CN110607529A - Malignant weed compound corrosion inhibitor and preparation method and application thereof - Google Patents

Malignant weed compound corrosion inhibitor and preparation method and application thereof Download PDF

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Publication number
CN110607529A
CN110607529A CN201910979692.1A CN201910979692A CN110607529A CN 110607529 A CN110607529 A CN 110607529A CN 201910979692 A CN201910979692 A CN 201910979692A CN 110607529 A CN110607529 A CN 110607529A
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China
Prior art keywords
corrosion inhibitor
compound
malignant weed
alternanthera
solution
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CN201910979692.1A
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Chinese (zh)
Inventor
李向红
邓书端
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Southwest Forestry University
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Southwest Forestry University
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Priority to CN201910979692.1A priority Critical patent/CN110607529A/en
Publication of CN110607529A publication Critical patent/CN110607529A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/04Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
    • C23G1/06Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08Iron or steel
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08Iron or steel
    • C23G1/081Iron or steel solutions containing H2SO4
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08Iron or steel
    • C23G1/083Iron or steel solutions containing H3PO4

Abstract

The invention discloses a malignant weed compound corrosion inhibitor and a preparation method and application thereof, wherein the malignant weed compound corrosion inhibitor comprises 0.1 ~ 1.0.0 g/L of alligator alternanthera extract, 0.05 ~ 0.1.1 g/L of N-heterocyclic compound, 0.1 ~ 1.0.0 g/L of cationic surfactant, 0.01 ~ 0.1.1 g/L of sodium bromide and the balance of pickling solution.

Description

Malignant weed compound corrosion inhibitor and preparation method and application thereof
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a malignant weed compound corrosion inhibitor, and a preparation method and application thereof.
Background
Alternanthera philoxeroides, perennial root herbaceous. The base of the stem is creeping, the upper part is extended, the stem is hollow and has branches, and fine and soft hair is dredged at the axillary position of the node. The leaves are opposite, the long round shape is inverted egg shape or inverted egg shape is in a needle shape, the tip is round and blunt, the awn tip is arranged, the base is gradually narrowed, the surface is stuck with hair, and the edge is provided with eyelashes. The head-shaped inflorescence grows in the leaf axils singly, and the total pedicel is 1-6 cm long; the bracts and the bracts are dried and stored; the quilt 5 is white and not as large; 5, the base of the stamen is combined into a cup shape, and the top of the degenerated stamen is split into 3-4 narrow strips; the ovary is inverted egg-shaped, and the stigma is head-shaped. The flowering period is 5-11 months. Most of pickling corrosion inhibitors aim at single acid species and single metal corrosion inhibition, and are strong in specificity, large in effect difference, unstable in chemical properties, large in working strength, easy to cause misoperation and large in risk of equipment corrosion accidents, and most of the corrosion inhibitors are expensive, high in toxicity, environment-friendly and the like, so that the problem of resource waste of the alligator alternanthera and the corrosion inhibitor are very necessary to develop.
Disclosure of Invention
The first purpose of the invention is to provide a malignant weed compound corrosion inhibitor; the second purpose is to provide a preparation method of the malignant weed compound corrosion inhibitor; the third purpose is to provide the application of the malignant weed compound corrosion inhibitor.
The first purpose of the invention is realized in such a way that the malignant weed compound corrosion inhibitor comprises 0.1 ~ 1.0.0 g/L of alternanthera philoxeroides extract, 0.05 ~ 0.1.1 g/L of N-heterocyclic compound, 0.1 ~ 1.0.0 g/L of cationic surfactant, 0.01 ~ 0.1.1 g/L of sodium bromide and the balance of pickling solution.
The second purpose of the invention is realized by mixing and stirring the raw materials in the formula ratio uniformly to obtain the target malignant weed compound corrosion inhibitor.
The third purpose of the invention is realized by the application of the malignant weed compound corrosion inhibitor in the acid pickling of steel materials.
The invention overcomes the defects of high price, high toxicity and environmental pollution of most corrosion inhibitors, and the metal corrosion inhibitor prepared by taking alligator alternanthera with wide sources, rich resources and high yield as a raw material has a synergistic effect by adding a synergistic assistant N-heterocyclic compound, a surfactant, a stabilizer sodium bromide and the balance of a pickling solution. The metal corrosion inhibitor provided by the invention has the advantages of no toxicity, low cost, strong adaptability, obvious inhibition of corrosion of acid on metal materials, no pollution after use, and safe and convenient use.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to be limiting in any way, and any modifications or alterations based on the teachings of the present invention are intended to fall within the scope of the present invention.
The malignant weed compound corrosion inhibitor comprises 0.1 ~ 1.0.0 g/L of alligator alternanthera extract, 0.05 ~ 0.1.1 g/L of N-heterocyclic compound, 0.1 ~ 1.0.0 g/L of cationic surfactant, 0.01 ~ 0.1.1 g/L of sodium bromide and the balance of pickling solution.
The N-heterocyclic compound is 3, 6-dichloropyridazine.
The cationic surfactant is octadecyl dimethyl benzyl ammonium chloride.
The alligator alternanthera extract is prepared by taking alligator alternanthera as a raw material and performing pretreatment, extraction, concentration, extraction and post-treatment steps, and specifically comprises the following steps:
A. pretreatment: drying, crushing and sieving the waste alligator alternanthera to obtain alligator alternanthera powder a;
B. extracting, namely adding an ethanol solution which is 20 ~ 40 times of the volume of the alligator alternanthera powder into the alligator alternanthera powder a, soaking for 2 ~ 4h at 10 ~ 30 ℃ to obtain a material b, refluxing and extracting the material b in a water bath at 50 ~ 80 ℃ for 2 ~ 6h, and performing suction filtration to obtain an extracting solution c;
C. concentrating the extracting solution c to 1/2 ~ 1/3 of the volume of the extracting solution c to obtain a concentrated solution d;
D. extracting, namely adding petroleum ether with the volume 2 ~ 5 times that of the concentrated solution d into the concentrated solution d, fully oscillating, standing for 12 ~ 48h to obtain a petroleum ether layer e and a lower-layer extracting solution f, recovering the petroleum ether layer e, adding petroleum ether with the volume 2 ~ 3 times that of the lower-layer extracting solution f into the lower-layer extracting solution f again, fully oscillating, standing for layering, and replacing the petroleum ether every 10 ~ 30min until the petroleum ether layer is colorless to obtain an extracting solution g;
E. and (3) post-treatment: evaporating and drying the extracting solution g to obtain the target alligator alternanthera extract.
The drying in the step A comprises air drying and constant temperature drying, and specifically comprises the steps of air drying the alternanthera philoxeroides, then placing the alternanthera philoxeroides in a blast oven, and drying at the constant temperature of 50 ~ 70 ℃ for 48 ~ 60 h.
The volume concentration of the ethanol solution in the step B is 20 ~ 60%.
And E, evaporating by adopting rotary evaporation.
The drying described in step E was carried out at a temperature of 50 ~ 70 ℃ for 12 ~ 24 h.
The preparation method of the alligator alternanthera extract specifically comprises the following operations:
A. pre-treating, namely collecting alligator alternanthera, drying in air, putting in a blast oven, drying at the constant temperature of ~ 70 ℃ for 48 ~ 60h, taking out, naturally cooling to room temperature, and crushing to obtain alligator alternanthera powder with the particle size of 300 ~ 1000 mu m;
B. extracting by adding 20 ~ 60% ethanol solution at room temperature (10 ~ 30 deg.C) into Alternanthera philoxeroides powder, soaking for 2 ~ 4h with a solid-to-liquid ratio of 1:20 ~ 40, and reflux-extracting in 50 ~ 80 deg.C water bath for 2 ~ 6 h;
C. concentrating, vacuum filtering the ethanol extractive solution to remove Alternanthera philoxeroides residue powder, and rotary evaporating the solution at 40 ~ 80 deg.C on rotary evaporator to 1/2 ~ 1/3 volume;
D. extracting, namely adding petroleum ether with the volume 2 ~ 5 times into the concentrated ethanol extracting solution, fully shaking, standing for 12 ~ 48h, separating the petroleum ether at the upper layer from the extracting solution at the lower layer, recovering the upper layer liquid, adding the lower layer liquid into a separating funnel again, adding petroleum ether with the volume 2 ~ 3 times, fully shaking, standing and layering, and replacing the petroleum ether every 10 ~ 30 minutes until the upper layer liquid is colorless;
E. and (3) performing rotary evaporation on the extracted subnatant to 40 ~ 60ml, putting the evaporated liquid into an evaporation dish, drying the liquid in a forced air drying oven at 50 ~ 70 ℃ for 12 ~ 24h, and shoveling the solid by using a crystal shovel to obtain the target alternanthera philoxeroides extract.
The preparation method of the malignant weed compound corrosion inhibitor provided by the invention is characterized in that all raw materials in the formula ratio are mixed and stirred uniformly to obtain the target object malignant weed compound corrosion inhibitor.
The application of the malignant weed compound corrosion inhibitor is the application of the malignant weed compound corrosion inhibitor in steel material pickling.
The invention is further illustrated by the following specific examples:
example 1
Preparation of Alternanthera philoxeroides extract
A. Pre-treating, namely collecting alligator alternanthera, drying in the air, putting in a blast oven, drying at the constant temperature of 60 ℃ ~ 70 ℃ for 60 ~ 72 h, taking out, naturally cooling to room temperature, and crushing to obtain alligator alternanthera powder with the particle size of 150 ~ 2000 mu m;
B. extracting by adding 10 ~ 70% ethanol solution into Alternanthera philoxeroides powder at room temperature (5 ~ 35 deg.C) for 2 ~ 6h with a solid-to-liquid ratio of 1:25 ~ 50, and reflux-extracting in 60 ~ 85 deg.C water bath for 3 ~ 9 h;
C. concentrating, vacuum filtering the ethanol extractive solution to remove Alternanthera philoxeroides residue powder, and rotary evaporating the solution at 45 ~ 75 deg.C on rotary evaporator to 1/4 ~ 1/2 volume;
D. extracting, namely adding petroleum ether with the volume 2 ~ 6 times into the concentrated ethanol extracting solution, fully shaking, standing for 15 ~ 60h, separating the petroleum ether at the upper layer from the extracting solution at the lower layer, recovering the upper layer liquid, adding the lower layer liquid into a separating funnel again, adding petroleum ether with the volume 2 ~ 5 times, fully shaking, standing and layering, and replacing the petroleum ether every 20 ~ 40 minutes until the upper layer liquid is colorless;
E. and (3) performing rotary evaporation on the extracted subnatant to 40 ~ 60mL, putting the evaporated liquid into an evaporation dish, drying the liquid in a forced air drying oven at 50 ~ 70 ℃ for 12 ~ 24h, and shoveling the solid by using a crystal shovel to obtain the target alternanthera philoxeroides extract.
Example 2
-malignant weed compound metal corrosion inhibitor
0.1g of alligator alternanthera extract, 0.05 g of 3, 6-dichloropyridazine, 0.5g of sodium abietate, 0.5g of octadecyl dimethyl benzyl ammonium chloride and 0.01g of sodium bromide in the embodiment 1 are taken, hydrochloric acid washing liquid with the volume of 1L and the concentration of 0.5 ~ 5.0.0 mol/L is added, and the mixture is uniformly stirred to obtain the target compound malignant weed metal corrosion inhibitor.
Example 3
-malignant weed compound metal corrosion inhibitor
Taking 0.5g of alligator alternanthera extract, 0.1g of 3, 6-dichloropyridazine, 0.5g of octadecyl dimethyl benzyl ammonium chloride and 0.10g of sodium bromide in the embodiment 1, adding 1L of sulfuric acid lotion with the concentration of 0.5 ~ 5.0.0 mol/L, and uniformly stirring to obtain the target plant compound corrosion inhibitor.
Example 4
-malignant weed compound metal corrosion inhibitor
1.0g of alligator alternanthera extract, 0.1g of 3, 6-dichloropyridazine, 1.0g of octadecyl dimethyl benzyl ammonium chloride and 0.1g of sodium bromide in the embodiment 1 are taken, 1L of phosphoric acid lotion with the concentration of 0.5 ~ 7.0.0 mol/L is added, and the mixture is uniformly stirred to obtain the target agricultural and forestry waste compound corrosion inhibitor.
Test example 1
Pickling of ferrous Material
The steel material is selected as cold-rolled steel sheet, the corrosion inhibitor compounded in the embodiment 2 is injected and mixed uniformly, the corrosion inhibition performance can be more than 95% at different temperatures (20 ~ 50 ℃ C.) and different corrosion soaking times (6 ~ 156 h), the table 1 shows 1.0 mol/L HCl test data, and the method is a weight loss method.
TABLE 1 Corrosion inhibition rate of plant compound corrosion inhibitor to cold rolled steel in 1.0 mol/L HCl
Test example 2
Pickling of ferrous Material
The steel material is selected as cold-rolled steel sheet, the corrosion inhibitor compounded in the embodiment 3 is injected and mixed uniformly, the corrosion inhibition performance can be more than 94% at different temperatures (20 ~ 50 ℃ C.) and different corrosion soaking times (6 ~ 48 h), the table 2 shows 3.0 mol/L HCl test data, and the method is a weight loss method.
TABLE 2 Corrosion inhibition rate of plant compound corrosion inhibitor to cold rolled steel in 3.0 mol/L HCl
Test example 3
Pickling of ferrous Material
The steel material is selected from cold rolled steel sheetExample 3 the well-formulated corrosion inhibitor is injected and mixed evenly, the corrosion inhibition performance can be more than 96% at different temperatures (20 ~ 50 ℃) and different corrosion soaking times (6 ~ 96 h), table 3 is 1.0 mol/L H2SO4Test data, the method is a weight loss method.
TABLE 3 plant Compound Corrosion inhibitor to Cold rolled Steel at 1.0 mol/L H2SO4Middle inhibition rate
Test example 4
Pickling of ferrous Material
The steel material is selected as cold-rolled steel sheet, the corrosion inhibitor compounded in the embodiment 4 is injected and evenly mixed, the corrosion inhibition performance can be more than 96 percent at different temperatures (20 ~ 50 ℃ C.) and different corrosion soaking times (6 ~ 120 h), and the corrosion inhibition performance is 1.0 mol/L H in the table 43PO4Test data, the method is a weight loss method.
TABLE 4 Compound plant corrosion inhibitor at 1.0 mol/L H for cold rolled steel3PO4Middle inhibition rate
Test example 5
Pickling of ferrous Material
The steel material is selected as cold-rolled steel sheet, the corrosion inhibitor compounded in the embodiment 4 is injected and evenly mixed, the corrosion inhibition performance can be more than 92 percent at different temperatures (20 ~ 50 ℃ C.) and different corrosion soaking times (6 ~ 120 h), and the corrosion inhibition performance is 7.0 mol/L H in a table 43PO4Test data, the method is a weight loss method.
TABLE 4 Compound plant corrosion inhibitor at 9.0 mol/L H for cold rolled steel3PO4Middle inhibition rate

Claims (10)

1. The malignant weed compound corrosion inhibitor is characterized by comprising 0.1 ~ 1.0.0 g/L of alligator alternanthera extract, 0.05 ~ 0.1.1 g/L of N-heterocyclic compound, 0.1 ~ 1.0.0 g/L of cationic surfactant, 0.01 ~ 0.1.1 g/L of sodium bromide and the balance of pickling solution.
2. The compound inhibitor for malignant weeds of claim 1, wherein the N-heterocyclic compound is 3, 6-dichloropyridazine.
3. A malignant weed formulated corrosion inhibitor according to claim 1, characterized in that the cationic surfactant is octadecyl dimethyl benzyl ammonium chloride.
4. The compound inhibitor for malignant weeds of claim 1, wherein the alternanthera philoxeroides extract is prepared from alternanthera philoxeroides serving as a raw material by the steps of pretreatment, extraction, concentration, extraction and post-treatment, and specifically comprises the following steps:
A. pretreatment: drying, crushing and sieving the waste alligator alternanthera to obtain alligator alternanthera powder a;
B. extracting, namely adding an ethanol solution which is 20 ~ 40 times of the volume of the alligator alternanthera powder into the alligator alternanthera powder a, soaking for 2 ~ 4h at 10 ~ 30 ℃ to obtain a material b, refluxing and extracting the material b in a water bath at 50 ~ 80 ℃ for 2 ~ 6h, and performing suction filtration to obtain an extracting solution c;
C. concentrating the extracting solution c to 1/2 ~ 1/3 of the volume of the extracting solution c to obtain a concentrated solution d;
D. extracting, namely adding petroleum ether with the volume 2 ~ 5 times that of the concentrated solution d into the concentrated solution d, fully oscillating, standing for 12 ~ 48h to obtain a petroleum ether layer e and a lower-layer extracting solution f, recovering the petroleum ether layer e, adding petroleum ether with the volume 2 ~ 3 times that of the lower-layer extracting solution f into the lower-layer extracting solution f again, fully oscillating, standing for layering, and replacing the petroleum ether every 10 ~ 30min until the petroleum ether layer is colorless to obtain an extracting solution g;
E. and (3) post-treatment: evaporating and drying the extracting solution g to obtain the target alligator alternanthera extract.
5. The compound malignant weed corrosion inhibitor according to claim 4, wherein the drying in step A comprises air drying and constant temperature drying, specifically, the alternanthera philoxeroides is dried in an air-blowing oven at 50 ~ 70 ℃ for 48 ~ 60h at constant temperature.
6. The malignant weed compound corrosion inhibitor according to claim 4, wherein the volume concentration of the ethanol solution in the step B is 20 ~ 60%.
7. The malignant weed formulated corrosion inhibitor according to claim 4, wherein the evaporation in step E is rotary evaporation.
8. The malignant weed formulated corrosion inhibitor according to claim 4, wherein the drying in step E is carried out at a temperature of 50 ~ 70 ℃ for 12 ~ 24 h.
9. A preparation method of the malignant weed compound corrosion inhibitor of claim 1 ~ 8, characterized in that the target object of the malignant weed compound corrosion inhibitor is obtained by mixing and stirring the raw materials in the formula ratio uniformly.
10. The application of the malignant weed compound corrosion inhibitor of claim 1 ~ 8, wherein the malignant weed compound corrosion inhibitor is applied to pickling of steel materials.
CN201910979692.1A 2019-10-15 2019-10-15 Malignant weed compound corrosion inhibitor and preparation method and application thereof Pending CN110607529A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN113549920A (en) * 2021-07-27 2021-10-26 西南林业大学 Broadleaf holly extract compound corrosion inhibitor and preparation method and application thereof

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Application publication date: 20191224