A kind of pyridyl-containing 1,3,4-oxadiazole water-soluble fluorescent polymer and its synthesis method

A technology of oxadiazole groups and fluorescent monomers, which is applied in the field of circulating water treatment agents, can solve the problems of complex post-purification treatment process, unfavorable safety and environmental protection, and numerous synthesis reaction steps, so as to achieve a safe and environmentally friendly synthesis process. Excellent water solubility and easy industrial operation

Active Publication Date: 2021-12-10
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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  • A kind of pyridyl-containing 1,3,4-oxadiazole water-soluble fluorescent polymer and its synthesis method
  • A kind of pyridyl-containing 1,3,4-oxadiazole water-soluble fluorescent polymer and its synthesis method

Examples

Experimental program
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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) Keep 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 8.5~9...

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 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 a reflux state, drop monomers 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 temperature was lower...

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 water-soluble fluorescent polymer containing pyridyl 1,3,4-oxadiazole and a synthesis method thereof, which specifically includes: (1) acrylic acid and 4-formylhydrazide pyridine in a dry phosphorus oxychloride environment In the system, negative pressure heating and reflux reaction for 5-6 hours to obtain fluorescent monomers; (2) Initiate polymerization of the synthesized fluorescent monomers, acrylic acid and maleic anhydride aqueous solution to synthesize water-soluble fluorescent monomers with a viscosity average molecular weight of 5000-10000 Label the aqueous solution of acrylic-maleic acid copolymer. The present invention utilizes unsaturated carboxylic acid containing carbon-carbon double bond and formic hydrazide of 1,3,4-oxadiazole containing pyridyl group to synthesize fluorescent monomer containing unsaturated carbon-carbon double bond, and further polymerizes into water-soluble fluorescent monomer Labeled copolymer; the method is simple and easy to operate, has low excitation energy, good concentration fluorescence linearity, mild reaction conditions, safe and environmentally friendly synthesis process, and is 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 Patents(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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