Preparation method of substituted pyridine carbonylhydrazone metal corrosion inhibitor

A metal corrosion inhibitor and a picolinyl hydrazone technology, which is applied in the field of preparation of a substituted picolinyl hydrazone metal corrosion inhibitor, can solve the problems of high hazard, large amount of corrosion inhibitor, unreasonable molecular design, etc. Good corrosion inhibition performance and good biodegradability

Inactive Publication Date: 2010-05-19
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, the amount of corrosion inhibitor is large, the cost is high, the molecular design is unreasonable, the synthesis

Method used

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  • Preparation method of substituted pyridine carbonylhydrazone metal corrosion inhibitor
  • Preparation method of substituted pyridine carbonylhydrazone metal corrosion inhibitor
  • Preparation method of substituted pyridine carbonylhydrazone metal corrosion inhibitor

Examples

Experimental program
Comparison scheme
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Example Embodiment

Example 1:

The methyl picolinate is one of methyl 2-picolinate, methyl 3-picolinate and methyl 4-picolinate.

Methyl 2-picolinate and hydrazine hydrate were mixed in a molar ratio of 1:1, and 4 times the volume of hydrazine hydrate was used as a solvent for the reaction in a three-necked flask. The mixture was refluxed at 75°C and reacted with magnetic stirring for 7 hours to obtain The product was distilled under reduced pressure, recrystallized with absolute ethanol, and dried to obtain 2-picolinic acid hydrazide. Then, 2-picolinic acid hydrazide and o-vanillin are reacted at a molar ratio of 1:1, 3 times the mass of picolinic acid hydrazide as a solvent, and then refluxed at 80°C and reacted with magnetic stirring for 8 hours, cooling, A large amount of light yellow crystals precipitated, filtered with suction, washed with absolute ethanol, and recrystallized to obtain a light yellow solid. The infrared spectrum shows that it is at 1681cm -1 There is a characteristic absorp...

Example Embodiment

Example 2:

Mark in the figure: Methyl A-picolinate (R 1 -COOCH 3 ), C-hydrazine hydrate, B-o-vanillin, D-solvent.

Use methyl 3-picolinate and hydrazine hydrate in a molar ratio of 1:1, and 4 times the volume of hydrazine hydrate as a solvent for the reaction in a three-necked flask or chemical reactor (such as Lab Max reactor). Reflux at °C and react with magnetic stirring for 7 hours to obtain the product by distillation under reduced pressure, recrystallizing with absolute ethanol, and drying to obtain 3-picolinic acid hydrazide. Then, 3-picolinic acid hydrazide and o-vanillin are reacted at a molar ratio of 1:1, 3 times the mass of picolinic acid hydrazide as a solvent, and refluxed at 80° C., reacted with magnetic stirring for 8 hours, and cooled. A large amount of light yellow crystals precipitated, filtered with suction, washed with absolute ethanol, and recrystallized to obtain a light yellow solid. The infrared spectrum shows that it is at 1659cm -1 There is a charact...

Example Embodiment

Example 3:

Synthesis of Schiff base of o-vanillin-4-pyridinecarboxylhydrazone

Use methyl 3-picolinate and hydrazine hydrate in a molar ratio of 1:1, and 4 times the volume of hydrazine hydrate as a solvent for the reaction in a three-necked flask or chemical reactor (such as Lab Max reactor). Reflux at °C and react with magnetic stirring for 7 hours to obtain the product by distillation under reduced pressure, recrystallizing with absolute ethanol, and drying to obtain 3-picolinic acid hydrazide. Then, 3-picolinic acid hydrazide and o-vanillin are reacted at a molar ratio of 1:1, 3 times the mass of picolinic acid hydrazide as a solvent, and refluxed at 80° C., reacted with magnetic stirring for 8 hours, and cooled. A large amount of light yellow crystals precipitated, filtered with suction, washed with absolute ethanol, and recrystallized to obtain a light yellow solid. The infrared spectrum shows that it is at 1659cm -1 There is a characteristic absorption peak of acylhydra...

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Abstract

The invention discloses a preparation method of substituted pyridine carbonylhydrazone metal corrosion inhibitor. The method comprises the following steps: using methylisonicotinate and hydrazine hydrate in a molar ratio of 1:1-1.2:1 and absolute ethanol or methanol used as solvent of which volume is 3-6 times of hydrazine hydrate to react for 6-8h in a three-neck flask under the condition of refluxing at 70-80 DEG C and magnetic stirring, obtaining a product to perform reduced pressure distillation, recrystallizing with absolute ethanol, drying to obtain pyridine formylhydrazine, then using the obtained pyridine formylhydrazine and o-vanillin in a molar ratio of 1:1-1:1.2 and absolute ethanol or methanol used as solvent of which volume is 2-5 times of pyridine formylhydrazine to react for 7-9h under the condition of refluxing at 70-90 DEG C and magnetic stirring, cooling, performing suction filtration, washing with absolute ethanol, and recrystallizing. The preparation method of the invention designs the corrosion inhibitor molecule with good oil solubility which meets the environmental protection requirements; and the corrosion inhibitor molecule is characterized by good biodegradability, low toxicity and corrosion resistance within the pH value range of 4-9, and has good corrosion resistance to A3 carbon steel and copper.

Description

technical field The invention relates to a substituted pyridineformylhydrazone compound for metal material protection, belongs to the field of molecular design of green corrosion inhibitors, and particularly relates to a preparation method of a substituted pyridineformylhydrazone metal corrosion inhibitor. Background technique Compared with the most commonly used inorganic corrosion inhibitors (nitrite, phosphate, polyphosphate, carbonate, silicate, borate, chromate), there are more types of synthetic organic corrosion inhibitors . However, there are still many deficiencies in the molecular structure design, synthesis route and process, and application performance of organic corrosion inhibitors, and its theoretical progress still lags far behind practice. The selection and design of the molecular structure of green corrosion inhibitors must not only consider the corrosion inhibition effect, but also take into account the biological activity and versatility. In order to ad...

Claims

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Application Information

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IPC IPC(8): C23F11/14
Inventor 刘峥王国瑞刘宝玉陈世亮
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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