CN110952105A - Jatropha curcas cake meal compound corrosion inhibitor and preparation method and application thereof - Google Patents
Jatropha curcas cake meal compound corrosion inhibitor and preparation method and application thereof Download PDFInfo
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- CN110952105A CN110952105A CN201911266861.3A CN201911266861A CN110952105A CN 110952105 A CN110952105 A CN 110952105A CN 201911266861 A CN201911266861 A CN 201911266861A CN 110952105 A CN110952105 A CN 110952105A
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- jatropha curcas
- corrosion inhibitor
- curcas cake
- compound corrosion
- cake
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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
- 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
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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
- 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
Abstract
The invention discloses a Jatropha curcas cake meal compound corrosion inhibitor and a preparation method and application thereof. The compound corrosion inhibitor for the jatropha curcas cake meal comprises 0.1-1.0 g/L of jatropha curcas cake meal extract, 0.05-0.5 g/L of oxime compound, 0.1-0.5 g/L of nonionic surfactant, 0.01-0.1 g/L of dimethylol urea and the balance of pickling solution. The preparation method is that the raw materials in the formula proportion are mixed and stirred evenly to obtain the target jatropha curcas cake meal compound corrosion inhibitor. The application is the application of the Jatropha curcas cake meal compound corrosion inhibitor in the acid cleaning of steel materials.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a Jatropha curcas cake meal compound corrosion inhibitor, and a preparation method and application thereof.
Background
Jatropha curcas (Jatropha curcas L.), also called Jatropha curcas, is a deciduous shrub or small tree species of the Jatropha genus of the euphorbiaceae family, growing mainly in subtropical regions. At present, a large number of trees are planted as energy sources of biodiesel. During the production of biodiesel, a large amount of by-product, namely cake meal, is generated from jatropha curcas. These cakes contain a large amount of protein and are good protein feed resources. The presence of toxic substances limits the further use of the meal. Therefore, it is very necessary to develop a compound corrosion inhibitor which can be prepared by using the jatropha curcas cake meal.
Disclosure of Invention
The first purpose of the invention is to provide a Jatropha curcas cake compound corrosion inhibitor; the second purpose is to provide a preparation method of the Jatropha curcas cake meal compound corrosion inhibitor; the third purpose is to provide the application of the Jatropha curcas cake meal compound corrosion inhibitor.
The first purpose of the invention is realized in such a way that the compound corrosion inhibitor for the Jatropha curcas cake pulp comprises 0.1-1.0 g/L of Jatropha curcas cake pulp extract, 0.05-0.5 g/L of oxime compound, 0.1-0.5 g/L of nonionic surfactant, 0.01-0.1 g/L of dimethylol urea and the balance of pickling solution.
The second purpose of the invention is realized by uniformly mixing and stirring the raw materials in the formula ratio to obtain the target Jatropha curcas cake meal compound corrosion inhibitor.
The third purpose of the invention is realized by applying the Jatropha curcas cake meal compound corrosion inhibitor to the acid washing 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 the Jatropha curcas cake as a raw material, adding the oxime compound, the nonionic surfactant and the dimethylol urea and the balance of the pickling solution has 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 compound corrosion inhibitor for the jatropha curcas cake meal comprises 0.1-1.0 g/L of jatropha curcas cake meal extract, 0.05-0.5 g/L of oxime compound, 0.1-0.5 g/L of nonionic surfactant, 0.01-0.1 g/L of dimethylol urea and the balance of pickling solution.
The oxime compound is dimethylglyoxime.
The nonionic surfactant is OT.
The jatropha curcas cake extract is prepared from jatropha curcas cake serving 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 the Jatropha curcas cake pulp to obtain Jatropha curcas cake pulp powder a;
B. extraction: adding an ethanol solution with the volume 20-40 times that of the Jatropha curcas cake meal into the Jatropha curcas cake meal powder a, and soaking at 10-30 ℃ for 2-4 h to obtain a material b; refluxing and extracting the material b in a water bath at the temperature of 50-80 ℃ for 2-6 h, and performing suction filtration to obtain an extracting solution c;
C. concentration: 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. and (3) extraction: adding petroleum ether with the volume 2-5 times that of the concentrated solution d into the concentrated solution d, fully oscillating, standing for 12-48 h 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 10-30 min 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 jatropha curcas cake 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 jatropha curcas cake, placing the dried material in a blast oven, and drying the material at the 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 Jatropha curcas cake extract comprises the following specific operations:
A. pretreatment: collecting Jatropha curcas seed cake meal, air-drying, placing in a blast oven, drying at a constant temperature of 60 ℃ for 48-60 h, taking out, naturally cooling to room temperature, and crushing to obtain Jatropha curcas seed cake meal powder with the particle size of 300-1000 mu m;
B. extraction: adding 20-60% ethanol solution into the Jatropha curcas cake meal powder, soaking for 2-4 h at room temperature (10-30 ℃), performing reflux extraction for 2-6 h in a water bath at 50-80 ℃, wherein the solid-liquid ratio is 1: 20-40;
C. concentration: vacuum-filtering the ethanol extract obtained by refluxing to remove Jatropha curcas cake residue powder contained in the ethanol extract, and then carrying out rotary evaporation and concentration on the ethanol extract on the solution on a rotary evaporator at 40-80 ℃ until the volume of the solution is 1/2-1/3;
D. and (3) extraction: adding petroleum ether with the volume 2-5 times that of the concentrated ethanol extract, fully shaking, standing for 12-48 h, 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 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) post-treatment: and (3) performing rotary evaporation on the extracted lower layer liquid to 40-60 ml, putting the evaporated liquid into an evaporation dish, drying the liquid in a forced air drying oven at 50-70 ℃ for 12-24 h, and shoveling the solid by a crystallization shovel to obtain the target jatropha curcas cake extract.
The preparation method of the Jatropha curcas cake meal compound corrosion inhibitor comprises the step of uniformly mixing and stirring the raw materials in the formula ratio to obtain the target Jatropha curcas cake meal compound corrosion inhibitor.
The application of the Jatropha curcas cake meal compound corrosion inhibitor is the application of the Jatropha curcas cake meal compound corrosion inhibitor in the acid cleaning of steel materials.
The invention is further illustrated by the following specific examples:
example 1
Preparation of Jatropha curcas cake extract
A. Pretreatment: collecting Jatropha curcas seed cake meal, air-drying, placing 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 Jatropha curcas seed cake meal powder with the particle size of 150-2000 mu m;
B. extraction: adding 10-70% ethanol solution into the Jatropha curcas cake meal powder, soaking for 2-6 h at room temperature (5-35 ℃) with the solid-liquid ratio of 1: 25-50, and then performing reflux extraction for 3-9 h in water bath at the temperature of 60-85 ℃;
C. concentration: vacuum-filtering the ethanol extract obtained by refluxing to remove Jatropha curcas cake residue powder contained in the ethanol extract, and then carrying out rotary evaporation and concentration on the ethanol extract on the solution at 45-75 ℃ on a rotary evaporator to obtain 1/4-1/2 volume;
D. and (3) extraction: adding petroleum ether with the volume 2-6 times that of the concentrated ethanol extract, fully shaking, standing for 15-60 hours, 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 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) post-treatment: and (3) performing rotary evaporation on the extracted lower layer liquid to 40-60 ml, putting the evaporated liquid into an evaporation dish, drying the liquid in a forced air drying oven at 50-70 ℃ for 12-24 h, and shoveling the solid by a crystallization shovel to obtain the target jatropha curcas cake extract.
Embodiment 2-preparation of Jatropha curcas cake meal compounded metal corrosion inhibitor
0.5g of Jatropha curcas cake extract, 0.1g of oxime compound dimethylglyoxime, 0.3 g of non-ionic surfactant OT and 0.1g of dimethylol urea in the example 1 are added with 1L of hydrochloric acid solution with the concentration of 0.5-5.0 mol/L, and the target Jatropha curcas cake compound corrosion inhibitor is obtained after uniform stirring.
Example 3 preparation of Jatropha curcas cake meal compounded metal corrosion inhibitor
1.0g of the jatropha curcas cake extract, 0.5g of oxime compound dimethylglyoxime, 0.5g of non-ionic surfactant OT and 0.1g of dimethylol urea in the example 1 are taken, 1L of sulfuric acid washing liquor with the concentration of 0.5-5.0 mol/L is added, and the mixture is uniformly stirred to obtain the target jatropha curcas cake compound corrosion inhibitor.
Example 4 preparation of invasive plant compounded corrosion inhibitor for steel pickling
1.0g of Jatropha curcas cake extract, 0.5g of oxime compound dimethylglyoxime, 0.5g of nonionic surfactant OT and 0.1g of dimethylol urea in the example 1 are taken, 1L of phosphoric acid lotion with the concentration of 0.5-10.0 mol/L is added, and the mixture is uniformly stirred to obtain the target agricultural and forestry waste compound corrosion inhibitor.
Test example 1 acid pickling of Steel Material
The steel material is selected as cold-rolled steel sheet, the corrosion inhibitor compounded in the embodiment 2 is injected and mixed uniformly, and the corrosion inhibition performance can reach more than 94% in different corrosion soaking times (6-156 hours) at different temperatures (20-50 ℃). Table 1 shows the 1.0 mol/L HCl test data, the method is weight loss.
TABLE 1 Corrosion inhibition rate of Jatropha curcas cake meal compound corrosion inhibitor on cold rolled steel in 1.0 mol/L HCl
Test example 2 acid pickling of Steel Material
The steel material is selected as cold-rolled steel sheet, the corrosion inhibitor compounded in the embodiment 3 is injected and uniformly mixed, and the corrosion inhibition performance can reach more than 94% in different corrosion soaking times (6-48 h) at different temperatures (20-50 ℃). Table 2 shows the 3.0 mol/L HCl test data, the method is weight loss.
TABLE 2 Corrosion inhibition rate of Jatropha curcas cake meal compound corrosion inhibitor on cold rolled steel in 3.0 mol/L HCl
Test example 3 acid cleaning of Steel Material
The steel material is selected as cold-rolled steel sheet, the corrosion inhibitor compounded in the embodiment 3 is injected and mixed uniformly, and the corrosion inhibition performance can reach more than 95% in different corrosion soaking times (6-96 h) at different temperatures (20-50 ℃). Table 3 shows 1.0 mol/L H2SO4Test data, the method is a weight loss method.
TABLE 3 Jatropha curcas cake compound corrosion inhibitor at 1.0 mol/L H for cold rolled steel2SO4Middle inhibition rate
Test example 4 acid pickling of Steel Material
The steel material is selected as cold-rolled steel sheet, the corrosion inhibitor compounded in the embodiment 4 is injected and mixed uniformly, and the corrosion inhibition performance can reach more than 93% in different corrosion soaking times (6-120 h) at different temperatures (20-50 ℃). Table 4 shows 1.0 mol/L H3PO4Test data, the method is a weight loss method.
TABLE 4 Jatropha curcas cake compound corrosion inhibitor at 1.0 mol/L H for cold rolled steel3PO4Middle inhibition rate
Test example 5 acid cleaning of Steel Material
The steel material is selected as cold-rolled steel sheet, the corrosion inhibitor compounded in the embodiment 4 is injected and mixed uniformly, and the corrosion inhibition performance can reach more than 91% in different corrosion soaking times (6-120 h) at different temperatures (20-50 ℃). Table 5 shows 7.0 mol/L H3PO4Test data, the method is a weight loss method.
TABLE 5 Jatropha curcas compound corrosion inhibitor at 7.0 mol/L H for cold rolled steel3PO4Middle inhibition rate
Claims (10)
1. The compound corrosion inhibitor for the jatropha curcas cake is characterized by comprising 0.1-1.0 g/L of jatropha curcas cake extract, 0.05-0.5 g/L of oxime compound, 0.1-0.5 g/L of nonionic surfactant, 0.01-0.1 g/L of dimethylol urea and the balance of pickling solution.
2. The Jatropha curcas cake compound corrosion inhibitor according to claim 1, wherein the oxime compound is dimethylglyoxime.
3. The Jatropha curcas cake meal compound corrosion inhibitor according to claim 1, wherein the nonionic surfactant is OT.
4. The Jatropha curcas cake compound corrosion inhibitor according to claim 1, wherein the Jatropha curcas cake extract is prepared by taking Jatropha curcas cake as a raw material through steps of pretreatment, extraction, concentration, extraction and post-treatment, and specifically comprises the following steps:
A. pretreatment: drying, crushing and sieving the Jatropha curcas cake pulp to obtain Jatropha curcas cake pulp powder a;
B. extraction: adding an ethanol solution with the volume 20-40 times that of the Jatropha curcas cake meal into the Jatropha curcas cake meal powder a, and soaking at 10-30 ℃ for 2-4 h to obtain a material b; refluxing and extracting the material b in a water bath at the temperature of 50-80 ℃ for 2-6 h, and performing suction filtration to obtain an extracting solution c;
C. concentration: 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. and (3) extraction: adding petroleum ether with the volume 2-5 times that of the concentrated solution d into the concentrated solution d, fully oscillating, standing for 12-48 h 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 10-30 min 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 jatropha curcas cake extract.
5. The compound corrosion inhibitor for the jatropha curcas cake meal according to claim 4, wherein the drying in the step A comprises air drying and constant temperature drying, and specifically, the jatropha curcas cake meal which is a waste is dried in an air drying oven and dried at a constant temperature of 50-70 ℃ for 48-60 hours.
6. The Jatropha curcas cake meal compound corrosion inhibitor according to claim 4, wherein the volume concentration of the ethanol solution in the step B is 20-60%.
7. The Jatropha curcas cake compound corrosion inhibitor according to claim 4, wherein the evaporation in step E is rotary evaporation.
8. The Jatropha curcas cake meal compound corrosion inhibitor according to claim 4, wherein the drying in the step E is drying at 50-70 ℃ for 12-24 h.
9. A preparation method of the Jatropha curcas cake meal compound corrosion inhibitor as defined in any one of claims 1 to 8, characterized in that the target Jatropha curcas cake meal compound corrosion inhibitor is obtained by mixing and stirring the raw materials in the formula ratio uniformly.
10. The application of the Jatropha curcas cake compound corrosion inhibitor in claims 1-8 is characterized in that the Jatropha curcas cake compound corrosion inhibitor is applied to acid washing of steel materials.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8790457B1 (en) * | 2011-05-06 | 2014-07-29 | Cortec Corporation | Bio-based corrosion inhibitors |
| CN105755484A (en) * | 2016-05-14 | 2016-07-13 | 西南林业大学 | High-efficient compounding plant inhibitor as well as preparation method and application thereof |
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2019
- 2019-12-11 CN CN201911266861.3A patent/CN110952105A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8790457B1 (en) * | 2011-05-06 | 2014-07-29 | Cortec Corporation | Bio-based corrosion inhibitors |
| CN105755484A (en) * | 2016-05-14 | 2016-07-13 | 西南林业大学 | High-efficient compounding plant inhibitor as well as preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 寇杰: "《腐蚀与防腐》", 31 July 2016, 中国石油大学出版社 * |
| 邓书端等: "迎春花叶提取物在磷酸介质中对钢的缓蚀作用", 《腐蚀研究》 * |
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Application publication date: 20200403 |