CN112442408B - Corrosion inhibitor composition and preparation method thereof - Google Patents

Corrosion inhibitor composition and preparation method thereof Download PDF

Info

Publication number
CN112442408B
CN112442408B CN202011354867.9A CN202011354867A CN112442408B CN 112442408 B CN112442408 B CN 112442408B CN 202011354867 A CN202011354867 A CN 202011354867A CN 112442408 B CN112442408 B CN 112442408B
Authority
CN
China
Prior art keywords
amide
acid
mixed
azelaic acid
corrosion inhibitor
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202011354867.9A
Other languages
Chinese (zh)
Other versions
CN112442408A (en
Inventor
江存
张侠婷
何彦波
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dexu New Materials Fogang Co ltd
Original Assignee
Dexu New Materials Fogang Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dexu New Materials Fogang Co ltd filed Critical Dexu New Materials Fogang Co ltd
Priority to CN202011354867.9A priority Critical patent/CN112442408B/en
Publication of CN112442408A publication Critical patent/CN112442408A/en
Application granted granted Critical
Publication of CN112442408B publication Critical patent/CN112442408B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M141/00Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
    • C10M141/12Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic compound containing atoms of elements not provided for in groups C10M141/02 - C10M141/10
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2215/042Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms containing hydroxy groups; Alkoxylated derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/08Amides
    • C10M2215/082Amides containing hydroxyl groups; Alkoxylated derivatives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/22Heterocyclic nitrogen compounds
    • C10M2215/223Five-membered rings containing nitrogen and carbon only
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2227/00Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/06Organic compounds derived from inorganic acids or metal salts
    • C10M2227/061Esters derived from boron
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/10Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

The application belongs to the technical field of metal cutting, and particularly relates to a corrosion inhibitor composition and a preparation method thereof. The application provides a corrosion inhibitor composition, which comprises isononanoic acid mixed amide, n-heptanoic acid triisopropanolamine soap, mixed azelaic acid amide, triethanolamine borate and benzotriazole; isononanoic acid mixed amides include isononanoic acid diisopropanolamide and isononanoic acid diethanolamide; the isononanoic acid diisopropanolamide has a structure shown in a formula I; the isononanoic acid diethanolamide has a structure shown in a formula II; triisopropanolamine n-heptanoate soaps have the structure of formula iii: the mixed azelaic acid amide comprises azelaic acid diiso-propanol amide, azelaic acid diethanol amide and azelaic acid mixed alcohol amide; the azelaic acid diisopropanol amide has formula IV; azelaic acid diethanolamide has formula V; the azelaic acid mixed alcohol amide has formula VI. The corrosion inhibitor composition can effectively solve the technical problem that the existing corrosion inhibitor cannot have the functions of no foam, corrosion inhibition, rust prevention and lubrication.

Description

Corrosion inhibitor composition and preparation method thereof
Technical Field
The application belongs to the technical field of metal cutting, and particularly relates to a corrosion inhibitor composition and a preparation method thereof.
Background
Metal cutting fluids are industrial fluids used in metal cutting/grinding processes to cool and lubricate tools and workpieces. In the actual use process, the cutting fluid usually corrodes a machine tool, a processing metal part and the like due to corruption, water, oxygen, processing guide rail oil, metal chips, dust and the like, and simultaneously destroys the stability of the cutting fluid, so that the cutting fluid fails. Therefore, it is necessary to add a corrosion inhibitor to the cutting fluid to prevent the cutting fluid from corroding metals during and after machining. However, in order to ensure smooth and efficient machining and reduce loss in a special machining mode such as milling or cutting, the cutting fluid needs to have excellent lubricity, cleaning property and the like in addition to certain corrosion inhibition. How to select the functional single agent and scientifically compound a plurality of functional auxiliary agents is very important.
The corrosion inhibitors on the market at present are often single in performance, only have two or three types, and even only have one function. The requirements of the metal cutting fluid cannot be met.
Disclosure of Invention
In view of the above, the application provides a corrosion inhibitor composition and a preparation method thereof, which can effectively solve the technical problems that the existing corrosion inhibitor has single performance and cannot meet the requirements of the existing metal cutting fluid.
The first aspect of the application provides a corrosion inhibitor composition, which comprises isononanoic acid mixed amide, n-heptanoic acid triisopropanolamine soap, mixed azelaic acid amide, triethanolamine borate and benzotriazole;
the isononanoic acid mixed amide comprises isononanoic acid diisopropanol amide and isononanoic acid diethanol amide;
the diisononyl isononanoate diisononyl amide has a structure shown in a formula I;
Figure BDA0002802321470000011
the isononanoic acid diethanolamide has a structure shown in a formula II;
Figure BDA0002802321470000021
the triisopropanolamine n-heptanoate soap has a structure of formula III:
Figure BDA0002802321470000022
the mixed azelaic acid amide comprises azelaic acid diiso-propanol amide, azelaic acid diethanol amide and azelaic acid mixed alcohol amide;
the azelaic acid diisopropanol amide has formula IV;
Figure BDA0002802321470000023
the azelaic acid diethanolamide has formula V;
Figure BDA0002802321470000024
the azelaic acid mixed alcohol amide has formula VI;
Figure BDA0002802321470000031
preferably, in the isononanoic acid mixed amide, the mass ratio of the isononanoic acid diisopropanol amide to the isononanoic acid diethanol amide is (3-6): 1.
preferably, the preparation method of the isononanoic acid mixed amide comprises the following steps:
mixing isononanoic acid, an alcohol amine mixture and a catalyst for reaction to prepare isononanoic acid mixed amide; wherein the alcohol amine mixture comprises diisopropanolamine and diethanolamine;
calculated according to the mass percentage, the method comprises the following steps:
24 to 39 percent of isononanoic acid;
61-76% of alcohol amine mixture;
the mass ratio of the diisopropanolamine to the diethanolamine is (4-7): 1;
the addition amount of the catalyst is 0.1-0.2% of the sum of the mass of the isononanoic acid and the mass of the alcohol amine mixture.
Preferably, in the preparation method of the isononanoic acid mixed amide, the catalyst is selected from 18-crown-6 or/and 15-crown-5;
the temperature of the mixing reaction is 110-125 ℃; the mixing reaction time is 4-5 h.
Preferably, in the method for preparing isononanoic acid mixed amide, the isononanoic acid is isononanoic acid with the temperature of 80-90 ℃.
Preferably, the preparation method of the triisopropanolamine n-heptanoate comprises the following steps:
heating n-heptanoic acid and triisopropanolamine to react to prepare triisopropanolamine n-heptanoic acid soap;
wherein, calculated according to the mass percentage, the method comprises the following steps:
18 to 25 percent of n-heptanoic acid;
75 to 82 percent of triisopropanolamine.
Preferably, in the preparation method of triisopropanolamine n-heptanoate, the heating reaction temperature is 110-130 ℃; the heating reaction time is 2-4 h.
Preferably, in the method for preparing triisopropanolamine n-heptanoate, the n-heptanoate is n-heptanoate with a temperature of 75 to 85 ℃.
Preferably, in the mixed azelaic acid amide, the mass percentages of the azelaic acid diisopropanol amide, the azelaic acid diethanol amide and the azelaic acid mixed alcohol amide are (65-75%): (13-15%): (12% to 20%).
Preferably, the preparation method of the mixed azelaic acid amide comprises the following steps: mixing the alcohol amine mixture, azelaic acid and a catalyst, and heating for reaction to obtain mixed azelaic acid amide;
wherein the alcohol amine mixture comprises diisopropanolamine and diethanolamine;
wherein, calculated according to the mass percentage, the method comprises the following steps:
67% -78% of alcohol amine mixture;
azelaic acid 22% -33%;
the mass ratio of the diisopropanolamine to the diethanolamine is (5-8) to 1; the addition amount of the catalyst is 0.1-0.2% of the sum of the mass of the alcohol amine mixture and the mass of the azelaic acid.
Preferably, in the preparation method of the mixed azelaic acid amide, the catalyst is selected from 18-crown-6 or/and 15-crown-5; the temperature of the heating reaction is 110-125 ℃; the heating reaction time is 4-5 h.
Preferably, in the preparation method of the mixed azelaic acid amide, the alcohol amine mixture is preheated to 80-90 ℃; discharging water generated in the reaction in the heating reaction process, and stopping heating until no water is distilled; and in the heating reaction process, water generated in the reaction is discharged through a vacuum pump.
Preferably, the corrosion inhibitor composition comprises, in mass percent:
Figure BDA0002802321470000041
in a second aspect, the present application provides a method for preparing a corrosion inhibitor composition, comprising the steps of: and mixing isononanoic acid mixed amide, n-heptanoic acid triisopropanolamine soap, mixed azelaic acid amide, triethanolamine borate and benzotriazole to prepare the corrosion inhibitor composition.
In a third aspect, the application provides the use of the corrosion inhibitor composition in metal processing.
The prior corrosion inhibitor in the prior art has single function or poor effect.
The application aims to develop a corrosion inhibitor composition which has excellent aluminum-copper corrosion inhibition, rust prevention, lubrication, no bubbles and certain cleaning performance. The additive can be used in a cutting fluid system as an additive, and can also be directly diluted to be used as a cutting fluid, so that the metal cutting efficiency is greatly improved. The embodiment of the application shows that the corrosion inhibitor composition has multiple performances of no foam, non-ferrous metal corrosion inhibition, ferrous metal rust prevention, lubrication and the like, and the addition of triisopropanolamine n-heptanoate soap in the corrosion inhibitor composition improves the corrosion inhibition efficiency of LY12 aluminum by 20 times, thereby meeting the requirements of metal cutting technology in industry.
Compared with the prior art, the method has the following advantages:
1. the corrosion inhibitor composition has good corrosion inhibition effect on nonferrous metals, and still has good corrosion inhibition effect on the nonferrous metals at the concentration of 0.025 percent;
2. the corrosion inhibitor composition is free of bubbles, and can avoid negative effects caused by foams in the processing process;
3. the corrosion inhibitor composition can be used as a multifunctional corrosion inhibitor with no foam, corrosion inhibition, rust prevention and lubrication, can also be directly diluted by water to be used as a processing liquid, does not need to waste time and labor for combining a formula, and saves time cost and labor cost;
4. the corrosion inhibitor composition is green and environment-friendly, and does not contain components such as S, P, Cl and the like which are commonly used in a lubricant;
5. the preparation method of the corrosion inhibitor composition is simple and easy to obtain.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is an infrared spectrum of a mixed isononanoic acid amide provided in the examples herein;
FIG. 2 is a nuclear magnetic spectrum of isononanoic acid mixed amide provided in the examples herein;
FIG. 3 is an IR spectrum of triisopropanolamine n-heptanoate soap provided in examples herein;
FIG. 4 is a nuclear magnetic spectrum of triisopropanolamine n-heptanoate soap provided in examples of the present application;
FIG. 5 is a NMR spectrum of a mixed azelaic acid amide as provided in the examples herein;
FIG. 6 is an IR spectrum of a mixed azelaic acid amide as provided in the examples herein;
FIG. 7 is a comparative reference diagram of the judgment criteria for cast iron scrap provided in example 5 of the present application;
FIG. 8 is a graph showing the mean torque values provided in examples 1 to 3 of the present application and comparative examples 1 to 3.
Detailed Description
The application provides a corrosion inhibitor composition and a preparation method thereof, which are used for solving the technical defects that the corrosion inhibitor in the prior art has single performance and can not meet the requirements of the existing metal cutting fluid.
The technical solutions in the embodiments of the present application will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Wherein, the raw materials or reagents used in the following examples are all sold in the market or made by the user;
the preparation method of isononanoic acid mixed amide (isononanoic acid mixed amide comprises isononanoic acid diisopropanol amide and isononanoic acid diethanol amide) in the embodiment of the application comprises the following steps:
(1) putting 46 mass percent of isononanoic acid into a reaction kettle, and heating to 90 ℃ for later use;
(2) slowly putting 54% of alcohol amine mixture by mass into a reaction kettle containing isononanoic acid, wherein the alcohol amine mixture comprises diisopropanolamine and diethanolamine; the mass ratio of diisopropanolamine to diethanolamine is 4: 1;
(3) adding catalyst 18-crown ether-6 accounting for 0.15 mass percent of the sum of the mass of the isononanoic acid and the alcohol amine mixture into a reaction kettle, heating to 120 ℃, reacting for about 4 hours at the temperature, simultaneously starting a vacuum pump to discharge water generated in the reaction, and stopping heating until no water is distilled out.
(4) Naturally cooling to room temperature, discharging to obtain isononanoic acid mixed amide (isononanoic acid mixed amide comprises isononanoic acid diisopropanol amide and isononanoic acid diethanol amide).
Wherein the isononanoic acid diisopropanol amide has a structure shown in a formula I;
Figure BDA0002802321470000061
the isononanoic acid diethanolamide has a structure shown in a formula II;
Figure BDA0002802321470000071
the infrared spectrum and nuclear magnetic spectrum detection is carried out on the embodiment of the application, and the results are shown in fig. 1 and fig. 2; FIGS. 1-2 illustrate the success of the examples of the present application in producing diisopropanolamide isononanoate and diethanolamide isononanoate.
The preparation method of the triisopropanolamine n-heptanoate soap comprises the following steps:
(1) putting 21% n-heptanoic acid into a reaction kettle, and heating to 80 ℃ for later use;
(2) 79 percent of triisopropanolamine is slowly put into a reaction kettle to react for 3 hours at the temperature of 125 ℃,
(3) stopping heating, naturally cooling to room temperature, and discharging to obtain the triisopropanolamine n-heptanoate soap.
The triisopropanolamine n-heptanoate soap has a structural formula shown as a formula III:
Figure BDA0002802321470000072
the results of the infrared spectrogram and the nuclear magnetic resonance hydrogen spectrum detection of the triisopropanolamine n-heptanoate prepared in the embodiment of the present application are shown in fig. 3 to 4, and fig. 3 to 4 illustrate that the triisopropanolamine n-heptanoate prepared in the embodiment of the present application is successfully prepared.
The preparation method of the mixed azelaic acid amide (the mixed azelaic acid amide comprises azelaic acid diiso-propanol amide, azelaic acid diethanol amide and azelaic acid mixed alcohol amide) in the embodiment of the application comprises the following steps:
(1) slowly adding 45% of alcohol amine mixture by mass into a reaction kettle, and heating to 80 ℃ for later use; wherein the alcohol amine mixture comprises diisopropanolamine and diethanolamine; the mass ratio of diisopropanolamine to diethanolamine is 5: 1.
(2) Then, azelaic acid with the mass percent of 55% is put into a reaction kettle containing alcohol amine mixture.
(3) Putting catalyst 18-crown ether-6 into a reaction kettle containing alcohol amine mixture and azelaic acid, heating to 120 ℃, reacting for about 4 hours at the temperature, simultaneously starting a vacuum pump to discharge water generated in the reaction, and stopping heating when no water is distilled; wherein, the addition amount of the 18-crown ether-6 is 0.2 percent of the sum of the mass of the alcohol amine mixture and the mass of the azelaic acid.
(4) Naturally cooling to room temperature, and discharging to obtain mixed azelaic acid amide (the mixed azelaic acid amide comprises diisopropanol amide of azelaic acid, diethanol amide of azelaic acid and mixed alcohol amide of azelaic acid).
Wherein the azelaic acid diisopropanol amide has formula IV;
Figure BDA0002802321470000081
azelaic acid diethanolamide has formula V;
Figure BDA0002802321470000082
the azelaic acid mixed alcohol amide has formula VI;
Figure BDA0002802321470000083
the results of nuclear magnetic spectrum and infrared spectrum analysis of the mixed azelaic acid amide (the mixed azelaic acid amide comprises azelaic acid diiso-propanol amide, azelaic acid diethanol amide and azelaic acid mixed alcohol amide) in the examples of the application are shown in fig. 5-6, and fig. 5-6 demonstrate that the products in the examples of the application comprise azelaic acid diiso-propanol amide, azelaic acid diethanol amide and azelaic acid mixed alcohol amide.
Comparative example 3, used in the following examples, is a commercially available sodium silicate of a conventional corrosion inhibitor.
Example 1
The embodiment of the application provides a first corrosion inhibitor composition, and the preparation method comprises the following steps:
according to the total mass of the multifunctional corrosion inhibitor, 40% by mass of isononanoic acid mixed amide, 25% by mass of n-heptanoic acid triisopropanolamine soap, 30% by mass of mixed azelaic acid amide, 4.5% by mass of triethanolamine borate and 0.5% by mass of benzotriazole are sequentially added, and the mixture is fully stirred by a stirrer until the mixture is uniformly mixed, and the mark is embodiment 1.
Example 2
The embodiment of the application provides a second corrosion inhibitor composition, and the preparation method comprises the following steps:
according to the total mass of the multifunctional corrosion inhibitor, 43 percent by mass of isononanoic acid mixed amide, 23 percent by mass of n-heptanoic acid triisopropanolamine soap, 27 percent by mass of mixed azelaic acid amide, 6.5 percent by mass of triethanolamine borate and 0.5 percent by mass of benzotriazole are sequentially added, and the mixture is fully stirred by a stirrer until the mixture is uniformly mixed, and the mark is embodiment 2.
Example 3
The embodiment of the application provides a third corrosion inhibitor composition, and the preparation method comprises the following steps:
according to the total mass of the multifunctional corrosion inhibitor, 38 percent by mass of isononanoic acid mixed amide, 32 percent by mass of n-heptanoic acid triisopropanolamine soap, 23 percent by mass of mixed azelaic acid amide, 6.5 percent by mass of triethanolamine borate and 0.5 percent by mass of benzotriazole are sequentially added, and the mixture is fully stirred by a stirrer until the mixture is uniformly mixed, and the mark is embodiment 3.
Comparative example 1
The comparative example of the present application provides a first control product, without the addition of triisopropanolamine n-heptanoate soap, prepared by a process comprising:
according to the total mass of the multifunctional corrosion inhibitor, 50 percent by mass of isononanoic acid mixed amide, 38 percent by mass of mixed azelaic acid amide, 11 percent by mass of triethanolamine borate and 1 percent by mass of benzotriazole are sequentially added, fully stirred by a stirrer until the mixture is uniformly mixed, and marked as comparative example 1.
Comparative example 2
The comparative example of the present application provides a second control product, with the addition of a small amount of triisopropanolamine n-heptanoate soap, prepared by a process comprising:
according to the total mass of the multifunctional corrosion inhibitor, 50% by mass of isononanoic acid mixed amide, 5% by mass of n-heptanoic acid triisopropanolamine soap, 35% by mass of mixed azelaic acid amide, 9% by mass of triethanolamine borate and 1% by mass of benzotriazole are sequentially added, and the mixture is fully stirred by a stirrer until the mixture is uniformly mixed, and the mark is a comparative example 2.
Example 4
The embodiment of the application provides the corrosion, rust prevention and copper corrosion inhibition tests of the embodiments 1-3 and the comparative examples 1-3, and the specific steps are as follows:
the rust and corrosion inhibiting properties of cast iron, LY12 aluminum, red copper and brass H62 of examples 1, 2, 3, 1, 2 and 3 (conventional corrosion inhibitor sodium silicate) were tested with reference to the corrosion test method in GB6144-2010 synthetic cutting fluid.
1. Preparing a working solution: example 1, example 2, example 3, comparative example 1, comparative example 2 and comparative example 3 were respectively configured as working fluids corresponding to concentrations of 0.025%, 0.05%, 0.1% and 0.5%, wherein the working fluids had solutes of example 1, example 2, example 3, comparative example 1, comparative example 2 and comparative example 3 (sodium silicate, a conventional corrosion inhibitor) and had tap water as a solvent; the blank comparative example was tap water.
2. Setting the thermostat to 55 ℃, and preheating;
3. taking out the metal test piece, and then washing the rust-proof oil with absolute ethyl alcohol;
4. after the metal test piece is dried, polishing the surface by 400-mesh sand paper to ensure that the surface has no pits, scratches or rusts;
5. cleaning the ground metal test piece with absorbent cotton in absolute ethyl alcohol, and wiping the test piece with filter paper;
6. putting the wiped metal test pieces into 50ml beakers respectively, and requiring the working solution in the step 1 to immerse the metal test pieces;
7. covering the culture dish, putting the beaker into a thermostat which is kept at the constant temperature of 55 +/-2 ℃, and recording the time for starting corrosion;
8. continuously standing for 8h, taking out the metal test piece, and comparing the metal test piece with the metal test piece before the test;
9. and (4) judging the standard:
TABLE 1 Corrosion criteria for cast iron, LY12 aluminum, copper and brass
No rust and luster like new Class A
Slight discoloration Class B
Moderate color change Class C
Severe discoloration Class D
In table 1, the cast iron sheet is qualified when reaching the A grade, and LY12 aluminum, red copper and brass H62 are qualified when reaching the A or B grade.
10. The test results are shown in table 2.
TABLE 2 Corrosion test results for cast iron, LY12 aluminum, red copper, brass H62
Figure BDA0002802321470000111
11. Conclusion of the experiment
The blank comparative example has excellent corrosion inhibition effect on LY12 aluminum, red copper, brass H62 and brass H70 under the condition that cast iron sheets, LY12 aluminum, red copper and brass H62 are corroded by 0.5% concentration of (conventional corrosion inhibitor sodium silicate) aqueous solutions of examples 1, 2, 3, 1, 2 and 3, wherein the corrosion inhibition effect of examples 1, 2 and 3 is better and can reach grade A of corrosion test. The level of triisopropanolamine n-heptanoate soap component of comparative examples 1 and 2 is outside the range of the corrosion inhibitor composition of the present application, and the corrosion inhibition effect is significantly inferior to that of examples 1, 2 and 3.
From comparative example 1, comparative example 2, example 1, example 2 and example 3, it was found that triisopropanolamine n-heptanoate soap plays a decisive role in the corrosion inhibition of nonferrous metals in the corrosion inhibitor composition of the present application, that triisopropanolamine n-heptanoate soap is not added in comparative example 1, that the triisopropanolamine n-heptanoate soap component content in comparative example 2 is out of the range of the present application, and that the minimum concentration of corrosion inhibition is 0.5%, but that the corrosion inhibition effect of comparative example 2 on nonferrous metals is slightly better than that of comparative example 1 due to the addition of a small amount of triisopropanolamine n-heptanoate soap. Examples 1, 2 and 3, in which triisopropanolamine n-heptanoate soap was added and the component contents were within the range of the present application, the minimum corrosion inhibition concentration of LY12 aluminum, red copper and brass H62 was reduced from 0.5% to 0.025%, and the corrosion inhibition rate was increased by 20 times. Compared with the comparative example 3 (the conventional corrosion inhibitor sodium silicate), the corrosion inhibitor has stronger comprehensive performance and wider application range.
Example 5
The embodiment of the application provides the rust-proof tests of the embodiments 1-3 and the comparative examples 1-3, and the specific steps are as follows:
1. preparing a working solution: respectively configuring example 1, example 2, example 3, comparative example 1, comparative example 2 and comparative example 3 (sodium silicate of a conventional corrosion inhibitor) into 1 percent of corresponding working solutions, wherein the solute in the working solutions is example 1, example 2, example 3, comparative example 1, comparative example 2 and comparative example 3 (sodium silicate of a conventional corrosion inhibitor), and the solvent is tap water; the blank comparative example was tap water.
2. The test steps are as follows: putting filter paper into a culture dish, weighing 2g +/-0.1 g of GG25 cast iron chips, spreading the GG25 cast iron chips on the filter paper, transferring 2ml of liquid to be detected by a dropper to wet all the cast iron chips, covering the culture dish, naturally placing for 2 hours at 18-28 ℃, washing off the cast iron chips on the filter paper by tap water, soaking the filter paper in acetone liquid for 5 seconds, and naturally drying at room temperature (18-28 ℃), wherein the evaluation standard of the cast iron chips is shown in Table 3. The test result is evaluated according to the number of rusty spots on the filter paper according to a grade of 0-4;
TABLE 32 h cast iron scrap evaluation criteria
Figure BDA0002802321470000131
3. The test results are shown in Table 4.
TABLE 42 h test results for cast iron filings
Name (R) Example 1 Example 2 Example 3 Comparative example 1 Comparative example 2 Comparative example 3 Blank comparative example
Grade of rust Level 0 Level 0 0 to 1 stage Level 0 Level 0 Stage 2 4 stage
4. Conclusion of the experiment
The results of the 2h tap water cast iron filings test show that examples 1, 2 and 3 all have excellent rust inhibitive properties. The content of triisopropanolamine n-heptanoate soap components in comparative example 1 and comparative example 2 is out of the range of the present application, and the rust inhibitive performance against iron filings is equivalent to that of example 1 and example 2, and slightly superior to that of example 3. The tri-isopropanolamine n-heptanoate soap has little influence on the rust prevention performance of the application. The rust inhibitive performance of comparative example 3 (sodium silicate, a conventional corrosion inhibitor) is also inferior to that of example 1, example 2 and example 3 of the present application.
Example 6
The embodiment of the application provides tapping torque test tests of embodiments 1-3 and comparative examples 1-3, and the tapping torque test method comprises the following specific steps:
a metal material provided with a prepared hole was directly subjected to a tapping test using a simulation tester, and the lubricating property of the machining was evaluated using an average torque value. Theoretically, the lower the tapping torque value, the better the lubricity. Tapping tests were performed on 1% working fluids of example 1, example 2, comparative example 1, comparative example 2, and comparative example 3 (sodium silicate, a conventional corrosion inhibitor), respectively. The test parameters were as follows: rotating speed: 1200 rpm; tapping depth: 12 mm; torsion: 400 Ncm; the tap type: m4 press tap; testing block material quality: 7075 and (3) aluminum. The average torque values are shown in table 5 and the tapping torque profile is shown in fig. 8.
TABLE 5 mean Torque values
Figure BDA0002802321470000132
Figure BDA0002802321470000141
As can be seen from the tapping torque test results, the average torque values of example 1, example 2 and example 3 were low at 128.8N/cm, 133.2N/cm and 131.5N/cm, respectively, followed by comparative example 1 and comparative example 2 at 146.4N/cm and 140.3N/cm, respectively, and the content of triisopropanolamine N-heptanoate soap component of comparative example 1 and comparative example 2 was out of the range of the present application, and the average tapping torque values thereof were respectively 13.7% and 9.0% higher than that of example 1, and the average tapping torque value of comparative example 3 (conventional corrosion inhibitor) was the largest at 228.2N/cm, higher than that of example 177.2, and example 1 and example 2 had the optimum lubricity.
Example 7
The examples of the present application provide the foaming tests of examples 1, 2 and 3, with the specific steps as follows:
examples 1, 2 and 3 were tested for foaming power according to the test method of GB/T7462-94 "determination of foaming power of surfactants improves foaming power in the Ross-Miles method".
1. Preparing a working solution: the preparation method comprises the steps of respectively preparing 0.25% of working solutions of example 1, example 2 and example 3, wherein solutes in the working solutions are example 1, example 2 and example 3, and solvents in the working solutions are all water;
2. a thermostatic water bath with a circulating water pump, wherein the temperature of the working solution of the embodiment 1, the working solution of the embodiment 2 and the working solution of the embodiment 3 is controlled at 50 +/-0.5 ℃;
3. cleaning an instrument: washing with water, and rinsing with a small amount of solution to be detected;
4. filling part of the solution to be detected in the step 2 into a separating funnel to a 150mm scale;
5. filling part of the solution to be detected in the step 2 into a measuring cylinder to 50ml of scale;
6. measuring 500ml of liquid to be tested which is kept at 50 +/-0.5 ℃ and pouring the liquid to be tested into a separating funnel, and slowly performing the operation to avoid generating foams, wherein the liquid to be tested is 0.25% of the working solution of the embodiment 1, the embodiment 2 and the embodiment 3 respectively;
7. the liquid in the separating funnel continuously flows down until the liquid level drops to the 150mm scale;
8. the results are expressed as the number of milliliters of foam formed (foam volume) at 30s, 3min, 5min, 8min, 10min, 12min and 15min after the liquid flow had stopped.
9. The test results are shown in table 4.
TABLE 4 foam height at different times
Figure BDA0002802321470000151
Compared with the corrosion inhibition, lubricity, rust prevention and foaming performance of LY12 aluminum, red copper and brass H62, the corrosion inhibitor composition disclosed by the application has excellent lubricity, aluminum corrosion inhibition and rust prevention performance, is free of bubbles, and has a wider development prospect and application range compared with the conventional aluminum corrosion inhibitors on the market.
The foregoing is only a preferred embodiment of the present application and it should be noted that those skilled in the art can make several improvements and modifications without departing from the principle of the present application, and these improvements and modifications should also be considered as the protection scope of the present application.

Claims (10)

1. The corrosion inhibitor composition is characterized by comprising isononanoic acid mixed amide, n-heptanoic acid triisopropanolamine soap, mixed azelaic acid amide, triethanolamine borate and benzotriazole;
the corrosion inhibitor composition comprises the following components in percentage by mass:
Figure FDA0003575598940000011
the isononanoic acid mixed amide comprises isononanoic acid diisopropanol amide and isononanoic acid diethanol amide;
the obtained diisopropanolamide isononanoate has a structure shown in a formula I;
Figure FDA0003575598940000012
the isononanoic acid diethanolamide has a structure shown in a formula II;
Figure FDA0003575598940000013
the triisopropanolamine n-heptanoate soap has a structure of formula III:
Figure FDA0003575598940000014
the mixed azelaic acid amide comprises azelaic acid diiso-propanol amide, azelaic acid diethanol amide and azelaic acid mixed alcohol amide;
the azelaic acid diisopropanol amide has formula IV;
Figure FDA0003575598940000021
the azelaic acid diethanolamide has formula V;
Figure FDA0003575598940000022
the azelaic acid mixed alcohol amide has formula VI;
Figure FDA0003575598940000023
2. the corrosion inhibitor composition according to claim 1, wherein the mass ratio of the diisopropanolamine isononanoate to the diethanolamide isononanoate in the mixed amide isononanoate is (3-6): 1.
3. corrosion inhibitor composition according to claim 1, characterized in that the isononanoic acid mixed amide is prepared by a process comprising the following steps:
mixing isononanoic acid, an alcohol amine mixture and a catalyst for reaction to prepare isononanoic acid mixed amide; wherein the alcohol amine mixture comprises diisopropanolamine and diethanolamine;
calculated according to the mass percentage, the method comprises the following steps:
24% -39% of isononanoic acid;
61% -76% of the alcohol amine mixture;
the mass ratio of the diisopropanolamine to the diethanolamine is (4-7): 1;
the addition amount of the catalyst is 0.1-0.2% of the sum of the mass of the isononanoic acid and the mass of the alcohol amine mixture.
4. Corrosion inhibitor composition according to claim 3, characterized in that in the process for the preparation of the isononanoic acid mixed amide the catalyst is selected from 18-crown-6 or/and 15-crown-5;
the temperature of the mixing reaction is 110-125 ℃; the mixing reaction time is 4-5 h.
5. The corrosion inhibitor composition of claim 1 wherein said n-heptanoic acid triisopropanolamine is prepared by a process comprising the steps of:
heating n-heptanoic acid and triisopropanolamine to react to prepare triisopropanolamine n-heptanoic acid soap;
wherein, calculated according to the mass percentage, the method comprises the following steps:
18 to 25 percent of n-heptanoic acid;
75 to 82 percent of triisopropanolamine.
6. The corrosion inhibitor composition as claimed in claim 5, wherein in the preparation method of triisopropanolamine n-heptanoate, the temperature of the heating reaction is 110 ℃ to 130 ℃; the heating reaction time is 2-4 h.
7. Corrosion inhibitor composition according to claim 1, characterized in that in the mixed azelaic acid amide, the mass percentages of the azelaic acid diiso-propanol amide, the azelaic acid diethanol amide and the azelaic acid mixed alcohol amide are (65% to 75%): (13-15%): (12% to 20%).
8. Corrosion inhibitor composition according to claim 1, characterized in that the process for the preparation of the mixed azelaic acid amide comprises the following steps: mixing the alcohol amine mixture, azelaic acid and a catalyst, and heating for reaction to obtain mixed azelaic acid amide;
wherein the alcohol amine mixture comprises diisopropanolamine and diethanolamine;
wherein, calculated according to the mass percentage, the method comprises the following steps:
67% -78% of alcohol amine mixture;
22 to 33 percent of azelaic acid;
the mass ratio of the diisopropanolamine to the diethanolamine is (5-8) to 1; the addition amount of the catalyst is 0.1-0.2% of the sum of the mass of the alcohol amine mixture and the mass of the azelaic acid.
9. Corrosion inhibitor composition according to claim 8, characterized in that in the process for the preparation of the mixed azelaic acid amide the catalyst is selected from the group consisting of 18-crown-6 or/and 15-crown-5; the temperature of the heating reaction is 110-125 ℃; the heating reaction time is 4-5 h.
10. A method for preparing a corrosion inhibitor composition according to any one of claims 1 to 9, characterized in that it comprises the following steps: and mixing isononanoic acid mixed amide, n-heptanoic acid triisopropanolamine soap, mixed azelaic acid amide, triethanolamine borate and benzotriazole to prepare the corrosion inhibitor composition.
CN202011354867.9A 2020-11-27 2020-11-27 Corrosion inhibitor composition and preparation method thereof Active CN112442408B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011354867.9A CN112442408B (en) 2020-11-27 2020-11-27 Corrosion inhibitor composition and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011354867.9A CN112442408B (en) 2020-11-27 2020-11-27 Corrosion inhibitor composition and preparation method thereof

Publications (2)

Publication Number Publication Date
CN112442408A CN112442408A (en) 2021-03-05
CN112442408B true CN112442408B (en) 2022-05-17

Family

ID=74737745

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011354867.9A Active CN112442408B (en) 2020-11-27 2020-11-27 Corrosion inhibitor composition and preparation method thereof

Country Status (1)

Country Link
CN (1) CN112442408B (en)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB989009A (en) * 1961-01-23 1965-04-14 Prod Chim Et De Synthese Soc D Improvements in and relating to ester-amides
CN1459493A (en) * 2002-05-22 2003-12-03 赵刚 Long acting green cutting fluid and its preparation method
CN101130873A (en) * 2006-08-23 2008-02-27 冯为民 Water-based antirust preparation technique
CN101161797A (en) * 2007-09-28 2008-04-16 北京东兴润滑剂有限公司 Water-soluble discharging medium compound for electrospark wire-electrode cutting
JP2008248229A (en) * 2007-03-08 2008-10-16 Nippon Steel Corp Temper rolling liquid and undiluted solution for temper rolling liquid
CN111117754A (en) * 2019-12-30 2020-05-08 深圳金泽万长石化有限公司 High-lubrication stable cutting fluid and preparation method thereof
CN111206250A (en) * 2020-01-20 2020-05-29 青岛科技大学 Mixed amide type water-based gas-phase antirust concentrated solution and preparation and use methods thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2795432B1 (en) * 1999-06-28 2001-08-24 Atofina CORROSION INHIBITOR COMPOSITIONS FOR HEAT TRANSFER FLUIDS

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB989009A (en) * 1961-01-23 1965-04-14 Prod Chim Et De Synthese Soc D Improvements in and relating to ester-amides
CN1459493A (en) * 2002-05-22 2003-12-03 赵刚 Long acting green cutting fluid and its preparation method
CN101130873A (en) * 2006-08-23 2008-02-27 冯为民 Water-based antirust preparation technique
JP2008248229A (en) * 2007-03-08 2008-10-16 Nippon Steel Corp Temper rolling liquid and undiluted solution for temper rolling liquid
CN101161797A (en) * 2007-09-28 2008-04-16 北京东兴润滑剂有限公司 Water-soluble discharging medium compound for electrospark wire-electrode cutting
CN111117754A (en) * 2019-12-30 2020-05-08 深圳金泽万长石化有限公司 High-lubrication stable cutting fluid and preparation method thereof
CN111206250A (en) * 2020-01-20 2020-05-29 青岛科技大学 Mixed amide type water-based gas-phase antirust concentrated solution and preparation and use methods thereof

Also Published As

Publication number Publication date
CN112442408A (en) 2021-03-05

Similar Documents

Publication Publication Date Title
CN101270478A (en) Metal cleaning agent
CN111961522A (en) Universal micro-emulsion cutting fluid for aluminum material processing, and preparation method and application thereof
CN111662773A (en) Long-acting total-synthesis magnesium alloy cutting fluid and processing method
CN104004579B (en) Machining center rust coolant liquid
WO2023071898A1 (en) Long-acting corrosion-inhibition aluminum alloy cutting fluid
CN106590907A (en) Graphene-containing metal cutting fluid and preparation method thereof
CN112745983A (en) Phosphorus-free alkaline water-based spray cleaning antirust agent and preparation method thereof
CN111961541A (en) Environment-friendly metal surface cleaning agent and preparation method thereof
CN103555410B (en) Water-based antirust grinding cooling liquid for automobile connecting rod as well as preparation method and application of water-based antirust grinding cooling liquid
CN112442408B (en) Corrosion inhibitor composition and preparation method thereof
CN108374175B (en) Metal polishing paste and preparation method and application thereof
CN104830492B (en) Cutting fluid
CN112481009B (en) Microemulsion cutting fluid for copper-aluminum-iron material processing and preparation method thereof
CN112626531B (en) Surfactant and application thereof
CN115161648B (en) Ultrahigh-pressure aluminum part cleaning agent and preparation method and application thereof
CN108441310A (en) A kind of intermetallic composite coating semi-synthetic cutting fluid and preparation method thereof
CN112480991B (en) Lubricant as well as preparation method and application thereof
CN107740109A (en) A kind of tumbling cleaning agent and preparation method thereof
CN107164052A (en) A kind of preparation method of the aqueous micro-emulsion cutting fluid of organic amine
CN105754700A (en) Environment-friendly micro-emulsified cooling liquid and preparation method
CN112126936A (en) Efficient surface cleaning agent for die-casting aluminum and magnesium alloy and preparation method thereof
CN112479907B (en) Triisopropanolamine soap n-heptanoic acid, preparation method and application thereof, and metal cleaning agent
CN112501618A (en) Antirust agent and preparation method and application thereof
CN1225939A (en) Water-base metal coolant
CN112708498B (en) Stainless steel aqueous cutting fluid and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant