CN115181977B - Preparation method of houttuynia cordata extract, houttuynia cordata extract and application of houttuynia cordata extract - Google Patents
Preparation method of houttuynia cordata extract, houttuynia cordata extract and application of houttuynia cordata extract Download PDFInfo
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- CN115181977B CN115181977B CN202210835706.4A CN202210835706A CN115181977B CN 115181977 B CN115181977 B CN 115181977B CN 202210835706 A CN202210835706 A CN 202210835706A CN 115181977 B CN115181977 B CN 115181977B
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- houttuynia cordata
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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
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
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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
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- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
The invention discloses a preparation method of a houttuynia cordata extract, which comprises the following steps: (1) Weighing 20-30 parts of houttuynia cordata powder and 150-200 parts of ethanol solution; (2) Reflux-heating herba Houttuyniae powder and ethanol solution, and vacuum filtering to obtain filtrate; (3) heating and evaporating the filtrate to obtain brown viscous liquid; (4) Drying the brown viscous liquid, and cooling to normal temperature to obtain herba Houttuyniae extract. The invention also discloses a houttuynia cordata extract, which is prepared by adopting the preparation method of the houttuynia cordata extract. The houttuynia cordata extract can be applied to a metal corrosion inhibitor, can form a good adsorption film layer on the surface of a base material, slows down corrosion of the base material, plays a good corrosion inhibition role, is extracted from edible houttuynia cordata, is simple in preparation process, low in cost, safe and nontoxic, and free of pollution to the environment, and is a green plant type corrosion inhibitor.
Description
Technical Field
The invention relates to the technical field of corrosion inhibitors, in particular to a preparation method of a houttuynia cordata extract, the houttuynia cordata extract and application thereof.
Background
The corrosion inhibitor is a chemical substance or compound which exists in the environment or medium in proper concentration and form and can prevent or slow down the corrosion of materials, and in various methods for metal corrosion prevention, the corrosion inhibitor is a method which has simple and convenient process, low cost and strong applicability, and has been widely applied to the fields of exploitation and refining of petroleum and natural gas, machinery, chemical industry, energy sources and the like. Production practices show that the corrosion rate of metals in acidic media far exceeds the corrosion rates in other media, and therefore, research on corrosion inhibitors for metals in acidic media is an important topic. Currently, corrosion inhibitors on the market can be divided into inorganic corrosion inhibitors (chromates, nitrites, silicates, molybdates, tungstates, polyphosphates, zinc salts and the like), organic corrosion inhibitors (phosphonic acids, phosphonates, phosphonic acids, boracic benzothiazoles, benzotriazoles, sulfonated lignin and the like) and polymer corrosion inhibitors according to chemical components, but because most of the inorganic corrosion inhibitors and the organic corrosion inhibitors contain heavy metal elements and phosphorus elements, direct discharge can pollute water bodies, and most of the polymer corrosion inhibitors have poor biocompatibility and are difficult to degrade, so that the adoption of the corrosion inhibitors on the market can cause environmental pollution and even harm human health in serious cases.
Disclosure of Invention
In view of the above, the present invention provides a preparation method of herba Houttuyniae extract, herba Houttuyniae extract and application thereof to solve the above problems.
The technical scheme adopted for solving the technical problems is as follows:
a preparation method of herba Houttuyniae extract comprises the following steps:
(1) Weighing 20-30 parts of cordate houttuynia powder and 150-200 parts of ethanol solution according to parts by weight;
(2) Placing herba Houttuyniae powder and ethanol solution in Soxhlet extractor, heating for refluxing, and vacuum filtering to obtain filtrate;
(3) Heating and evaporating the filtrate in a rotary evaporator to obtain brown viscous liquid;
(4) Drying the brown viscous liquid in a blast drier, and cooling to normal temperature to obtain herba Houttuyniae extract.
Further, the preparation method of the houttuynia cordata powder in the step (1) comprises the following steps:
selecting cordate houttuynia stem and leaf, washing the cordate houttuynia stem and leaf with water for 3-5 times, drying in a blast drier, grinding and crushing to obtain cordate houttuynia powder.
Further, the temperature of the blast drier is 50-60 ℃,
further, the drying time is 10-12 h.
Further, the mass fraction of the ethanol solution in the step (1) is 70%.
Further, the heating reflux time in the step (2) is 4-6 h.
Further, the temperature of the blast drier in the step (4) is 60-70 ℃.
Further, the drying time in the step (4) is 20-24 hours.
A herba Houttuyniae extract is prepared by the method for preparing herba Houttuyniae extract.
Further, the houttuynia cordata extract is used as a metal corrosion inhibitor.
The beneficial effects of the invention are as follows:
the houttuynia cordata corrosion inhibitor prepared by the invention contains polar groups such as hydroxyl, carboxyl and carbonyl which are easy to protonate in an acidic medium, the protonated corrosion inhibitor can be adsorbed on the surface of a base material through electrostatic action and form a good adsorption film layer, so that the corrosion of the base material is slowed down, and a good corrosion inhibition effect is achieved.
Drawings
FIG. 1 is an infrared spectrogram of a houttuynia cordata corrosion inhibitor in an experimental example of the invention;
FIG. 2 is a Tafel polarization curve diagram of Q235 steel in 1M hydrochloric acid medium containing houttuynia cordata corrosion inhibitors with different concentrations in experimental examples of the invention;
FIG. 3 is an electrochemical impedance spectrum of Q235 steel in 1M hydrochloric acid solution containing houttuynia cordata extract with different concentrations in experimental example of the present invention;
FIG. 4 is an equivalent circuit diagram of Q235 steel in 1M hydrochloric acid medium to which houttuynia cordata extract was added in experimental example of the present invention.
Detailed Description
The present invention will now be described in detail with reference to the accompanying drawings. The figure is a simplified schematic diagram illustrating the basic structure of the invention only by way of illustration, and therefore it shows only the constitution related to the invention.
The invention provides a houttuynia cordata corrosion inhibitor, which comprises a houttuynia cordata extract, and a preparation method of the houttuynia cordata extract comprises the following steps:
(1) Selecting cordate houttuynia stem and leaf, washing the cordate houttuynia stem and leaf with water for 3-5 times, drying in a blast drier at 50-60 ℃ for 10-12 h, grinding and crushing to obtain cordate houttuynia powder.
(2) According to the weight portions, 20 to 30 portions of cordate houttuynia powder and 150 to 200 portions of 70 percent ethanol solution are respectively weighed.
(3) Placing houttuynia cordata powder and ethanol solution in a Soxhlet extractor, heating and refluxing for 4-6 hours, and carrying out vacuum filtration to obtain filtrate.
(4) The filtrate was heated in a rotary evaporator to evaporate, thus obtaining a brown viscous liquid.
(5) And (3) placing the brown viscous liquid into a blast drier, drying for 20-24 hours at the temperature of 60-70 ℃, and cooling to normal temperature to obtain the cordate houttuynia extract.
Examples
The houttuynia cordata corrosion inhibitor of the embodiment comprises houttuynia cordata extracts, and the preparation method of the houttuynia cordata extracts comprises the following steps:
(1) Selecting stems and leaves of houttuynia cordata, washing stems and leaves of houttuynia cordata with water for 4 times, drying in a blast drier at 60 ℃ for 12 hours, grinding and crushing to obtain houttuynia cordata powder.
(2) 30 parts of cordate houttuynia powder and 200 parts of 70% ethanol solution in mass fraction are respectively weighed according to parts by weight.
(3) Placing houttuynia cordata powder and ethanol solution in a Soxhlet extractor, heating and refluxing for 4-6 hours, and carrying out vacuum filtration to obtain filtrate.
(4) The filtrate was heated in a rotary evaporator to evaporate, thus obtaining a brown viscous liquid.
(5) Drying the brown viscous liquid in a blast drier at 60deg.C for 24 hr, and cooling to room temperature to obtain herba Houttuyniae extract.
Experimental example
(1) Infrared characterization:
taking a certain amount of samples of the houttuynia cordata corrosion inhibitor prepared in the embodiment, dissolving the samples with chloroform, and carrying out infrared spectrum test on the houttuynia cordata corrosion inhibitor by adopting a KBr tabletting method, wherein the measurement range is 400-4000 cm -1 The measurement results are shown in fig. 1. In FIG. 1, strong absorption peaks at 1730cm-1 and 1621cm-1 are C=O and C=C stretching vibration peaks, and strong absorption broad dispersion peaks at 3350cm-1 are stretching vibration of O-H among carboxyl (-COOH), hydroxyl (-OH) and phenolic hydroxyl (Ar-OH)A peak. As can be seen from FIG. 1, the houttuynia cordata corrosion inhibitor contains polar groups such as hydroxyl, carboxyl, carbonyl and the like which are easy to protonate in an acidic medium, and the protonated corrosion inhibitor can be adsorbed on the surface of a substrate through electrostatic action to form a good adsorption film layer, so that the corrosion of the substrate is slowed down, and a good corrosion inhibition effect is achieved.
(2) Weight loss experiment:
selecting six Q235 steel sample plates, sequentially polishing the surfaces of the six Q235 steel sample plates to have mirror surface effects by using sand paper with the specification of 220#, 800#, 1000#, 2000#, sequentially flushing by using absolute ethyl alcohol and deionized water, drying by using electric hair drier cold air, accurately weighing and recording the six polished Q235 steel sample plates by using an electronic analytical balance; weighing 0.4g, 0.8g, 1.2g, 1.6g and 2.0g of the houttuynia cordata corrosion inhibitor samples prepared in the embodiment respectively, weighing six parts of 1M hydrochloric acid, adding the weighed houttuynia cordata corrosion inhibitor samples into five parts of 1M hydrochloric acid respectively, simultaneously leaving one part of 1M hydrochloric acid as a blank reference example, sequentially soaking six Q235 steel sample plates into the 1M hydrochloric acid of the blank example and the 1M hydrochloric acid containing the houttuynia cordata corrosion inhibitors with different concentrations in an environment of 25 ℃, taking out after 3 hours, cleaning according to the method, drying, accurately weighing, and calculating a weightlessness average value through multiple experiments; then, the soaking time was changed to 24 hours, the above experiment was repeated, and the corrosion inhibition efficiency was calculated, and the results are shown in Table 1.
Table 1: weight loss and corrosion inhibition efficiency of sample wafer in 1M hydrochloric acid containing houttuynia cordata corrosion inhibitors with different concentrations
As shown in Table 1, the houttuynia cordata corrosion inhibitor has good corrosion inhibition effect on the Q235 steel sample, and the greater the concentration of the houttuynia cordata corrosion inhibitor is, the greater the adsorption coverage of the houttuynia cordata corrosion inhibitor on the surface of the sample is, the higher the corrosion inhibition efficiency is, and when the concentration of the houttuynia cordata corrosion inhibitor reaches 2.0g/L, the corrosion inhibition efficiency is the maximum. Compared with the corrosion inhibition efficiency soaked for 3 hours, the corrosion inhibition efficiency soaked for 24 hours has small change, which indicates that the adsorption film formed by the houttuynia cordata corrosion inhibitor on the surface of the sample wafer has good adsorption film, and the phenomenon of rupture of the adsorption film caused by corrosion of the steel sheet does not occur after long-time soaking.
(3) Electrochemical testing:
the corrosion inhibition efficiency of the houttuynia cordata corrosion inhibitor is tested by adopting an electrochemical workstation under the environment of 25 ℃, the research electrode is a Q235 steel cylindrical electrode with a non-working surface encapsulated by epoxy resin, the surface treatment is carried out on the research electrode before working, the treatment method is the same as that of a weightlessness experiment, and the working area is 1cm 2 The reference electrode adopts a saturated calomel electrode, and the auxiliary electrode adopts a platinum electrode. First, an open circuit potential (E) ocp ) Measurement, wait E ocp Polarization curve test is carried out after stabilization, and scanning interval is + -300 mV (vs E) ocp ) The scan rate was 0.5mV/s and the test results are shown in FIG. 2; as can be seen from FIG. 2, the corrosion potential E of Q235 steel after adding the houttuynia cordata corrosion inhibitor corr Negative, corrosion current density I c The corrosion inhibition efficiency eta is calculated by the formula (1), which is smaller and smaller along with the increase of the concentration of the cordate houttuynia extract, which shows that the anodic dissolution and cathodic hydrogen evolution reaction of the Q235 steel are inhibited to a certain extent.
In the formula, ic and I' c represent corrosion current densities of Q235 steel in corrosion media without and with houttuynia cordata corrosion inhibitors, respectively, and the results are shown in Table 2.
Table 2: tafel polarization curve fitting parameter values
As can be seen from Table 2, E after adding the houttuynia cordata corrosion inhibitor corr Negative migration is within 50mV, and cathode and anode reactions are obviously inhibited at the same time, so that the cordate houttuynia corrosion inhibitor can be presumed to be a mixed corrosion inhibitor, and the mechanism is a geometric coverage effect, namely, a large number of corrosion inhibition molecules of the cordate houttuynia corrosion inhibitor are adsorbed on the surface of an electrode of Q235 steel, thereby reducing corrosion reaction active points and inhibiting corrosion reaction. In addition, after the houttuynia cordata corrosion inhibitor is added, the Tafel slope of the cathode and the anode is increasedb c And b a The corrosion inhibition effect of the corrosion inhibition molecules in the houttuynia cordata corrosion inhibitor is mainly realized by inhibiting the hydrogen evolution process, the corrosion inhibition efficiency eta is increased along with the increase of the concentration of the houttuynia cordata corrosion inhibitor, and the corrosion inhibition efficiency reaches 93.82% when the concentration of the houttuynia cordata extract is 2.0g/L, which is basically consistent with the experimental result of a weightless method.
At E ocp Applying a sine wave of + -5 mV to perform electrochemical impedance spectrum test, and scanning at a frequency range of 10- 2 ～10 5 Hz, test results are shown in fig. 3; finally, adopting Zview software of Solartron company to analyze impedance spectrum; as can be seen from FIG. 3, the impedance spectra of the Q235 steel only comprises one capacitive arc in the blank solution and the solution added with the houttuynia cordata corrosion inhibitor, which shows that the electrode reaction is controlled by only one time constant.
The impedance spectra were fitted using an equivalent circuit as shown in FIG. 4, and the resulting data are shown in Table 3, where R f Is membrane resistance, R ct For the charge transfer resistance, consider the "dispersion effect", a constant phase angle element CPE f And CPE (customer premise equipment) dl The representation represents a film capacitance and an electric double layer capacitance, respectively. Corrosion inhibition efficiency was calculated by formula (2):
wherein R is o ct 、R ct The charge transfer resistance of the system without and with HCE added is shown in table 3.
Table 3: EIS spectrum fitting obtained parameter value (houttuynia cordata corrosion inhibitor)
As can be seen from fig. 3 and table 3, as the concentration of the houttuynia cordata corrosion inhibitor increases, the radius of the arc resistance increases gradually, the charge transfer resistance increases gradually, the corrosion inhibition efficiency increases gradually, and the electric double layer capacitor decreases gradually, which indicates that the surface of the Q235 steel forms a compact adsorption film layer due to adsorption of a large number of houttuynia cordata corrosion inhibitor molecules with smaller dielectric constants, and the contact of water molecules on the surface of the Q235 steel is prevented. When the concentration of the houttuynia cordata extract is 2.0g/L, the corrosion inhibition efficiency of the houttuynia cordata corrosion inhibitor reaches 93.76% at the highest.
Therefore, the houttuynia cordata corrosion inhibitor prepared by the invention contains polar groups such as hydroxyl, carboxyl, carbonyl and the like which are easy to protonate in an acidic medium, the protonated corrosion inhibitor can be adsorbed on the surface of a base material through electrostatic action and form a good adsorption film layer, and the corrosion of the base material is slowed down, so that a good corrosion inhibition effect is achieved.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. The technical scope of the present invention is not limited to the description, but must be determined according to the scope of claims.
Claims (8)
1. The application of the houttuynia cordata extract as the metal corrosion inhibitor is characterized in that the concentration of the corrosion inhibitor is 0.4020g/L or 0.8050g/L, the soaking time is 24 hours,
the preparation method of the houttuynia cordata extract comprises the following steps:
(1) Weighing 20-30 parts of houttuynia cordata powder and 150-200 parts of ethanol solution according to parts by weight;
(2) Placing herba Houttuyniae powder and ethanol solution in Soxhlet extractor, heating for refluxing, and vacuum filtering to obtain filtrate;
(3) Heating and evaporating the filtrate in a rotary evaporator to obtain brown viscous liquid;
(4) Drying the brown viscous liquid in a blast drier, and cooling to normal temperature to obtain herba Houttuyniae extract.
2. The use of a houttuynia cordata extract as a metal corrosion inhibitor according to claim 1, wherein the preparation method of the houttuynia cordata powder in the step (1) comprises the following steps:
selecting cordate houttuynia stems and leaves, washing the cordate houttuynia stems and leaves with water for 3-5 times, drying in a blast drier, grinding and crushing to obtain cordate houttuynia powder.
3. The use of a houttuynia cordata extract as a metal corrosion inhibitor according to claim 2, wherein the temperature of the blast drier in the step (1) is 50-60 ℃.
4. The use of a houttuynia cordata extract as a metal corrosion inhibitor according to claim 2, wherein the drying time is 10-12 hours.
5. The use of a houttuynia cordata extract as claimed in claim 1, wherein the mass fraction of the ethanol solution in the step (1) is 70%.
6. The use of a houttuynia cordata extract as a metal corrosion inhibitor according to claim 1, wherein the heating reflux time in the step (2) is 4-6 hours.
7. The use of a houttuynia cordata extract as a metal corrosion inhibitor according to claim 1, wherein the temperature of the blast drier in the step (4) is 60-70 ℃.
8. The use of a houttuynia cordata extract as a metal corrosion inhibitor according to claim 1, wherein the drying time in the step (4) is 20-24 hours.
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