Method for comparing capacities of different types of zeolite molecular sieves for adsorbing acidic substances in phosphate fire-resistant oil

Abstract

The invention relates to the field of phosphate fire-resistant oil detection, and particularly discloses a method for comparing the capacity of different types of zeolite molecular sieves for adsorbing acidic substances in phosphate fire-resistant oil. The test method comprises the following steps: S1, determining the acid value of the phosphate fire-resistant oil; s2, cleaning and drying the zeolite molecular sieve; s3, uniformly mixing the zeolite molecular sieve and the phosphate fire-resistant oil to obtain a mixture; s4, sealing and storing the mixture in a constant-temperature drying box; s5, sampling and detecting the acid value of the phosphate fire-resistant oil at set intervals, and recording; s6, drawing a measured acid value-time curve of the phosphate fire-resistant oil; the experimental operation is simple, the period is short, and the method is suitable for comparing the capabilities of different types of zeolite molecular sieves for adsorbing acidic substances in phosphate fire-resistant oil.

Description

Technical Field

[0001] The present application relates to the field of phosphate ester fire-resistant oil detection, and more specifically, to a method for comparing the ability of different types of zeolite molecular sieves to adsorb acidic substances in phosphate ester fire-resistant oil. Background Art

[0002] Phosphate ester fire-resistant oils are transparent, uniform, and free of sediment. They also have low volatility and stable physical properties, making them commonly used in hydraulic control systems in power plants. However, a major operational issue with phosphate ester fire-resistant oils is rapid acidity increase, leading to aging. This elevated acidity further degrades oil quality, shortening service life and significantly impacting performance. Therefore, phosphate ester fire-resistant oils require filtration to remove acidic substances.

[0003] Zeolite molecular sieves are widely used to adsorb acidic and alkaline substances, including those in phosphate ester fire-resistant fuels. However, there is currently no test method to compare the ability of different types of zeolite molecular sieves to adsorb acidic substances in phosphate ester fire-resistant fuels. Based on this, the present application is proposed. Summary of the Invention

[0004] In order to achieve the purpose of comparing the ability of different types of zeolite molecular sieves to adsorb acidic substances in phosphate ester fire-resistant fuel, the present application provides a method for comparing the ability of different types of zeolite molecular sieves to adsorb acidic substances in phosphate ester fire-resistant fuel.

[0005] This application provides a method for comparing the ability of different types of zeolite molecular sieves to adsorb acidic substances in phosphate ester fire-resistant fuels, using the following technical solution: A method for comparing the ability of different types of zeolite molecular sieves to adsorb acidic substances in phosphate ester fire-resistant oils comprises the following steps: S1. Determine the acid value of phosphate ester fire-resistant oil; S2, cleaning the zeolite molecular sieve and drying it; S3, mixing the zeolite molecular sieve and the phosphate fire-resistant oil uniformly to obtain a mixture; S4. Storing the mixture in a constant temperature drying oven; S5. Take samples of the phosphate ester fire-resistant oil at regular intervals to test the acid value and record the results. S6. Draw the measured acid value-time curve of the phosphate ester fire-resistant oil.

[0006] By adopting the above technical solution, the zeolite molecular sieves produced by manufacturers vary in size, containing tiny powders and impurities. These powders and impurities easily enter the phosphate ester fire-resistant oil, thereby affecting the accuracy of acidic substance detection in the phosphate ester fire-resistant oil. In this application, the zeolite molecular sieve is cleaned to remove the powder and impurities on the zeolite molecular sieve, thereby ensuring the accuracy of acidic substance detection in the phosphate ester fire-resistant oil. The method of this application is used to plot acid value-time curves of different types of zeolite molecular sieves to achieve the purpose of comparing the ability of different types of zeolite molecular sieves to adsorb acidic substances in the phosphate ester fire-resistant oil.

[0007] Preferably, in step S5, the acid value of the phosphate ester fire-resistant oil is detected by titrating the phosphate ester fire-resistant oil with a potassium hydroxide ethanol solution.

[0008] By adopting the above technical solution, the titration of phosphate ester fire-resistant oil with potassium hydroxide ethanol solution has the advantages of reducing the hydrolysis of phosphate ester fire-resistant oil and reducing the interference of side reactions.

[0009] Preferably, the concentration of the potassium hydroxide ethanol solution is 0.01 mol / L to 0.05 mol / L.

[0010] Preferably, in step S3, the mass ratio of the zeolite molecular sieve to the phosphate ester fire-resistant oil is 1:5 to 1:20.

[0011] By adopting the above technical solution, in the experiment, there will be phosphate fire-resistant oil instead of acidic substances on the surface of the zeolite molecular sieve. Therefore, the mass ratio of the zeolite molecular sieve and the phosphate fire-resistant oil needs to be reasonable. If the ratio is too large, the phosphate fire-resistant oil may be quickly consumed while the molecular sieve may still not be saturated; if the ratio is too small, the acid value of the phosphate fire-resistant oil changes very little. Based on this, this application sets the mass ratio of the zeolite molecular sieve and the phosphate fire-resistant oil to 1:5~1:20.

[0012] Preferably, the sampling mass of the phosphate ester fire-resistant oil is 0.5-10 g.

[0013] By adopting the above technical solution, a significant problem encountered during the testing of the ability of zeolite molecular sieves to adsorb acidic substances in phosphate ester fire-resistant oils is that the acid value of phosphate ester fire-resistant oils fluctuates greatly. Specifically, the acid value of phosphate ester fire-resistant oils ranges from 0.05mgKOH / g to 15mgKOH / g. As a result, if the national standard GB / T 264 for the acid value test of petroleum products is followed, the volume of 0.05mol / L potassium hydroxide ethanol solution will differ by 200 times, resulting in the data precision of the experimental results not meeting the national standard GB / T 264. To address this situation, the present application adjusted the concentration and sampling quality of the potassium hydroxide ethanol solution to improve the data precision of the experimental results.

[0014] Preferably, in step S2, the drying temperature of the zeolite molecular sieve is (70±5)°C.

[0015] Preferably, in step S5, the sampling interval is 2 to 24 hours.

[0016] Preferably, in step S4, the mixture needs to be sealed and stored.

[0017] By adopting the above technical solution, under constant temperature conditions, the phosphate ester fire-resistant oil evaporates very quickly, and sealed storage can reduce the volatility of the phosphate ester fire-resistant oil, thereby further improving the accuracy of the test data.

[0018] Preferably, in step S2, the zeolite molecular sieve is washed with water for more than 2 hours.

[0019] By adopting the above technical solution, the impurities on the zeolite molecular sieve can be washed away by cleaning the zeolite molecular sieve, thereby reducing the impact of the impurities on the experimental data.

[0020] In summary, this application has the following beneficial effects: The present invention discloses a test method for comparing the adsorption of acidic substances in phosphate ester fire-resistant oils by different types of zeolite molecular sieves. The method improves the sampling quality of phosphate ester fire-resistant oils, the preparation method and concentration of potassium hydroxide ethanol titration solution used in the determination of the acid value of petroleum products in GB / B264, shortens the chemical titration process time, and improves data accuracy. The experimental operation of the present invention is simple and the cycle time is short, achieving the purpose of comparing the adsorption capacity of different types of zeolite molecular sieves for acidic substances in phosphate ester fire-resistant oils. By fixing the mixing ratio of zeolite molecular sieve and phosphate ester fire-resistant oil and the sampling mass, the experimental results are made comparable.

[0021] The mass loss caused by evaporation of the phosphate ester fire-resistant oil in the experiment was reduced by sealing and storing the mixture of zeolite molecular sieve and phosphate ester fire-resistant oil. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is the acid value-time curve of Example 1 of the present application; Figure 2 This is the acid value-time curve of Example 2 of the present application; Figure 3 This is the acid value-time curve of Example 3 of the present application. DETAILED DESCRIPTION

[0023] The present invention is further described in detail below with reference to the accompanying drawings and examples. The water used in this application is pure water that meets the third-grade water specification in GB / T6682. The burette volume, titrant concentration, and sample mass in this application are given in Table 1.

[0024] Table 1

[0025] Prepare cresol red acid-base indicator Take 0.1 g of cresol red, grind it finely, and dissolve it in 100 ml of ethanol. After boiling in a water bath for 5 minutes, remove the conical flask and slowly titrate with ethanolic potassium hydroxide solution. When the solution turns from orange-red to deep red and returns to orange-red after cooling, the preparation is complete.

[0026] Prepare potassium hydroxide ethanol solution (0.01N) Place 0.5g of potassium hydroxide in a beaker, add 420mL of ethanol to dissolve, cool, and transfer to a polyethylene container. Then, dilute to 1000mL with 95% ethanol to obtain a potassium hydroxide ethanol solution. Table 2 shows the volume correction table. The potassium hydroxide ethanol solution is calibrated at 20°C. When used at temperatures other than 20°C, the volume of the standard titrant solution must be corrected. The volume correction amounts are shown in Table 2. During titration, generally maintain a titration rate of (7±1) mL / min.

[0027] Prepare potassium hydroxide ethanol solution (0.05N) Place 2.5g of potassium hydroxide in a beaker, add 420mL of ethanol to dissolve, cool, transfer to a polyethylene container, and allow to stand. Then, dilute to 1000mL with 95% ethanol to obtain a potassium hydroxide ethanol solution. The volume correction table is shown in Table 2. The potassium hydroxide ethanol solution is calibrated at 20°C. When used at temperatures other than 20°C, the volume of the standard titrant solution must be corrected. The volume correction amounts are shown in Table 2. During titration, generally maintain a titration rate of (7±1) mL / min.

[0028] Table 2 Example 1

[0029] A method for comparing the ability of different types of zeolite molecular sieves to adsorb acidic substances in phosphate ester fire-resistant fuels comprises the following steps: S0, constant temperature drying oven set temperature is 70℃±5℃; S1. Determine the acid value of phosphate ester fire-resistant oil according to GB / T264 petroleum product acid value determination method, wherein the concentration of potassium hydroxide ethanol solution is 0.05 mol / L and the indicator is cresol red acid-base indicator; S2, washing the zeolite molecular sieve with pure water for 4 hours to remove impurities contained in the zeolite molecular sieve, then placing the washed zeolite molecular sieve in a constant temperature drying oven and drying it for 30 hours, and then taking it out, wherein the zeolite molecular sieve adopts Dandong small particle filter element; S3, adding 10g of zeolite molecular sieve and 120g of phosphate fire-resistant oil into a ground-mouth bottle and mixing evenly to obtain a mixture, wherein the mass ratio of zeolite molecular sieve to phosphate fire-resistant oil is 1:12; S4. Seal the ground-mouth bottle with a stretch film and store the mixture in a constant temperature drying oven; S5. Every 24 hours, sample and test the acid value of the phosphate ester fire-resistant oil and record the acid value. The mass of the phosphate ester fire-resistant oil sample is 10 g, the concentration of the potassium hydroxide ethanol solution is 0.05 mol / L, and the indicator is cresol red acid-base indicator. S6. Draw the acid value-time curve of the measured phosphate ester fire-resistant oil (refer to Figure 1 ). Example 2

[0030] A method for comparing the ability of different types of zeolite molecular sieves to adsorb acidic substances in phosphate ester fire-resistant fuels comprises the following steps: S0, constant temperature drying oven set temperature is 70℃±5℃; S1. Determine the acid value of phosphate ester fire-resistant oil according to GB / T264 method for determining acid value of petroleum products, wherein the concentration of potassium hydroxide ethanol solution is 0.01 mol / L and the indicator is cresol red acid-base indicator; S2, the zeolite molecular sieve was washed with pure water for 2.25h to remove impurities contained in the zeolite molecular sieve, and then the washed zeolite molecular sieve was placed in a constant temperature drying oven and dried for 25h before being taken out, wherein the zeolite molecular sieve adopts Luoyang large particle filter element; S3, adding 10g of zeolite molecular sieve and 200g of phosphate fire-resistant oil into a ground-mouth bottle and mixing them evenly to obtain a mixture, wherein the mass ratio of zeolite molecular sieve to phosphate fire-resistant oil is 1:20; S4. Seal the ground-mouth bottle with a stretch film and store the mixture in a constant temperature drying oven; S5. Every 24 hours, sample and test the acid value of the phosphate ester fire-resistant oil and record the acid value. The mass of the phosphate ester fire-resistant oil sample is 0.5 g, the concentration of the potassium hydroxide ethanol solution is 0.01 mol / L, and the indicator is cresol red acid-base indicator. S6. Draw the acid value-time curve of the measured phosphate ester fire-resistant oil (refer to Figure 2 ). Example 3

[0031] A method for comparing the ability of different types of zeolite molecular sieves to adsorb acidic substances in phosphate ester fire-resistant fuels comprises the following steps: S0, constant temperature drying oven set temperature is 70℃±5℃; S1. Determine the acid value of phosphate ester fire-resistant oil according to GB / T264 method for determining acid value of petroleum products, wherein the concentration of potassium hydroxide ethanol solution is 0.01 mol / L and the indicator is cresol red acid-base indicator; S2, the zeolite molecular sieve was washed with pure water for 2.25h to remove impurities contained in the zeolite molecular sieve, and then the washed zeolite molecular sieve was placed in a constant temperature drying oven and dried for 25h before being taken out, wherein the zeolite molecular sieve adopts Luoyang large particle filter element; S3, adding 10g of zeolite molecular sieve and 50g of phosphate fire-resistant oil into a ground-mouth bottle and mixing evenly to obtain a mixture, wherein the mass ratio of zeolite molecular sieve to phosphate fire-resistant oil is 1:5; S4. Seal the ground-mouth bottle with a stretch film and store the mixture in a constant temperature drying oven; S5. Every 2 hours, sample the phosphate ester fire-resistant oil for testing the acid value and record the acid value. The mass of the phosphate ester fire-resistant oil sample is 0.5 g, the concentration of the potassium hydroxide ethanol solution is 0.01 mol / L, and the indicator is cresol red acid-base indicator. S6. Draw the acid value-time curve of the measured phosphate ester fire-resistant oil (refer to Figure 3 ).

[0032] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make non-creative modifications to the present embodiment as needed, but as long as they are within the scope of the claims of the present application, they are protected by the patent law.

Claims

1. A method for comparing the ability of different types of zeolite molecular sieves to adsorb acidic substances in phosphate ester fire-resistant oils, characterized in that: The process includes the following steps: S1. Determine the acid value of phosphate ester fire-resistant oil; S2, cleaning the zeolite molecular sieve and drying it; S3, mixing the zeolite molecular sieve and the phosphate fire-resistant oil uniformly to obtain a mixture; S4. Storing the mixture in a constant temperature drying oven; S5. Take samples of the phosphate ester fire-resistant oil at regular intervals to test the acid value and record the results. S6. Draw the measured acid value-time curve of the phosphate ester fire-resistant oil.

2. The method of claim 1, wherein: In the step S5, the acid value of the phosphate ester fire-resistant oil is detected by titrating the phosphate ester fire-resistant oil with a potassium hydroxide ethanol solution.

3. The method of comparing the adsorption capacity of different types of zeolite molecular sieves for acidic substances in phosphate ester fire-resistant oils according to claim 2, characterized in that: The concentration of the potassium hydroxide ethanol solution is 0.01mol / L~0.05mol / L.

4. The method of claim 1, wherein: In step S3, the mass ratio of the zeolite molecular sieve to the phosphate ester fire-resistant oil is 1:5-1:

20.

5. The method of comparing the adsorption capacity of different types of zeolite molecular sieves for acidic substances in phosphate ester fire-resistant oils according to claim 3, characterized in that: In step S5, the mass of the phosphate fire-resistant oil sample is 0.5-10 g.

6. The method of claim 1, wherein: In step S2, the drying temperature of the zeolite molecular sieve is (70±5)°C.

7. The method of claim 1, wherein: In step S5, the sampling interval is 2 to 24 hours.

8. The method of claim 1, wherein: In step S4, the mixture needs to be sealed and stored.

9. The method of claim 1, wherein: In step S2, the zeolite molecular sieve is washed with water for more than 2 hours.

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