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Preparation method of epoxy acrylic acid extraction resin and application of epoxy acrylic acid extraction resin to extraction and separation of germanium

An epoxy acrylic acid extraction resin and epoxy acrylic acid extraction technology are applied in the field of germanium extraction and separation, which can solve the problems of extraction agent loss and achieve the effects of less extraction agent loss, simple synthesis method, and convenient recycling

Inactive Publication Date: 2017-07-07
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The invention provides a preparation method of epoxy acrylic acid extraction resin and its application in extracting and separating germanium. The invention is to chelate the extraction agent N235 inside the epoxy acrylic resin by suspension polymerization method to form extraction resin microspheres , which solves the problem of a large amount of extractant loss when the extraction resin prepared by physical impregnation is used to extract and separate germanium

Method used

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  • Preparation method of epoxy acrylic acid extraction resin and application of epoxy acrylic acid extraction resin to extraction and separation of germanium
  • Preparation method of epoxy acrylic acid extraction resin and application of epoxy acrylic acid extraction resin to extraction and separation of germanium
  • Preparation method of epoxy acrylic acid extraction resin and application of epoxy acrylic acid extraction resin to extraction and separation of germanium

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preparation example Construction

[0025] 1) Preparation of epoxy acrylic resin: Add 1-100 parts of epoxy resin to the device, then add 0.01-1 part of polymerization inhibitor p-methoxyphenol, 0.01-1 part of benzyldimethylamine, stir and heat up to After 80°C, use a constant pressure dropping funnel to add 1 to 50 parts of acrylic acid dropwise, and drop it within 1-2 hours, then raise the temperature to 100°C for 4-5 hours, and stop the reaction after the acid value is less than 10. Cool down to 80°C, add 1-50 parts of styrene, and stir for 100-120 minutes to prepare epoxy acrylic resin for later use.

[0026] 2) Preparation of epoxy acrylic acid extraction resin: Add 1-100 parts of deionized water, 1-10 parts of magnesium chloride solution, 1-20 parts of sodium hydroxide solution in sequence in the device, stir evenly, heat up to 75°C, and fully react 10-20 minutes, then use the constant pressure dropping funnel to add 1-50 parts of epoxy acrylic resin that has been prepared, 1-50 parts of extraction agent N2...

Embodiment 1

[0030] The preparation of embodiment 1 bisphenol A epoxy acrylic acid extraction resin

[0031] 1) Add 58.05g of bisphenol A epoxy resin into the device, then add 1.20g of p-methoxyphenol, 0.27g of benzyldimethylamine, stir and heat up to 80°C, then add 19.45g of it dropwise with a constant pressure dropping funnel Add acrylic acid dropwise within 1-2 hours, then raise the temperature to 100°C for 4-5 hours, stop the reaction after the acid value is less than 10, drop the temperature to 80°C, add 33.45g styrene, and stir for 100- 120min, prepared bisphenol A epoxy acrylic resin for subsequent use.

[0032] 2) Add 58ml of deionized water, 2.5ml of magnesium chloride solution (1mol / L), and 5ml of sodium hydroxide solution to the device in turn, stir evenly, heat up to 75°C, fully react for 10-20 minutes, and then use a constant pressure dropping funnel Add 10g of prepared bisphenol A epoxy acrylic resin dropwise, 10g of extractant N235, the mixed solution of 9.5g of TMPTA and N...

Embodiment 2

[0034] The preparation of embodiment 2 E51 epoxy acrylic extraction resin

[0035] 1) Add 58.80g of E51 epoxy resin to the device, then add 0.12g of p-methoxyphenol, 0.17g of triethylbenzyl ammonium, stir and raise the temperature to 80°C, add 19.45g of acrylic acid dropwise with a constant pressure dropping funnel , and drop it within 1-2h, then raise the temperature to 110°C and react for 4-5h, after the acid value is less than 10, stop the reaction, cool down to 60°C, add 34.50g of styrene, and stir for 30-60min , to prepare E51 epoxy acrylic resin for subsequent use.

[0036] 2) Add 58ml of deionized water, 2.5ml of magnesium chloride solution (1mol / L), and 5ml of sodium hydroxide solution to the device in turn, stir evenly, heat up to 75°C, fully react for 10-20 minutes, and then use a constant pressure dropping funnel Add 20g of prepared E51 epoxy acrylic resin, 20g of extractant N235, 9.2g of TMPTA and N-methylimidazolium rhenium ionic liquid dropwise, and then add 0.0...

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Abstract

The invention discloses epoxy acrylic acid extraction resin. A method comprises the following steps that 1, epoxy resin is added into a device, then polymerization inhibitors and benzyl dimethylamine are added, after stirring is conducted, crylic acid is dropwise added, a temperature rise reaction is conducted, styrene is added, stirring is conducted again, and epoxy acrylic acid resin is prepared; and 2, deionized water, a magnesium chloride solution and a sodium hydroxide solution are sequentially added into the device, are stirred evenly and have a reaction fully, then the epoxy acrylic acid resin, extraction agents N235, TMPTA and N methylimidazole rhenium ion mixed liquid are dropwise added in sequence and are stirred evenly, then acetophenone peroxide and cobalt iso-octoate are added, the rotation speed is adjusted to be 300-400 r / min, the temperature is increased to 80 DEG C, suspension polymerization is conducted for 80-120 min, beaded grain products are washed and dried, and then the epoxy acrylic acid extraction resin is obtained. The epoxy acrylic acid extraction resin is good in extraction and separation effect for germanium and high in selectivity, the preparation method is simple and low in cost and the epoxy acrylic acid extraction resin can be recycled conveniently and reused.

Description

technical field [0001] The invention belongs to the technical field of extracting and separating germanium, and in particular relates to a preparation method of epoxy acrylic acid extraction resin and its application in extracting and separating germanium. Background technique [0002] Germanium is a rare metal with good semiconductor properties. It is an indispensable and important element for new functional materials such as compound semiconductors, electro-optical materials, and special alloys. It has great development potential. However, germanium is rarely found in nature. Most of the independent mineral deposits are doped with other elements. Therefore, the extraction and separation process of germanium has become a research hotspot. The germanium produced in modern industry mainly comes from by-products of copper, zinc and lead smelting. The production method is complicated, the yield is low, the cost is high, and the environment is seriously polluted. Contents of t...

Claims

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Application Information

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IPC IPC(8): C22B3/28C22B41/00C08G59/17
CPCC08G59/1466C22B41/00C22B3/28Y02P10/20
Inventor 房大维周忠凯单炜军熊英臧树良
Owner LIAONING UNIVERSITY
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