阅读说明：本技术 一种防锈剂及其制备方法和应用 (Antirust agent and preparation method and application thereof ) 是由 何锦凤 何锦梅 何彦波 于 2020-11-27 设计创作，主要内容包括：本申请属于金属加工的技术领域,尤其涉及一种防锈剂及其制备方法和应用。本申请第一方面提供了一种防锈剂,包括壬二酸二异丙醇酰胺、壬二酸二乙醇酰胺和壬二酸混合醇酰胺；所述壬二酸二异丙醇酰胺具有式Ⅰ；所述壬二酸二异丙醇酰胺具有式Ⅱ；所述壬二酸混合醇酰胺具有式Ⅲ。本申请第二方面提供了所述防锈剂的制备方法,包括以下步骤：将醇胺混合物、壬二酸和催化剂混合,加热反应,得到防锈剂；其中,所述醇胺混合物包括二异丙醇胺和二乙醇胺。本申请提供了一种防锈剂及其制备方法和应用,能有效解决现有的防锈剂存在的防锈性能较差的技术问题。(The application belongs to the technical field of metal processing, and particularly relates to an antirust agent and a preparation method and application thereof. The first aspect of the application provides a rust inhibitor, which comprises azelaic acid diisopropanol amide, azelaic acid diethanol amide and azelaic acid mixed alcohol amide; the azelaic acid diisopropanol amide has formula I; the azelaic acid diisopropanol amide has formula II; the azelaic acid mixed olamide has formula iii. The second aspect of the application provides a preparation method of the antirust agent, which comprises the following steps: mixing the alcohol amine mixture, azelaic acid and a catalyst, and heating for reaction to obtain the antirust agent; wherein the alcohol amine mixture comprises diisopropanolamine and diethanolamine. The application provides an antirust agent, a preparation method and application thereof, which can effectively solve the technical problem of poor antirust performance of the existing antirust agent.)

1. A rust inhibitor is characterized by comprising azelaic acid diisopropanol amide, azelaic acid diethanol amide and azelaic acid mixed alcohol amide;

the azelaic acid diisopropanol amide has formula I;

the azelaic acid diethanolamide has a formula II;

the azelaic acid mixed alcohol amide has formula III;

2. a method for producing the rust inhibitor according to claim 1, characterized by comprising the steps of: mixing the alcohol amine mixture, azelaic acid and a catalyst, and heating for reaction to obtain the antirust agent;

wherein the alcohol amine mixture comprises diisopropanolamine and diethanolamine.

3. The preparation method according to claim 2, comprising the following steps of:

67% -78% of alcohol amine mixture;

azelaic acid 22% -33%;

the mass ratio of the diisopropanolamine to the diethanolamine is (5-8) to 1.

4. The process according to claim 2, wherein the catalyst is selected from 18-crown-6 and/or 15-crown-5.

5. The method according to claim 2, wherein the amount of the catalyst added is 0.1-0.2% of the sum of the masses of the alcohol amine mixture and the azelaic acid.

6. The method according to claim 2, wherein the temperature of the heating reaction is 110 ℃ to 125 ℃; the heating reaction time is 4-5 h.

7. The method according to claim 2, characterized in that the alcohol amine mixture is preheated to 80-90 ℃.

8. The method of claim 2, wherein the heating further comprises discharging water produced by the reaction and stopping the heating until no more water is distilled.

9. The method according to claim 8, wherein the reaction process is heated, and water produced by the reaction is discharged by a vacuum pump.

10. Use of the rust inhibitor of claim 1 or the rust inhibitor produced by the production method of any one of claims 2 to 9 in metal working.

Technical Field

The application belongs to the technical field of metal processing, and particularly relates to an antirust agent and a preparation method and application thereof.

Background

The water-based antirust agent is an antirust agent which can be diluted by water in the using process, and in the metal processing process, the antirust agent is added, so that not only can the workpiece not be corroded in the working procedure, but also the equipment such as a machine tool, a cutter and the like which is contacted with the workpiece in the processing process can not be corroded. Early water-based rust inhibitors mostly contained an alkaline aqueous solution of nitrite, chromate or phosphate, and were widely used because of their advantages of low cost, convenient use, and easy removal. However, the rust inhibitor has strong toxicity, causes environmental pollution or causes eutrophication when discharged into water, and also forms a layer of white frost on the surface of the metal, thereby influencing the normal operation of the next process.

In recent years, with the development of corrosion inhibition technology and the improvement of environmental awareness, water-soluble rust inhibitors are mainly developed towards organic rust inhibitors, and common rust inhibitors include fatty acid soaps, carboxylic acids, esters, amides, phosphate esters and the like. These rust inhibitors can adsorb on the metal surface by physical and chemical actions, thereby changing the state of the metal surface and playing a role of rust prevention.

However, the existing antirust agent has the problems of insufficient antirust, the requirements on workpieces which are easy to rust or working procedures with long antirust time are often not met, the addition amount of the antirust agent needs to be increased, the production cost is high, other performances of the system are inhibited, and the like.

Disclosure of Invention

In view of the above, the application provides an antirust agent, a preparation method and an application thereof, which can effectively solve the technical problem of poor antirust performance of the existing antirust agent.

The first aspect of the application provides a rust inhibitor, which comprises azelaic acid diisopropanol amide, azelaic acid diethanol amide and azelaic acid mixed alcohol amide;

the azelaic acid diisopropanol amide has formula I;

the azelaic acid diethanolamide has a formula II;

the azelaic acid mixed alcohol amide has formula III;

the second aspect of the application provides a preparation method of the antirust agent, which comprises the following steps: mixing the alcohol amine mixture, azelaic acid and a catalyst, and heating for reaction to obtain the antirust agent;

wherein the alcohol amine mixture comprises diisopropanolamine and diethanolamine.

Preferably, the method comprises the following steps of:

67% -78% of alcohol amine mixture;

azelaic acid 22% -33%;

the mass ratio of the diisopropanolamine to the diethanolamine is (5-8) to 1.

Preferably, the catalyst is selected from 18-crown-6 or/and 15-crown-5.

Preferably, 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, the temperature of the heating reaction is 110-125 ℃; the heating reaction time is 4-5 h.

Preferably, the alcohol amine mixture is preheated to 80-90 ℃.

Preferably, the heating reaction process further comprises discharging water produced by the reaction, and stopping heating until no more water is distilled.

Preferably, the reaction process is heated, and water generated by the reaction is discharged by a vacuum pump.

The third aspect of the application provides the application of the antirust agent or the antirust agent prepared by the preparation method in metal processing.

The water-based antirust agent in the prior art contains more toxic components, and the antirust performance of the water-based antirust agent without toxic components is not ideal, so that the application aims to invent the environment-friendly water-based antirust agent which does not contain toxic components, can completely reach the antirust level of a nitrite water-based antirust agent product on ferrous metals and has excellent antirust performance, and solve the problem that the existing antirust agent cannot be environment-friendly and antirust.

According to the application, an amide mixture with a proper carbon chain length and structure is selected to react with azelaic acid, so that the mixed amide which does not contain toxic components such as sodium sulfite and the like and has more excellent antirust performance and foamless performance is obtained, and the mixed amide comprises azelaic acid diisopropanol amide, azelaic acid diethanol amide and azelaic acid mixed alcohol amide.

Compared with the prior art, the antirust agent has the following advantages:

1. the preparation method of the antirust agent is simple, easy to operate, relatively low in production cost and more beneficial to industrialization.

2. The antirust agent does not contain toxic components such as sodium sulfite and the like, and is healthy and environment-friendly.

3. The antirust agent has good antirust property, can be suitable for scenes with high antirust requirements in practical application, reduces the using amount of the antirust agent, and saves the production cost.

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 a nuclear magnetic spectrum of a rust inhibitor provided in an example of the present application;

FIG. 2 is an IR spectrum of a rust inhibitor provided in an example of the present application;

fig. 3 is a comparative reference diagram of the judgment criteria for cast iron scrap provided in example 2 of the present application.

Detailed Description

The application provides an antirust agent, a preparation method and an application thereof, which are used for solving the technical defect of poor antirust performance of the antirust agent in the prior art.

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.

The raw materials and reagents used in the following examples are commercially available or self-made.

Example 1

The embodiment of the application provides a preparation method of an antirust agent, which specifically 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, discharging and preparing the antirust agent which is marked as example 1.

The results of nuclear magnetic spectrum and infrared spectrum analysis of the antirust agent in the embodiment of the application are shown in fig. 1-2, and fig. 1-2 illustrate that the antirust agent in the embodiment of the application comprises azelaic acid diisopropanolamine, azelaic acid diethanolamide and azelaic acid mixed alcohol amide.

Example 2

The embodiment of the application is to carry out the rust-proof test on the rust inhibitor, the triethanolamine borate rust inhibitor and the sodium nitrite rust inhibitor in the embodiment 1, and the specific steps are as follows:

1. preparing a working solution: respectively configuring example 1, comparative example 1 (triethanolamine borate) and comparative example 2 (sodium nitrite) into working solutions with different concentrations of 0.2%, 0.35%, 0.5%, 0.8% and 1%, wherein the solute in the working solutions is example 1, comparative example 1 and comparative example 2, 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 1. The test result is evaluated according to the number of rusty spots on the filter paper according to a grade of 0-4;

TABLE 12 h criterion for cast iron filings

3. The test results are shown in Table 2.

TABLE 22 h cast iron scrap test results

4. And (4) test conclusion:

the results of the 2h tap water cast iron filing test show that example 1 has excellent rust inhibitive properties. The rust inhibitive performance of comparative example 1 and comparative example 2 was also inferior to that of example 1 of the present invention. The mixed alcohol amine is selected to react with the azelaic acid, and the synthesized mixed amide has excellent antirust property.

Example 3

In the embodiment of the application, the foaming test is performed on the antirust agent, triethanolamine borate, oleic acid diethanolamide and tall oil acid diethanolamide in the embodiment 1, and the specific steps are as follows:

the foaming power of example 1, comparative example 1 (triethanolamine borate), comparative example 2 (oleic acid diethanolamide) and comparative example 3 (tall oil acid diethanolamide) was tested according to the test method of GB/T7462-94 "determination of foaming power of surfactant improves foaming power in Ross-Miles method".

1. Preparing a working solution: example 1, comparative example 1 (triethanolamine borate), comparative example 2 (oleic acid diethanolamide) and comparative example 3 (tall oil acid diethanolamide) were respectively prepared into 0.25% of working solutions, wherein the solute in the working solutions is example 1, comparative example 1 (triethanolamine borate), comparative example 2 (oleic acid diethanolamide) and comparative example 3 (tall oil acid diethanolamide), and the solvent is tap water;

2. a constant-temperature water bath with a circulating water pump, wherein the temperature of the example 1, the comparative example 2 and the comparative example 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 liquid to be detected into a separating funnel to a 150mm scale;

5. filling part of liquid to be detected into a measuring cylinder to 50ml of scale;

6. measuring 500ml of liquid to be detected which is 0.25 percent of working solution of example 1, comparative example 1 (triethanolamine borate), comparative example 2 (oleic acid diethanolamide) and comparative example 3 (tall oil acid diethanolamide) and is kept at 50 +/-0.5 ℃ and pouring the liquid to be detected into a separating funnel, and slowly performing the operation to avoid generating foams;

7. the liquid in the separating funnel continuously flows down until the liquid level drops to the 150mm scale;

8. the results are expressed in milliliters of foam formed (foam volume) at 30s, 3min, 5min, 8min, 10min, 12min and 15min after the flow had stopped.

9. The test results are shown in table 3.

TABLE 3

As can be seen from Table 3, the initial foam volumes of comparative example 2 and comparative example 3 were 290ml and 240ml, respectively, and the foam remaining after 15min was 70ml and 50ml, respectively, and it can be seen that the foams of comparative example 2 and comparative example 3 were abundant and difficult to eliminate. Example 1 the initial foam volume and the foam residual volume at 15min were both 0ml, and it can be seen that example 1 meets the requirement of no foam.

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.