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Pyridyl-containing 1, 3, 4-oxadiazole water-soluble fluorescent polymer and synthesis method thereof

A polymer, oxadiazole group technology, used in chemical instruments and methods, luminescent materials, descaling and water softening, etc., can solve problems such as unfavorable safety and environmental protection, complex post-purification treatment process, strict reaction conditions, etc. problems, to achieve the effect of safety and environmental protection in the synthesis process, excellent water solubility, and the process is simple and easy to operate.

Active Publication Date: 2020-04-28
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing disclosed fluorescent tracer monomers for polycarboxylate scale inhibitors and dispersants for water treatment agents usually use high temperature, high pressure or inert gas environments for synthesis, and the reaction conditions are strict, or the synthesis reaction steps Various technical problems such as complex post-purification treatment process are not conducive to safety and environmental protection

Method used

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  • Pyridyl-containing 1, 3, 4-oxadiazole water-soluble fluorescent polymer and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1 (synthesis of unsaturated fluorescent monomers containing 1,3,4-oxadiazole groups)

[0024] (1) At room temperature, add 75.0g of acrylic acid with a mass content >99.5% and 129.6g of 4-formylhydrazinopyridine (molar ratio is about 1:1) into a 1000mL three-neck reactor with a drying device;

[0025] (2) Connect the reactor to the vacuum pump and maintain the pressure state of the system at -0.03 ~-0.04MPa, add 400.0g of phosphorus oxychloride after distillation and drying, and react under stirring conditions at 78±2°C under micro-reflux 7.5 hours until the system is yellow-brown uniform and transparent;

[0026] (3) Maintain the vacuum of the system within the range of -0.01~-0.02MPa, distill under reduced pressure until no liquid is distilled out of the system, distill out and recover 221.7g of phosphorus oxychloride, quickly add 480g of ice-water mixture to the kettle and use 30% hydrogen Sodium oxide aqueous solution adjusts the pH value of the system to 8...

Embodiment 2

[0032] At 60±2°C, dissolve 72g of maleic anhydride in 60g of deionized water, mix well and pour into the monomer dropping tank for later use; according to m 荧光单体 :m AA :m MA = 0.012:1:0.40 ratio, respectively weigh 2.16g of the fluorescent monomer synthesized in the above-mentioned embodiment 1, 50g of isopropanol, 200g of deionized water, 22.1g of hydrogen peroxide aqueous solution and 180g of acrylic acid with a mass percentage content of 27.5%. Put into the kettle in sequence according to a certain mass ratio; add a certain amount of sodium hydroxide aqueous solution to adjust the pH value and control the pH value of the system to 4.5; raise the temperature to reflux state, add monomer dropwise to initiate polymerization, and maintain the pH value of the system within the range of 4.0~4.5 , after the addition of the monomer was completed, the insulation reaction was carried out for 1 hour, the isopropanol was evaporated under negative pressure for recycling, and the temper...

Embodiment 3

[0034] Dissolve 150g of maleic anhydride in 100g of deionized water at 55±2°C, mix well and pour into the monomer dropping tank for later use; 荧光单体 :m AA :m MA= 0.020:1:0.30 ratio, respectively weigh 10.0g of the fluorescent monomer synthesized in the above embodiment 1, 120g of isopropanol, 1000g of deionized water, 50.8g of hydrogen peroxide aqueous solution and 500g of acrylic acid with a mass percentage content of 27.5% Put into the kettle in sequence according to a certain mass ratio; raise the temperature to the reflux state, drop the monomer to initiate polymerization, maintain the pH value of the system in the range of 4.0~4.5, after the monomer is added dropwise, keep the reaction for 1.5 hours, and steam out the isopropyl under negative pressure Alcohol recycling, cooling down and adding water to dilute to obtain 1618.21g of a yellow fluorescently labeled MA-AA copolymer sodium salt solution with an active content of 40.61%. After testing, the viscosity-average mole...

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Abstract

The invention discloses a pyridyl-containing 1, 3, 4-oxadiazole water-soluble fluorescent polymer and a synthesis method thereof. The synthesis method specifically comprises the steps that 1, acrylicacid and 4-formylhydrazine pyridine are subjected to a negative-pressure heating reflux reaction for 5-6 h in a dry phosphorus oxychloride environment system, and a fluorescent monomer is obtained; and (2) polymerization of the synthesized fluorescent monomer, acrylic acid and a maleic anhydride aqueous solution are initiated to synthesize a water-soluble fluorescently-labeled acrylic acid-maleicacid copolymer aqueous solution with the viscosity-average molecular weight of 5000-10000. The preparation method comprises the following steps: synthesizing a fluorescent monomer containing unsaturated carbon-carbon double bonds by utilizing unsaturated carboxylic acid containing the carbon-carbon double bonds and formyl hydrazine of pyridyl-containing 1, 3, 4-oxadiazole, and further polymerizingto obtain the water-soluble fluorescence labeling copolymer; the method is simple in process, easy to operate, low in excitation energy, good in concentration fluorescence linearity, mild in reactioncondition, safe and environment-friendly in synthesis process and easy to realize large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of application of circulating water treatment agents, and in particular relates to a water-soluble fluorescent polymer containing pyridyl 1,3,4-oxadiazole and a synthesis method thereof. Background technique [0002] Water-soluble carboxylic acid copolymer has become an earlier water-soluble copolymer water treatment scale inhibitor developed at home and abroad. This type of product has a strong chelating and dispersing ability for calcium and magnesium ions in water, and the product is environmentally friendly. Pollution, no "eutrophication" of water bodies, and low production and use costs have always been valued and favored by people. Most of the products use water-soluble organic carboxylic acids such as acrylic acid as the main monomer. The use of organic phosphine agents can be used to determine the dosing cycle and dosage through online detection and analysis of phosphorus content in water, while the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/06C08F226/06C08F222/06C02F5/12C07D413/04C09K11/06
CPCC08F220/06C02F5/12C07D413/04C09K11/06C09K2211/145C09K2211/1466C09K2211/1475C08F226/06C08F222/06
Inventor 王燕平程终发李鹏飞陆久田刘全华齐晓婧王宇
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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