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Preparing method of polysaccharide-based microsphere with dithizone structure

A technology of dithizone and microspheres, which is applied to the preparation of microspheres, microcapsule preparations, chemical instruments and methods, etc., can solve problems such as modification of dithizone, and achieve the effects of mild reaction conditions, broad application prospects and simple process.

Inactive Publication Date: 2019-08-09
程兰青
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the main bodies of solid substrates are mostly polymer resins and microspheres, and there is no case of modifying dithizone on polysaccharide microsphere media.

Method used

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  • Preparing method of polysaccharide-based microsphere with dithizone structure
  • Preparing method of polysaccharide-based microsphere with dithizone structure
  • Preparing method of polysaccharide-based microsphere with dithizone structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 4g of agarose, put it in 100mL of deionized water, and heat it to 90°C in a 250mL flask to dissolve; measure 400mL of liquid paraffin, put it in a 1L beaker, add 1g of Span 20, 3g of Span 60, and heat to 70°C. Slowly pour the agarose aqueous solution into liquid paraffin, stir at high speed, and slowly cool down to 25°C at a rate of 1°C / 2min. After the reaction is completed, filter out the microspheres, wash the microspheres with ethanol and deionized water respectively, sieve, and take Appropriate particle size range for use.

[0028] Drain the washed microspheres, weigh 10g of microspheres and put them in a 250mL flask, add 50mL of deionized water, 0.8g of PEG1000, and 10g of epichlorohydrin, and react at 40°C for 16h. The microspheres were washed with ethanol and deionized water, respectively.

[0029] The washed microspheres were drained, weighed 10g of microspheres and placed in a 250mL flask, added 100mL of acetone solution containing 4g of dithizone, and r...

Embodiment 2

[0031] Weigh 4g of dextran, put it in 100mL of deionized water, and heat it to 80°C in a 250mL flask to dissolve; measure 300mL of cyclohexane, put it in a 1L beaker, add 4g of Span 80, heat to 80°C, and dissolve the agarose Slowly pour the aqueous solution into cyclohexane, stir at high speed, and slowly cool down to 25°C at a rate of 1°C / 2min. After the reaction is completed, filter out the microspheres, wash the microspheres with ethanol and deionized water, and sieve to obtain suitable particles. spare diameter range.

[0032] Drain the washed microspheres, weigh 10g of microspheres and put them in a 250mL flask, add 30mL of deionized water, 0.5g of PEG800, and 15g of epichlorohydrin, and react at 40°C for 16h. The microspheres were washed with ethanol and deionized water, respectively.

[0033] The washed microspheres were drained, weighed 10g of microspheres and placed in a 250mL flask, added 100mL of acetone solution containing 7g of dithizone, and reacted with mechani...

Embodiment 3

[0036] Weigh 8g of dextran in 100mL deionized water, heat to 80°C in a 250mL flask to dissolve; measure 600mL of cyclohexane, put it in a 1L beaker, add 4g of Span 80, 2g of oleic acid, and heat to 80°C , slowly pour the agarose aqueous solution into cyclohexane, stir at high speed, and slowly cool down to 25°C at a speed of 1°C / 2min. After the reaction is completed, filter out the microspheres, wash the microspheres with ethanol and deionized water, and sieve , take the appropriate particle size range for later use.

[0037] The washed microspheres were drained, weighed 10g of microspheres and placed in a 250mL flask, added 60mL of deionized water, 0.2g of tetrabutylammonium bromide, and 20g of epoxy bromide, and reacted at 40°C for 16h. The microspheres were washed with ethanol and deionized water, respectively.

[0038] The washed microspheres were drained, weighed 10g of microspheres and placed in a 250mL flask, added 100mL of acetone solution containing 5g of dithizone, ...

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Abstract

The invention discloses a preparing method of a polysaccharide-based microsphere with a dithizone structure. According to the method, agarose and glucan are taken as aqueous-phase raw materials, cyclohexane, liquid paraffin and methylbenzene are taken as oil phases, Span80, Span60 and the like are taken as emulsifiers, and reversed phase suspension is utilized for preparing the polysaccharide microsphere; then epoxy chloropropane or epibromohydrin is taken as halogen ligand, and then the halogen is modified on the surface of the microsphere under catalysis of PEG or tetrabutylammonium bromide;then a dithizone acetone solution is added, and the dithizone polysaccharide microsphere is obtained after a reaction. The method is easy to operate and mild in condition, and has a wide applicationprospect in the field of trace heavy metal analysis and the field of heavy metal pollution removal.

Description

technical field [0001] The invention relates to a polysaccharide microsphere with a functional group, in particular to a preparation method of a polysaccharide-based microsphere with a dithizone structure. Background technique [0002] Yellow dithizone (C 13 h 12 N 4 S), also known as lead reagent, blue-black crystalline powder. It is prone to oxidation reaction in the air, so its stability is relatively poor, and sulfur dioxide aqueous solution can be used to protect its solubility. Dithizone is an excellent heavy metal chelating agent because its structure contains multiple N and S electron-donating ligands. It is often used for color development in the photometric analysis of trace heavy metals. It is complexed with metal ions Will appear yellow, orange or red. [0003] Because dithizone-structured molecules have a good complexing effect on metal ions, they have good application effects in the detection and adsorption of trace and trace metal ions. It plays a very i...

Claims

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Application Information

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IPC IPC(8): C08J7/12C08J3/16B01J13/02B01J20/24B01J20/28B01J20/30B01J20/286C02F1/28C08L5/12C08L5/02C02F101/20
CPCB01J13/02B01J20/22B01J20/24B01J20/28021B01J20/286C02F1/286C02F2101/20C08J3/16C08J7/12C08J2305/02C08J2305/12
Inventor 程兰青
Owner 程兰青
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