CN108754510A - A kind of compound restrainer and preparation method thereof containing Schiff - Google Patents
A kind of compound restrainer and preparation method thereof containing Schiff Download PDFInfo
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- CN108754510A CN108754510A CN201810651109.XA CN201810651109A CN108754510A CN 108754510 A CN108754510 A CN 108754510A CN 201810651109 A CN201810651109 A CN 201810651109A CN 108754510 A CN108754510 A CN 108754510A
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- methionine
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- 0 CCI1(C)=C/C=C/CC(C)/C=C1\C(N)=C*1CC(C)C1 Chemical compound CCI1(C)=C/C=C/CC(C)/C=C1\C(N)=C*1CC(C)C1 0.000 description 2
Classifications
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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
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
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- Organic Chemistry (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention belongs to carbon steel pickling technical fields,Disclose a kind of compound restrainer and preparation method thereof containing Schiff,60mL chloroform solns are first added in three-necked flask,Then 5.35g pyridine-2-formaldehydes and 7.45g methionine are added,Magnetic agitation,1h is heated to reflux all to dissolve to solid,Then 5 drop glacial acetic acids are added dropwise and as catalyst and adjust reacting liquid pH value,After continuing heating reflux reaction for 24 hours,It is stirred to react 2h at room temperature,Then reaction solution is put into crystallisation by cooling in refrigerator,Decompression filters removing solvent and obtains yellow-brown solid,Through recrystallizing methanol,Methionine Schiff derivative is obtained after vacuum drying,Methionine Schiff derivative is weighed to compound by certain mass ratio with sodium carboxymethylcellulose,A kind of compound restrainer is made.Composite corrosion inhibitor provided by the invention has excellent corrosion inhibition in 0.5M hydrochloric acid lotions to carbon steel metal, and for inhibition efficiency up to 94% or more, inhibiter consumption is few, and it is existing insufficient in use to overcome single methionine corrosion inhibiter.
Description
Technical field
The invention belongs to carbon steel pickling technical fields more particularly to a kind of composite corrosion inhibitor and preparation method thereof, specifically
Say it is a kind of methionine Schiff derivative 2- (N- picolylimines) -4- methylmercapto butyric acids (MD) and carboxymethyl cellulose
Sodium (MD) compound corrosion inhibitor and preparation method thereof.
Background technology
Important method one of of the pickling as chemical cleaning, it is quick, efficient due to its features such as, be widely used in carbon steel
The incrustation scale of equipment (including boiler, dynamical system, heat exchanger etc.) and its component is removed and derusting process.Hydrochloric acid is as most common
Spent pickling acid can also dissolve plain steel while chemical reaction with the incrustation scale or rusty scale of metal surface, to equipment and
Its component causes different degrees of corrosion, not only influences industrial production efficiency, and there is also security risks.Corrosion inhibiter is a kind of with suitable
When concentration and form be present in environment (medium) can slow down either prevent corrosion chemical substance or compound.Addition
Corrosion inhibiter is anti-corrosion measure the most main in acid cleaning process, because it is with of low cost, simple process, strong applicability, protection
The advantages that effect is good is widely used in pickling of metal field.Amino acids substance because having hydrophile amino, carboxylic simultaneously
The groups such as base and hydrophobic substituent group, it is nontoxic to environment in addition, water-soluble is good, corrosion mitigating effect is good, of low cost etc. excellent
Gesture and be widely used as metal inhibitor use.Methionine (Met) is a kind of sulfur-containing amino acid, contained by S, N atom in acid
Property solution in there is potential corrosion inhibition to metal material, and it has the advantages that amino acid inhibitor, is a kind of to have very much hair
The green corrosion inhibitor of potentiality is opened up, but when methionine is as corrosion inhibiter, since its molecular structure is fairly simple, the suction in metal surface
Attached property is insufficient, lacks hydrophobic structure in addition, there is the deficiencies that inhibition efficiency is not high or dosage is excessive, to limit it
Practical application in corrosion control field.By introducing polar group or hydrophobic group containing N, O, S atom on methionine molecule
Group can effectively improve its corrosion inhibition, and currently used synthetic method is accessed by the amidation process on amido or carboxyl
Various groups, but such method is there is severe reaction conditions, step is complicated or expensive reagents, the deficiencies of toxicity is big, limits
Its application development.In addition, with the raising of corrosion control requirement and the progress of inhibiter technology, if several corrosion inhibiter compounding is made
With using the synergistic effect between them, less corrosion inhibiter being used to obtain higher inhibition efficiency.But current methionine is multiple
Research with inhibition system is also concentrated mainly on methionine and other amino acid, methionine and organic molecule or inorganic compound
Between, synergistic slow corrosion performance study between methionine and organic polymer also less studies have reported that.
In conclusion problem of the existing technology is：
(1) single methionine is as carbon steel pickling corrosion inhibitor, and because its molecular structure is simple, in metal surface, adsorptivity is not
The shortcomings of sufficient, causes its inhibition efficiency not high, cannot be satisfied the demand of practical application.
(2) when methionine is as carbon steel pickling corrosion inhibitor, to obtain higher inhibition efficiency, larger add is generally required
Amount, causes cost to increase, the wasting of resources and environmental pollution limit development and application of the methionine as corrosion inhibiter.
(3) the methionine derivative synthesizing process for accessing various groups by amidation process at present, there is reaction items
Part is harsh, and step is complicated or expensive reagents, the deficiencies of toxicity is big, limits its application development.
(4) methionine compound slow corrosion system is concentrated mainly on methionine and other amino acid, methionine and organic molecule
Or the synergistic slow corrosion between inorganic compound, these compound slow corrosion systems are not high in the prevalence of inhibition efficiency, or compounding chemical combination
The problems such as object toxicity is big, expensive, cannot be satisfied practical application request.
Solve the difficulty and meaning of above-mentioned technical problem：
Firstly, since Schiff contains C=N double bonds this special constructions, there is good coordination ability, can and transition
Metal forms complicated complex, so as to firmly be attracted to metal surface, effectively inhibits corrosion.In addition, according to knot
Structure is with physical property relationship the study found that the molecule containing the larger atom of electronegativity (such as N, O, S atom), it is possible to provide lone electron
It is right, just it can be formed on its surface protective film with the d rail effects of metal；Therefore, a kind of egg ammonia containing pyridine groups is synthesized
Sour Schiff derivative will can be obviously improved the corrosion inhibition of methionine, while the synthesis technology of Schiff is simpler,
Operability is stronger, and the cost of synthesis is relatively low, can effectively solve the deficiency of existing methionine derivative synthesis, have larger market
Application value.
Secondly, sodium carboxymethylcellulose (CMC) is a kind of organic high molecular compound, nontoxic, of low cost, is contained
There is a large amount of polar group (hydroxyl, carboxyl etc.), metal surface can be attracted to, makes up methionine Schiff derivative inhibition
The defect of film enhances the compactness of corrosion inhibiter adsorbed film, forms synergistic slow corrosion effect, further promotes corrosion inhibition, to real
Existing less corrosion inhibiter obtains higher inhibition efficiency, reduces the dosage of methionine Schiff derivative corrosion inhibiter, this is to promoting
Industrial applications into methionine Schiff derivative corrosion inhibiter are of great significance.
Invention content
In view of the problems of the existing technology, the present invention provides one kind containing the compound restrainer of Schiff and its system
Preparation Method, corrosion inhibiter preparation process is easy, chemical property is stable, of low cost.
The invention is realized in this way the methionine Schiff derivative and its compound slow with sodium carboxymethylcellulose
The preparation method of erosion agent includes the following steps：
60mL chloroform solns are added in step 1 in the three-necked flask equipped with oil bath heating and magnetic stirring apparatus,
Then 5.35g pyridine-2-formaldehydes (PCD) and 7.45g methionine (Met) are added in flask, start magnetic agitation, is heated to reflux
1h is all dissolved to solid；
5 drop glacial acetic acids are added dropwise into reaction flask and as catalyst and adjust reacting liquid pH value, continue to heat back for step 2
After stream reaction for 24 hours, then reaction 2h is stirred at room temperature, reaction solution is then put into crystallisation by cooling in refrigerator, decompression, which filters, to be removed
Solvent obtains yellow-brown solid, and product is dried in vacuo to obtain methionine Schiff derivative 2- (N- pyridines after recrystallizing methanol
Methylene imine) -4- methylmercapto butyric acids (MD)；
Step 3, using good synergistic corrosion inhibition between above-mentioned synthetic product MD and sodium carboxymethylcellulose (CMC),
Take methionine Schiff derivative (MD) with sodium carboxymethylcellulose (CMC) by 4：3 mass ratio is compounded, and obtains one
Kind high efficiency composition corrosion inhibiter.
Further, in the step 1：Pyridine-2-formaldehyde 0.05mol；Methionine 0.05mol.
Further, the synthesis of methionine Schiff derivative 2- (N- the picolylimines) -4- methylmercapto butyric acids
Reaction equation is：
Another object of the present invention is to provide a kind of preparation sides of the compound restrainer containing Schiff by described
Compound restrainer prepared by method, the corrosion inhibiter is by a kind of methionine Schiff derivative 2- (N- picolylimines)-
4- methylmercapto butyric acids (MD) press 4 with sodium carboxymethylcellulose (MD):3 mass ratio compounding is made, and has to carbon steel class equipment excellent
Good hydrochloric acid pickling corrosion inhibition performance, inhibition efficiency is up to 94% or more, and dosage is few, and overcoming single methionine corrosion inhibiter makes
It is insufficient present in process.
Another object of the present invention is to provide a kind of boiler anti-corrosion compounds prepared by the heat exchanger.
Another object of the present invention is to provide a kind of dynamical system anti-corrosion compounds prepared by the heat exchanger.
Another object of the present invention is to provide a kind of heat exchanger anti-corrosion compounds prepared by the heat exchanger.
In conclusion advantages of the present invention and good effect are：
The present invention has investigated the corrosion inhibiter in 0.5M hydrochloric acid lotions to carbon steel metal using weight-loss method and method of polarization curve
The corrosion inhibition of material, and observe by metallographic microscope the erosion profile of carbon steel sample, the results showed that, the composite corrosion inhibitor
There is excellent corrosion inhibition to carbon steel metal in 0.5M hydrochloric acid lotions, inhibition efficiency is up to 94% or more, and corrosion inhibiter is used
Amount is few, and it is existing insufficient in use to overcome single methionine corrosion inhibiter.Pyridine ring is introduced into methionine molecule
A kind of Schiff compound is made, increases the equiatomic electron rich group containing N, O on methionine molecule, further enhances
Its carbon steel surface adsorption capacity, to improve its corrosion inhibition to carbon steel.Utilize 2- (N- picolylimines) -4-
Good Synergistic inhibition between methylmercapto butyric acid and sodium carboxymethylcellulose, by 2- (N- picolylimines) -4- first sulphur
Base butyric acid compounds in proportion with sodium carboxymethylcellulose, is prepared for a kind of efficient metal composite corrosion inhibitor.
Description of the drawings
Fig. 1 is the preparation method flow chart of the compound restrainer provided in an embodiment of the present invention containing Schiff.
Fig. 2 is tafel pole of the carbon steel provided in an embodiment of the present invention in the 0.5M hydrochloric acid lotions containing different inhibition systems
Change curve graph.
Fig. 3 be it is provided in an embodiment of the present invention be free of or 0.5M hydrochloric acid lotions containing different corrosion inhibiter in impregnate for 24 hours after
The surface shape Manners metallographs of carbon steel sample；
In figure：(a) blank sample；(b) corrosion inhibiter is free of；(c) Met containing 40mg/L；(d) MD+30mg/L containing 40mg/L
CMC。
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
A kind of compound restrainer containing Schiff (Schiff) alkali provided in an embodiment of the present invention, by methionine and pyrrole
Methionine Schiff derivative 2- (N- picolylimines) -4- methylmercapto butyric acids are made in the reaction of pyridine -2- formaldehyde, then by it
It compounds and is made with sodium carboxymethylcellulose.
As shown in Figure 1, the preparation method of the compound restrainer provided in an embodiment of the present invention containing Schiff includes
Following steps：
S101：60mL chloroform solns are added in the three-necked flask equipped with oil bath heating and magnetic stirring apparatus, so
5.35g pyridine-2-formaldehydes (PCD) and 7.45g methionine (Met) are added in flask afterwards, magnetic agitation is started, is heated to reflux 1h
It is all dissolved to solid；
S102：5 drop glacial acetic acids are added dropwise into reaction flask and as catalyst and adjust reacting liquid pH value, continue to be heated to reflux
After reaction for 24 hours, then reaction 2h is stirred at room temperature, reaction solution is then put into crystallisation by cooling in refrigerator, it is molten that decompression filters removing
Agent obtains yellow-brown solid, and product is dried in vacuo to obtain methionine Schiff derivative 2- (N- pyridine first after recrystallizing methanol
Base imines) -4- methylmercapto butyric acids (MD)；
S103：Utilize above-mentioned synthetic product 2- (N- picolylimines) -4- methylmercapto butyric acids (MD) and carboxymethyl cellulose
Good synergistic corrosion inhibition between plain sodium (CMC) takes MD with sodium carboxymethylcellulose (CMC) by 4：3 mass ratio is answered
Match, obtains a kind of high efficiency composition corrosion inhibiter.
The synthetic reaction equation of 2- (N- picolylimines) -4- methylmercapto butyric acids provided in an embodiment of the present invention is：
Sodium carboxymethylcellulose molecular formula：
60mL chloroform solns are added in the three-necked flask equipped with oil bath heating and magnetic stirring apparatus, then will
5.35g pyridine-2-formaldehydes (PCD) and 7.45g methionine (Met) are added in flask, start magnetic agitation, are heated to reflux 1h to admittedly
Body all dissolves, and 5 drop glacial acetic acids are then added dropwise and as catalyst and adjust reacting liquid pH value, after continuing back flow reaction for 24 hours, then
Continue to be stirred to react 2h at room temperature, reaction solution is then put into crystallisation by cooling in refrigerator, decompression suction filtration removing solvent obtains pale brown
Color solid, product are dried in vacuo and methionine Schiff derivative 2- (N- picolylimines)-are made after recrystallizing methanol
4- methylmercapto butyric acids (MD).
MD is weighed with sodium carboxymethylcellulose (CMC) by 4：3 mass ratio mixing compounding, obtains a kind of carbon steel hydrochloric acid acid
Wash composite corrosion inhibitor.Composite corrosion inhibitor is put by the concentration of 70mg/L in hydrochloric acid pickler, acid cleaning process can be effectively prevent
Corrosion of the middle hydrochloric acid solution to plain steel.
1. weight-loss method is tested
By a collection of carbon steel coupon sample of same size, with sand paper, (600# -2000#) polishing is bright step by step, and acetone cleaning removes
Oil, cold wind drying, electronic balance are precisely weighed and (are accurate to 0.0001g), then it is dipped to the hydrochloric acid of 0.5M at 25 DEG C
It in washing lotion, takes out simultaneously after a certain period of time, deionized water is rinsed, and drying is precisely weighed, and parallel test three times, is counted according to formula (1)
Calculate inhibition efficiency η.
In formula, Δ mοIt respectively represents and is free of and the average weightlessness of the steel disc of when containing corrosion inhibiter with Δ m, g.
Inhibition efficiency of 1 carbon steel of table in the 0.5M hydrochloric acid lotions containing different corrosion inhibiter
As shown in table 1, in the hydrochloric acid lotion of 0.5M, single methionine corrosion inhibiter is in a concentration of 40mg/L, to carbon
The inhibition efficiency highest of steel only has 65.66%, and as its a concentration of 160mg/L, only have to the inhibition efficiency highest of carbon steel
85.37%, otherwise it there is a problem that inhibition efficiency is not high or dosage is excessive.It is multiple using 40mg/L MD+30mg/L CMC
Corrosion inhibiter is closed, to the inhibition efficiency of carbon steel up to 95.97%, dosage is small, and inhibition efficiency is high, can meet the requirement of practical application.
2. polarization curve test experiments
Electro-chemical test is carried out using CHI660E electrochemical workstations, with the cylindrical Q235 steel discs of a diameter of 1.13cm
For working electrode, in addition to working face, lap epoxy encapsulation is polishing to minute surface with sand paper before test, cleans, removes step by step
It is used after oil.With the calomel electrode (SCE) equipped with Luggin capillary salt bridge for reference electrode, 4cm2Platinum plate electrode be auxiliary
Electrode.Wait for working electrode open circuit potential (E in testing solutionOCP) after stabilization, then carry out polarization curve test.
Tafel polarization curve of 2 carbon steel of table in the 0.5M hydrochloric acid lotions containing different inhibition systems tests main electrochemistry
Parameter
Note：EcorrIndicate the corrosion potential of metal, βc、βaThe Tafel slopes of cathode and anode, I are indicated respectivelycIndicate corrosion
Current density, η indicate inhibition efficiency.
As shown in table 2 and Fig. 2, tafel polarization curve of the carbon steel in the 0.5M hydrochloric acid lotions of the system containing compound slow corrosion is surveyed
Test result shows that composite corrosion inhibitor has excellent corrosion inhibition, inhibition efficiency dense with MD carbon steel in 0.5M hydrochloric acid lotions
The increase of degree and increase, as a concentration of 40mg/L of MD, a concentration of 30mg/L of CMC, inhibition efficiency up to 94.72%,
Far above the inhibition efficiency 63.60% of the single methionine of 40mg/L.
3. erosion profile photo is as shown in Figure 3.
As shown in figure 3, Fig. 3 a are blank sample, the cut of polishing is high-visible, without apparent corrosion phenomenon, Fig. 3 b examinations
Sample surface shows apparent and dense distribution corrosion product, and surface irregularity illustrates sample by heavy corrosion.The surfaces Fig. 3 c
Still there is more corrosion product, but closeness is substantially reduced compared with Fig. 3 b, it is certain to illustrate that methionine (Met) has sample
Corrosion inhibition.Fig. 3 d specimen surfaces are opposed flattened, it is seen that the cut of polishing, only some subtle borrosion holes, this illustrates MD and CMC
Press 4：3 mass have good Synergistic inhibition than compound corrosion inhibitor to carbon steel sample, hence it is evident that are better than methionine corrosion inhibiter.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (6)
1. a kind of preparation method of the compound restrainer containing Schiff, which is characterized in that the answering containing Schiff
Metal inhibitor preparation method is closed to include the following steps：
60mL chloroform solns are added, then in step 1 in the three-necked flask equipped with oil bath heating and magnetic stirring apparatus
By 5.35g pyridine-2-formaldehydes (and 7.45g methionine be added flask in, start magnetic agitation, be heated to reflux 1h to solid whole
Dissolving；
5 drop glacial acetic acids are added dropwise into reaction flask and as catalyst and adjust reacting liquid pH value, continue to be heated to reflux anti-for step 2
After answering for 24 hours, then reaction 2h is stirred at room temperature, reaction solution is then put into crystallisation by cooling in refrigerator, decompression, which filters, removes solvent
Yellow-brown solid is obtained, product is dried in vacuo to obtain methionine Schiff derivative 2- (N- picolyls after recrystallizing methanol
Imines) -4- methylmercapto butyric acids；
Step 3 is cooperateed with using good between above-mentioned synthetic product methionine Schiff derivative and sodium carboxymethylcellulose
Corrosion inhibition takes methionine Schiff derivative with sodium carboxymethylcellulose by 4:3 mass ratio compounding obtains compound slow
Lose agent.
2. the preparation method of the compound restrainer containing Schiff as described in claim 1, which is characterized in that the 2-
The synthetic reaction equation of (N- picolylimines) -4- methylmercapto butyric acids is：
3. compound pickling prepared by a kind of preparation method of compound restrainer containing Schiff described in claim 1 is delayed
Lose agent.
4. boiler anti-corrosion compound prepared by a kind of heat exchanger described in claim 3.
5. dynamical system anti-corrosion compound prepared by a kind of heat exchanger described in claim 3.
6. heat exchanger anti-corrosion compound prepared by a kind of heat exchanger described in claim 3.
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| CN114164430A (en) * | 2021-11-30 | 2022-03-11 | 哈尔滨工业大学（深圳） | Metal corrosion inhibitor and preparation method thereof |
| CN115181977A (en) * | 2022-07-15 | 2022-10-14 | 重庆工业职业技术学院 | Preparation method of houttuynia cordata extract, houttuynia cordata extract and application of houttuynia cordata extract |
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| CN115181977A (en) * | 2022-07-15 | 2022-10-14 | 重庆工业职业技术学院 | Preparation method of houttuynia cordata extract, houttuynia cordata extract and application of houttuynia cordata extract |
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