CN110565098A - Invasive plant compound metal corrosion inhibitor and preparation method and application thereof - Google Patents
Invasive plant compound metal corrosion inhibitor and preparation method and application thereof Download PDFInfo
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- CN110565098A CN110565098A CN201910978687.9A CN201910978687A CN110565098A CN 110565098 A CN110565098 A CN 110565098A CN 201910978687 A CN201910978687 A CN 201910978687A CN 110565098 A CN110565098 A CN 110565098A
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- corrosion inhibitor
- metal corrosion
- invasive plant
- compound metal
- mikania micrantha
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/04—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in markedly acid liquids
-
- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/04—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
- C23G1/06—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors
- C23G1/063—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors heterocyclic compounds
-
- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/08—Iron or steel
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
the invention discloses an invasive plant compound metal corrosion inhibitor and a preparation method and application thereof, wherein the invasive plant compound metal corrosion inhibitor comprises 0.1 ~ 1.0g/L of mikania micrantha extract, 0.05 ~ 0.5g/L of N heterocyclic compound, 0.1 ~ 0.5g/L of anionic surfactant, 0.01 ~ 0.1g/L of sodium bromide and the balance of pickling solution.
Description
Technical Field
the invention belongs to the technical field of materials, and particularly relates to an invasive plant compound metal corrosion inhibitor, and a preparation method and application thereof.
Background
Mikania micrantha ((academic name:Mikania micrantha Kunth), also known as Eupatorium minor, or Eupatorium pseudopatorium minor. Is perennial herb or shrub climbing vine of the Compositae, and is smooth to have more soft hair; stem-like, sometimes tubular, with edges; thin leaf, light green, oval or halberd, tapered, cauline leaf mostly arrow-shaped or halberd-shaped, with deep concave, nearly complete margin to coarse wavy teeth, orTeeth, length 4.0-13.0 cm, width 2.0-9.0 cm. The conifer is terminal or lateral, the compound inflorescence gathers the umbelliform branch; small head-shaped inflorescence, white corolla, bell-shaped throat, long small teeth and bending; the lean fruit is black, and granular protrusions are dispersed on the surface of the lean fruit; when the crown is fresh, the color is white. Native to south and central america, it is now widely spread to tropical regions of asia, such as india, malaysia, thailand, indonesia, nipaler, philippines, babu new guinea, solomon, indian ocean christmas island and some islands on the pacific, including feijia, west samaria, north queensland australia, becoming one of the most harmful weeds in today's tropical and subtropical regions of the world. Mikania micrantha emerged as a weed in hong kong in china approximately in 1919, and was found in shenzhen in 1984, and has been widely distributed in the zhujiang delta region in 2008. This species has been listed as one of the most harmful 100 alien invasive species in the world. Also listed in China are the first foreign invasive species. Most of the pickling corrosion inhibitors aim at single acid species and single metal corrosion inhibition, and have the advantages of strong specificity, large effect difference, unstable chemical properties, field configuration, high working strength, easy misoperation and larger risk of equipment corrosion accidents, and the problems of high price, high toxicity, environmental pollution and the like of most of the corrosion inhibitors, so the development of the pickling corrosion inhibitors capable of solving the problem of invasion of invasive plant mikania micrantha is very necessary.
Disclosure of Invention
The first purpose of the invention is to provide a complex metal corrosion inhibitor for invasive plants; the second purpose is to provide a preparation method of the invasive plant compound metal corrosion inhibitor; the third purpose is to provide the application of the invasive plant compound metal corrosion inhibitor.
the first purpose of the invention is realized in such a way that the invasive plant compound metal corrosion inhibitor comprises 0.1 ~ 1.0g/L of mikania micrantha extract, 0.05 ~ 0.5g/L of N heterocyclic compound, 0.1 ~ 0.5g/L of anionic surfactant, 0.01 ~ 0.1g/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 object invading plant compound metal corrosion inhibitor.
The third purpose of the invention is realized by the application of the invasive plant compound metal corrosion inhibitor in the 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 invasive plant mikania micrantha as a raw material to prepare the mikania micrantha extract, adding the synergistic N heterocyclic compound, the surfactant and the stabilizer sodium bromide and the balance of the pickling solution has a synergistic effect. 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 invasive plant compound metal corrosion inhibitor comprises 0.1 ~ 1.0g/L of mikania micrantha extract, 0.05 ~ 0.5g/L of N heterocyclic compound, 0.1 ~ 0.5g/L of anionic surfactant, 0.01 ~ 0.1g/L of sodium bromide and the balance of pickling solution.
The N heterocyclic compound is 2-hydroxypyridine.
The anionic surfactant is sodium lignosulfonate.
The mikania micrantha extract is prepared from an invasive plant mikania micrantha as a raw material through the steps of pretreatment, extraction, concentration, extraction and post-treatment, and specifically comprises the following steps:
A. pretreatment: drying, crushing and sieving mikania micrantha to obtain mikania micrantha powder a;
B. extracting, namely adding an ethanol solution of which the volume is 20 ~ 40 times that of mikania micrantha powder into the mikania micrantha powder a, soaking for 2 ~ 4 hours at 10 ~ 35 ℃ to obtain a material b, refluxing and extracting the material b in a water bath at 50 ~ 80 ℃ for 2 ~ 6 hours, 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. 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 mikania micrantha extract.
and the drying in the step A comprises air drying and constant temperature drying, and specifically comprises the steps of air drying the waste mikania micrantha, then placing the waste mikania micrantha in a blast oven, and drying the waste mikania micrantha at a constant temperature of 50 ~ 70 ℃ for 48 ~ 60 hours.
and the volume concentration of the ethanol solution in the step B is 20 ~ 60%.
And E, evaporating by adopting rotary evaporation.
and E, drying at 50 ~ 70 ℃ for 12 ~ 24 h.
The preparation method of the mikania micrantha extract provided by the invention specifically comprises the following operations:
A. pre ~ treatment, namely collecting mikania micrantha, drying the mikania micrantha in air, putting the mikania micrantha in an air ~ blowing oven, drying the mikania micrantha at a constant temperature of 60 ℃ for 48 ~ 60 hours, taking out the mikania micrantha, naturally cooling the mikania micrantha to room temperature, and crushing the mikania micrantha to obtain mikania mic;
B. the extraction method comprises the steps of adding 20 ~ 60% ethanol solution into mikania micrantha powder, soaking for 2 ~ 4 hours at room temperature (10 ~ 35 ℃), enabling the solid ~ liquid ratio to be 1:20 ~ 40, and then carrying out reflux extraction for 2 ~ 6 hours in water bath at 50 ~ 80 ℃;
C. concentrating, namely performing vacuum filtration on the ethanol extract obtained by refluxing to remove mikania micrantha residue powder contained in the ethanol extract, and performing rotary evaporation and concentration on the solution on a rotary evaporator at 40 ~ 80 ℃ to 1/2 ~ 1/3 of the volume of the solution;
D. extracting, namely adding petroleum ether with the volume 2 ~ 5 times of that of the concentrated ethanol extract, fully shaking, standing for 12 ~ 48h, separating the petroleum ether at the upper layer from the extract at the lower layer, recovering the upper layer liquid, adding the lower layer liquid into a separating funnel again, adding the petroleum ether with the volume 2 ~ 3 times of that of the lower layer liquid, 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 post ~ treatment, namely 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 crystallization shovel to obtain the target mikania micrantha extract.
the preparation method of the invasive plant compound metal 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 invasive plant compound metal corrosion inhibitor.
the application of the invasive plant compound metal corrosion inhibitor is the application of the invasive plant compound metal corrosion inhibitor in steel material pickling.
The invention is further illustrated by the following specific examples:
example 1
Preparation of Mikania micrantha extract
A. pre-treatment, namely collecting mikania micrantha, drying the mikania micrantha in air, putting the mikania micrantha in an air-blowing oven, drying the mikania micrantha for 60 ~ 72 hours at a constant temperature of between 60 and 70 ℃, taking out the mikania micrantha, naturally cooling the mikania micrantha ~ room temperature, and crushing the mikania micrantha with the particle size of 150 ~;
B. the extraction method comprises the steps of adding 10 ~ 70% ethanol solution into mikania micrantha powder, soaking for 2 ~ 6 hours at room temperature (5 ~ 35 ℃), enabling the solid ~ liquid ratio to be 1:25 ~ 50, and then carrying out reflux extraction for 3 ~ 9 hours in water bath at the temperature of 60 ~ 85 ℃;
C. concentrating, namely performing vacuum filtration on the ethanol extract obtained by refluxing to remove mikania micrantha residue powder contained in the ethanol extract, and performing rotary evaporation and concentration on the solution on a rotary evaporator at 45 ~ 75 ℃ to obtain a solution with a volume of 1/4 ~ 1/2;
D. extracting, namely adding petroleum ether with the volume 2 ~ 6 times of that of the concentrated ethanol extract, fully shaking, standing for 15 ~ 60h, separating the petroleum ether at the upper layer from the extract at the lower layer, recovering the upper layer liquid, adding the lower layer liquid into a separating funnel again, adding the petroleum ether with the volume 2 ~ 5 times of that of the lower layer liquid, 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 post ~ treatment, namely 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 crystallization shovel to obtain the target mikania micrantha extract.
example 2
Preparation of invasive plant compound metal corrosion inhibitor
taking 0.10 g of the mikania micrantha extract, 0.5g of 2 ~ hydroxypyridine, 0.5g of sodium lignosulfonate and 0.01g of sodium bromide in the embodiment 1, adding 1L of hydrochloric acid solution with the concentration of 0.5 ~ 5.0 mol/L, and uniformly stirring to obtain the target invasive plant compound corrosion inhibitor.
Example 3
Preparation of invasive plant compound metal corrosion inhibitor
taking 1.0g of the mikania micrantha extract, 0.5g of 2 ~ hydroxypyridine, 0.5g of sodium lignosulfonate and 0.05g of sodium bromide in example 1, adding 1L of sulfuric acid lotion with the concentration of 0.5 ~ 5.0 mol/L, and uniformly stirring to obtain the target invasive plant compound corrosion inhibitor.
Example 4
Preparation of invasive plant compound metal corrosion inhibitor
taking 1.0g of the mikania micrantha extract, 0.5g of 2 ~ hydroxypyridine, 0.5g of sodium lignosulfonate and 0.1g of sodium bromide in the example 1, adding 1L of phosphoric acid lotion with the concentration of 0.5 ~ 10.0 mol/L, and uniformly stirring to obtain the target agricultural and forestry waste compound corrosion inhibitor.
Test example 1
Pickling of ferrous Material
the steel material is selected as a cold ~ rolled steel sheet, the corrosion inhibitor compounded in the embodiment 2 is injected and uniformly mixed, the corrosion inhibition performance can be more than 95% at different temperatures (20 ~ 50 ℃) and different corrosion soaking times (6 ~ 156 hours), the table 1 shows 1.0 mol/L HCl test data, and the method is a weight loss method.
TABLE 1 Corrosion inhibition ratio of invasive 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 a cold ~ rolled steel sheet, the corrosion inhibitor compounded in the embodiment 3 is injected and uniformly mixed, the corrosion inhibition performance can be more than 92% at different temperatures (20 ~ 50 ℃) and different corrosion soaking times (6 ~ 48 hours), the table 2 shows 3.0 mol/L HCl test data, and the method is a weight loss method.
TABLE 2 Corrosion inhibition ratio of invasive 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 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 95% at different temperatures (20 ~ 50 ℃) and different corrosion soaking times (6 ~ 96 hours), and the corrosion inhibition performance is 1.0 mol/L H in the table 32SO4Test data, the method is a weight loss method.
TABLE 3 combination of corrosion inhibitors for invasive plants at 1.0 mol/L H for cold rolled steel2SO4middle 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 mixed uniformly, the corrosion inhibition performance can be more than 95% at different temperatures (20 ~ 50 ℃) 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 invasion of the Compound plant Corrosion inhibitor to Cold rolled Steel at 1.0 mol/L H3PO4Middle 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 mixed uniformly, the corrosion inhibition performance can be more than 90% at different temperatures (20 ~ 50 ℃) and different corrosion soaking times (6 ~ 120 h), and the corrosion inhibition performance is 9.0 mol/L H in the 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 invasive plant compound metal corrosion inhibitor is characterized by comprising 0.1 ~ 1.0g/L of mikania micrantha extract, 0.05 ~ 0.5g/L of N heterocyclic compound, 0.1 ~ 0.5g/L of anionic surfactant, 0.01 ~ 0.1g/L of sodium bromide and the balance of pickling solution.
2. The invasive plant compound metal corrosion inhibitor according to claim 1, characterized in that the N heterocyclic compound is 2-hydroxypyridine.
3. The invasive plant compound metal corrosion inhibitor according to claim 1, characterized in that the anionic surfactant is sodium lignosulfonate.
4. The invasive plant compound metal corrosion inhibitor according to claim 1, wherein the mikania micrantha extract is prepared from an invasive plant mikania micrantha as a raw material through the steps of pretreatment, extraction, concentration, extraction and post-treatment, and specifically comprises the following steps:
A. Pretreatment: drying, crushing and sieving mikania micrantha to obtain mikania micrantha powder a;
B. extracting, namely adding an ethanol solution of which the volume is 20 ~ 40 times that of mikania micrantha powder into the mikania micrantha powder a, soaking for 2 ~ 4 hours at 10 ~ 35 ℃ to obtain a material b, refluxing and extracting the material b in a water bath at 50 ~ 80 ℃ for 2 ~ 6 hours, 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. 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 mikania micrantha extract.
5. the invasive plant compound metal corrosion inhibitor according to claim 4, wherein the drying in the step A comprises air drying and constant temperature drying, and specifically, waste mikania micrantha is air ~ dried and then placed in a forced air oven to be dried for 48 ~ 60 hours at a constant temperature of 50 ~ 70 ℃.
6. the invasive plant compound metal corrosion inhibitor according to claim 4, wherein the volume concentration of the ethanol solution in the step B is 20 ~ 60%.
7. The invasive plant compound metal corrosion inhibitor according to claim 4, wherein the evaporation in the step E is rotary evaporation.
8. the invasive plant compound metal corrosion inhibitor according to claim 4, wherein the drying in the step E is carried out at a temperature of 50 ~ 70 ℃ for 12 ~ 24 h.
9. a preparation method of the invasive plant compound metal corrosion inhibitor as claimed in any one of claims 1 to 8, characterized in that the target invasive plant compound metal corrosion inhibitor is obtained by mixing and stirring the raw materials in the formula ratio uniformly.
10. the application of the invasive plant compound metal corrosion inhibitor of claims 1-8, which is characterized in that the invasive plant compound metal corrosion inhibitor is applied to pickling of steel materials.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113549919A (en) * | 2021-07-27 | 2021-10-26 | 西南林业大学 | Marigold extract compound corrosion inhibitor and preparation method and application thereof |
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Non-Patent Citations (1)
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| SLIVIA MARSELYA: "pemanfaatan daun sembung rambat(mikania micrantha) sebagai inhibitor borosi baja ramah lingkungan dalam medium asam klorida", 《DIPLOMA THESIS,UNIVERSITAS ANDALAS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113549919A (en) * | 2021-07-27 | 2021-10-26 | 西南林业大学 | Marigold extract compound corrosion inhibitor and preparation method and application thereof |
| CN113549919B (en) * | 2021-07-27 | 2023-08-29 | 西南林业大学 | Tagetes extract compound corrosion inhibitor and preparation method and application thereof |
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