine is a widely existing element, and its compounds are also used in more and more aspects. For example, in the electronics industry, epoxy resins are often used as encapsulants and adhesives for electronic components, but during the synthesis of epoxy resins, because of the presence of epichlorohydrin intermediates, epoxy resins are often used A certain amount of elemental chlorine is present. However, if the chlorine content in the epoxy resin is too high, it will be hydrolyzed to produce hydrochloric acid under certain circumstances, causing corrosion of electronic components. Therefore, it is necessary to minimize the chlorine content during the preparation of epoxy resins. [0003] In the related art, the chlorine removal method in the preparat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F122/26B01J20/26B01J20/30
CPCC08F122/26B01J20/261B01J2220/4812Y02W30/62
Inventor 杜彪
Owner 智仑超纯环氧树脂(西安)有限公司
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