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Preparation method of tree-shaped Schiff base corrosion inhibitor

The technology of Schiff base and corrosion inhibitor is applied in the field of preparation of dendritic Schiff base corrosion inhibitor, which can solve the problems of few adsorption sites, low corrosion inhibition performance and high reaction temperature of Schiff base corrosion inhibitor, To achieve the effects of easy control of reaction conditions, good dispersibility and less side reactions

Active Publication Date: 2016-01-20
成都恒固新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the prior art, although the method of reacting aldehyde and amine to generate a Schiff base corrosion inhibitor is simple, the reaction is carried out at 90°C, the reaction temperature is relatively high, and side reactions will increase at the same time, which is not conducive to purification. , in the recrystallization purification process, single solvent is used for recrystallization, the yield of this operation is low, the adsorption sites of the prepared Schiff base corrosion inhibitor are few, and its corrosion inhibition performance is not high

Method used

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  • Preparation method of tree-shaped Schiff base corrosion inhibitor
  • Preparation method of tree-shaped Schiff base corrosion inhibitor
  • Preparation method of tree-shaped Schiff base corrosion inhibitor

Examples

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Comparison scheme
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Embodiment 1

[0033] A kind of preparation method of novel dendritic Schiff base corrosion inhibitor comprises the following steps:

[0034] (1) Synthesis of Schiff base monomer BEA: Add 0.86g (14.3mmol) ethylenediamine and 30mL chloroform to a three-necked flask equipped with a stirrer, reflux condenser and thermometer, then add 0.8g (5.8mmol) ) water absorbent K 2 CO 3 , stir and mix well, and slowly add 0.53g (3.0mmol) of 4-trifluoromethylbenzaldehyde at 40°C using a constant pressure feeder. After the dropwise addition, raise the temperature to 65°C and reflux for 6h to obtain a dark brown transparent liquid, rotary evaporation, and drying to obtain a crude product. Put the crude product into a round-bottomed flask, then add a certain amount of dichloromethane, and slowly add methanol when heating and boiling in a water bath at 60°C until the product is completely dissolved. It can be put into the refrigerator for 2 days; wherein the volume ratio of dichloromethane and methanol is 1:1...

Embodiment 2

[0036] The preparation of embodiment 2 control group 1

[0037] The preparation method of matched group Schiff base corrosion inhibitor comprises the following steps:

[0038] (1) Add aniline to a three-necked flask equipped with a stirrer, a reflux condenser and a thermometer, use absolute ethanol as a solvent, stir and slowly add cinnamaldehyde using a constant pressure feeder, react at 90°C for 6 hours, and obtain a deep red transparent Liquid; wherein the molar ratio of aniline and cinnamaldehyde is 1:1.2; the relationship between the added solvent ethanol and the content of reactant aniline is 60mL / g;

[0039](2) Purification of the crude product: recrystallize with a single solvent methanol to obtain a pure Schiff base corrosion inhibitor, that is, slowly add methanol to the product under the condition of a water bath at 60 °C until the product is completely dissolved, and then continue to add the previously added amount of 15 % methanol, put it in the refrigerator for ...

Embodiment 3

[0040] The preparation of embodiment 3 control group 2

[0041] Under stirring at room temperature, slowly add a certain amount of salicylaldehyde dropwise into anhydrous ethanol containing a certain amount of o-phenylenediamine, stir for 10 minutes, reflux at 148-150°C for 4 hours, evaporate most of the ethanol, filter with suction, and dry. And recrystallize 3 times with 95% ethanol, obtain yellow crystal, productive rate 64.3%; Wherein n (salicylaldehyde): n (o-phenylenediamine)=2:1; The relationship of the added amount of aldehyde satisfies 30mL / g.

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Abstract

The invention discloses a preparation method of a tree-shaped Schiff base corrosion inhibitor. The method comprises the following steps: 1, uniformly mixing ethylene diamine, trichloromethane and K2CO3, adding 4-trifluoromethylbenzaldehyde at 40DEG C, heating to 65DEG C, reacting for 6h to obtain a dark-brown transparent liquid, concentrating, drying, and re-crystallizing to obtain a Schiff base monomer; and 2, uniformly mixing the Schiff base monomer, dichloromethane and K2CO3, adding trimesoyl chloride at 35DEG C, heating to 50DEG C, reacting for 8h to obtain a milky yellow liquid, concentrating, and drying to obtain the tree-shaped Schiff base corrosion inhibitor. A reaction solvent with a low boiling point is selected to participate in reactions in the preparation process, so the reaction temperature is reduced to 65DEG C, the cost is reduced, and side reactions are few; and a mixed solvent is adopted to re-crystallize and purify a crude product, so the yield is improved, the novel tree-shaped Schiff base corrosion inhibitor prepared in the invention has many adsorption sites, and the corrosion performance of the tree-shaped Schiff base corrosion inhibitor is improved.

Description

technical field [0001] The invention belongs to the technical field of corrosion inhibitor production, and in particular relates to a preparation method of a tree-shaped Schiff base corrosion inhibitor. Background technique [0002] Schiff base (Schiffbase) refers to a class of organic compounds containing imine groups (-HC=N-) or methylimine groups (-RC=N-). The N atom in the core part of the Schiff base has a lone pair of electrons and has a strong coordination ability. Various functional groups can be introduced on both sides of the C=N double bond in the Schiff base to derivatize it. Its synthesis is relatively easy, and various aldehydes or ketones with carbonyl groups can be flexibly selected for reaction. By changing the connected substituents and changing the atomic nature and position of the electron donor, many Schiff base ligands with different properties and variable structures can be developed from chain to ring, from monodentate to multidentate, and Then a va...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/02C23F11/04
Inventor 何毅周艳秋杨冉冉施太和詹迎青
Owner 成都恒固新材料科技有限公司
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