Method for rapidly evaluating performance of phosphate fire-resistant oil based on microwave catalysis

The hydrolysis and oxidation process of phosphate fuel-resistant oil is accelerated through microwave catalysis, and the problem of long detection cycles in the existing technology is solved, fast and accurate performance evaluation is achieved, and the safe operation of the power generation system is ensured.

CN119104703APending Publication Date: 2024-12-10XIAN THERMAL POWER RES INST CO LTD +1
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Patent Information

Application Number
CN202411301713.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-18
Publication Date
2024-12-10

AI Technical Summary

Technical Problem

The phosphate fuel resistance performance evaluation method in the prior art has a long detection cycle, and its stable performance cannot be evaluated quickly and accurately, which affects the safe operation of the power generation system.

Method used

Using a microwave catalysis-based method, a catalyst with a porous structure is formed by mixing metal salts with a support and microwave catalysis is performed in a microwave reactor, and oxygen is used to accelerate the hydrolysis and oxidation process in the phosphate anti-fuel oil, shortening the detection cycle.

Benefits of technology

The rapid and accurate evaluation of the fuel resistance of phosphate ester is achieved, and the detection cycle is shortened from the traditional 164 hours to 30-60 minutes, improving work efficiency and safety.

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Abstract

The invention belongs to the technical field of phosphate fire-resistant oil for electric power, and particularly relates to a method for rapidly evaluating the stability of fire-resistant oil. The preparation method specifically comprises the following steps: dissolving metal salt in water, mixing and stirring, and fully dissolving; adding a carrier, fully mixing, and then evaporating and drying to remove moisture to obtain a metal catalyst with a porous structure; the method comprises the following steps: mixing a metal catalyst, water and triaryl phosphate, adding the mixture into a microwave reactor, carrying out microwave catalysis, continuously introducing oxygen, after the microwave catalysis reaction is finished, cooling, taking out an oil sample, filtering to remove the metal catalyst to obtain a treated oil sample, detecting the acid value and resistivity of the oil sample, and evaluating the stability of the oil sample. By utilizing the high efficiency of microwave catalysis, the evaluation period is greatly shortened, and the working efficiency is improved.
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Description

Technical Field

[0001] The invention belongs to the technical field of phosphate fire-resistant oil for electric power, and in particular relates to a method for rapidly evaluating the stability performance of fire-resistant oil. Background Art

[0002] Phosphate ester fire-resistant oil is used in the turbine speed control system of power plants. It has lubricating and flame retardant effects. Its quality determines the safety and reliability of the speed control system, and also affects the service life of the oil itself. The better the stability of phosphate ester fire-resistant oil, the slower the oil deterioration rate during use, and the higher the safety and reliability of equipment operation. If the deterioration rate is fast, the acid value increases rapidly and the resistivity decreases gradually, which will cause corrosion to the equipment and seriously threaten the safe and stable operation of the equipment. Therefore, it is very important to evaluate the performance of phosphate ester fire-resistant oil.

[0003] At present, the evaluation of the performance of phosphate ester fire-resistant oil is mainly based on the technical index system in DL / T571 "Guidelines for Operation and Maintenance of Phosphate Ester Fire-Resistant Oil for Power Plants" widely used in the power industry. This standard specifies a number of key parameters including acid value, resistivity and moisture content, providing a clear basis for evaluation for power generation companies. When all indicators of phosphate ester fire-resistant oil meet the standard requirements, it is considered a qualified product and can be safely put into use; otherwise, remedial measures such as oil regeneration and replacement of new oil should be taken according to the specific situation to restore or improve the performance of the oil.

[0004] However, although this method has been widely adopted in practice and has played an important guiding role, its limitations cannot be ignored. The testing process of some key indicators such as hydrolysis stability and oxidation stability is complicated and time-consuming, which not only increases the testing cost, but also may delay the timely treatment of oil products due to the long testing cycle, posing a potential threat to the safe operation of the power generation system.

[0005] In view of the above shortcomings, the power industry is also constantly exploring more efficient and accurate methods for evaluating the performance of phosphate fire-resistant oils. The closed cup aging test method for power oil is one of them. It accelerates the aging process of oil products under specific conditions to simulate the deterioration in long-term operation, thereby evaluating its stability. However, this method also faces the problem of long test cycles (such as 164 hours), which limits its flexibility and efficiency in practical applications. Summary of the invention

[0006] The purpose of the present invention is to solve the problem that the stability of phosphate ester fire-resistant oil cannot be quickly evaluated in the above-mentioned prior art, and to provide a method for quickly and accurately evaluating the flame retardant performance of phosphate ester, which has the characteristics of short detection cycle and high accuracy.

[0007] In order to achieve the above object, the present invention adopts the following technical solutions:

[0008] The present invention provides a method for quickly evaluating the performance of phosphate fire-resistant oil based on microwave catalysis, which specifically comprises the following steps:

[0009] S1: dissolving a metal salt in water, mixing and stirring to fully dissolve; adding a carrier, fully mixing, and then evaporating and drying to remove water to obtain a metal catalyst with a porous structure;

[0010] S2: Mix a metal catalyst, water and triaryl phosphate and add them into a microwave reactor for microwave catalysis and continuously introduce oxygen. After the microwave catalytic reaction is completed, the oil sample is taken out after cooling, and the metal catalyst is filtered out to obtain a treated oil sample. The acid value and resistivity of the oil sample are tested to evaluate its stability.

[0011] Preferably, the metal salt is one or more of copper sulfate, manganese sulfate and cobalt sulfate.

[0012] Preferably, the carrier is one or more of diatomaceous earth, kaolin and molecular sieve.

[0013] Preferably, the mass ratio of the metal salt to the carrier is (1-10):(1-20).

[0014] Preferably, the mass of the metal catalyst in S2 is 2% to 5% of the mass of the triaryl phosphate.

[0015] Preferably, the mass of the water in S2 is 1% to 3% of the mass of the triaryl phosphate.

[0016] Preferably, the flow rate of the oxygen introduced is 100 to 500 mL / min.

[0017] Preferably, the purity of the oxygen is not less than 99.9%.

[0018] Preferably, the power of the microwave reactor is 100-1000W.

[0019] Preferably, the microwave catalysis time is 30 to 60 minutes.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] The metal salt of the present invention is loaded on a carrier to form a metal catalyst with a porous structure, and the metal catalyst can promote the generation of free radicals. At the same time, the present invention adopts microwave catalysis, and under the action of oxygen, the system can generate a large number of free radicals in a short time, accelerating the hydrolysis and oxidation process of unstable triaryl phosphate in phosphate fire-resistant oil, so as to achieve the purpose of quickly evaluating its performance in a short time. DETAILED DESCRIPTION

[0022] In order to enable those skilled in the art to better understand the solutions of the present invention, the technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only embodiments of a part of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work should fall within the scope of protection of the present invention.

[0023] It should be understood that when used in this specification and the appended claims, the terms "include" and "comprises" indicate the presence of described features, integers, steps, operations, elements and / or components, but do not exclude the presence or addition of one or more other features, integers, steps, operations, elements, components and / or combinations thereof.

[0024] It should also be understood that the terms used in the present specification are only for the purpose of describing specific embodiments and are not intended to limit the present invention. As used in the present specification and the appended claims, unless the context clearly indicates otherwise, the singular forms "a", "an" and "the" are intended to include plural forms.

[0025] It should be further understood that the term "and / or" used in the present description and the appended claims refers to any and all possible combinations of one or more of the associated listed items, and includes these combinations.

[0026] The present invention proposes a method for rapidly evaluating the performance of phosphate fire-resistant oil by using microwave catalysis. The main component of phosphate fire-resistant oil is triaryl phosphate, and its degradation usually includes two processes of hydrolysis and oxidation. Hydrolysis refers to the cleavage of ester bonds in triaryl phosphate to generate monobasic or dibasic acids and free phenols, resulting in an increase in the acid value of the oil sample; oxidation refers to the free radical chain reaction of hydrocarbon substituent groups in triaryl phosphate, resulting in the degradation of phosphate. The present invention adopts microwave catalysis, and under the action of oxygen, the system can generate a large number of free radicals in a short time, accelerate the hydrolysis and oxidation process of unstable triaryl phosphate in phosphate fire-resistant oil, so as to achieve the purpose of rapidly evaluating its performance in a short time.

[0027] The present invention provides a method for quickly evaluating the performance of phosphate fire-resistant oil based on microwave catalysis, which specifically comprises the following steps:

[0028] S1: dissolving a metal salt in water, mixing and stirring to fully dissolve; then adding a carrier, mixing fully, and then evaporating and drying to remove water to obtain a metal catalyst with a porous structure;

[0029] S2: Mix a metal catalyst, water and a triaryl phosphate and add them into a reaction vessel, place the reaction vessel in a microwave reactor, turn on the microwave reactor and the stirring device, continuously introduce oxygen, and after microwave catalysis for a period of time at a certain power, close the reactor, take out the oil sample after cooling, filter out the metal catalyst, obtain the treated oil sample, detect the acid value and resistivity of the oil sample, and evaluate its stability.

[0030] The metal salt is one or more of copper sulfate, manganese sulfate and cobalt sulfate. The metal salts such as copper sulfate, manganese sulfate and cobalt sulfate are selected. These metal ions have good catalytic activity and cooperate with microwaves to promote the oxidation reaction of phosphate fire-resistant oil, thereby simulating the degradation process in actual operation; the carrier is one or more of diatomaceous earth, kaolin and molecular sieve. Using diatomaceous earth, kaolin and molecular sieve as carriers not only increases the specific surface area of ​​the catalyst, improves the dispersibility and stability of the catalyst, but also enhances the contact efficiency between the catalyst and the reactant, and accelerates the reaction rate; the mass ratio of the metal salt to the carrier is (1-10): (1-20).

[0031] The mass of the metal catalyst in S2 is 2% to 5% of the mass of the triaryl phosphate; the mass of the water in S2 is 1% to 3% of the mass of the triaryl phosphate.

[0032] The flow rate of the oxygen introduced is 100-500 mL / min; the purity of the oxygen is not less than 99.9%; the continuous introduction of high-purity (not less than 99.9%) oxygen simulates the working environment of phosphate fire-resistant oil under high temperature, high pressure and oxygen presence, accelerates the oxidative degradation process, and makes the evaluation closer to the actual working conditions.

[0033] The power of the microwave reactor is 100-1000W; the microwave catalysis time is 30-60min.

[0034] The microwave reactor is a variable frequency microwave reactor. The present invention adopts a variable frequency microwave reactor, which can achieve the high temperature and high pressure conditions required for the reaction in a relatively short time, while avoiding the temperature gradient problem in the traditional heating method, and ensuring the uniformity and controllability of the reaction; the water is deionized water.

[0035] The present invention utilizes the high efficiency of microwave catalysis, greatly shortens the evaluation cycle, and improves work efficiency.

[0036] Example 1

[0037] Take two different phosphate fire-resistant oils, A and B, and perform the following steps respectively:

[0038] 0.8 g of copper sulfate was dissolved in 30.0 g of deionized water, mixed and stirred to fully dissolve, and then 8.0 g of molecular sieve was added to the solution, mixed thoroughly, and then evaporated and dried to remove water to obtain a molecular sieve catalyst loaded with copper sulfate; 5 g of molecular sieve catalyst loaded with copper sulfate, 1.0 g of deionized water and 100.0 g of phosphate fire-resistant oil were added to a reaction container, the reaction container was placed in a variable frequency microwave reactor, the microwave reactor and the stirring device were turned on, oxygen was continuously introduced at a rate of 200 ml / min, microwave catalysis was performed at a power of 200 W for 40 minutes, the reactor was closed, the oil sample was taken out after cooling, the metal catalyst was filtered to remove the treated oil sample, the acid value and resistivity of the oil sample were detected, and the stability of the two phosphate fire-resistant oils A and B was evaluated.

[0039] Example 2

[0040] Take two different phosphate fire-resistant oils, A and B, and perform the following steps respectively:

[0041] Take 0.8g of copper sulfate and dissolve it in 30.0g of deionized water, mix and stir, fully dissolve, then add 8.0g of molecular sieve to the solution, mix thoroughly, then evaporate and dry to remove water, and obtain a molecular sieve catalyst loaded with copper sulfate. Take 5.0g of catalyst, 3.0g of deionized water and 100.0g of phosphate fire-resistant oil and add them to a reaction container, place the reaction container in a variable frequency microwave reactor, turn on the microwave reactor and the stirring device, continuously introduce oxygen at a rate of 300ml / min, and at a power of 300w, microwave catalysis for 40min, then close the reactor, cool and take out the oil sample, filter to remove the metal catalyst, obtain the treated oil sample, detect the acid value and resistivity of the oil sample, and evaluate the stability of the two phosphate fire-resistant oils A and B.

[0042] Example 3

[0043] Take two different phosphate fire-resistant oils, A and B, and perform the following steps respectively:

[0044] 0.8g of copper sulfate was dissolved in 30.0g of deionized water, mixed and stirred, fully dissolved, then 12.0g of molecular sieve was added to the solution, fully mixed, then evaporated and dried to remove water, and a molecular sieve catalyst loaded with copper sulfate was obtained. 2.0g of catalyst, 2.0g of deionized water and 100.0g of phosphate fire-resistant oil were added to a reaction vessel, the reaction vessel was placed in a variable frequency microwave reactor, the microwave reactor and the stirring device were turned on, oxygen was continuously introduced at a rate of 500ml / min, and microwave catalysis was performed at a power of 500w for 40min, then the reactor was closed, the oil sample was taken out after cooling, the metal catalyst was removed by filtration, and the treated oil sample was obtained, the acid value and resistivity of the oil sample were detected, and the stability of the two phosphate fire-resistant oils A and B was evaluated.

[0045] Example 4

[0046] 1.8 g of manganese sulfate is dissolved in 30.0 g of deionized water, mixed and stirred to fully dissolve, then 1.8 g of diatomaceous earth is added to the solution, mixed fully, then evaporated and dried to remove water, and a diatomaceous earth catalyst loaded with manganese sulfate is obtained; 2 g of the diatomaceous earth catalyst loaded with manganese sulfate, 1.0 g of deionized water and 100.0 g of phosphate fire-resistant oil are added to a reaction container, the reaction container is placed in a variable frequency microwave reactor, the microwave reactor and the stirring device are turned on, oxygen is continuously introduced at a rate of 100 ml / min, microwave catalysis is performed for 30 minutes at a power of 100 W, the reactor is closed, the oil sample is taken out after cooling, the metal catalyst is filtered to remove the metal catalyst, the treated oil sample is obtained, the acid value and resistivity of the oil sample are detected, and the stability of the phosphate fire-resistant oil is evaluated.

[0047] Example 5

[0048] 0.8 g of cobalt sulfate is dissolved in 30.0 g of deionized water, mixed and stirred to fully dissolve, then 16.0 g of clay is added to the solution, mixed fully, then evaporated and dried to remove water, and a clay catalyst loaded with cobalt sulfate is obtained; 3 g of the clay catalyst loaded with cobalt sulfate, 1.0 g of deionized water and 100.0 g of phosphate fire-resistant oil are added to a reaction container, the reaction container is placed in a variable frequency microwave reactor, the microwave reactor and the stirring device are turned on, oxygen is continuously introduced at a rate of 200 ml / min, microwave catalysis is performed for 35 minutes at a power of 400 W, the reactor is closed, the oil sample is taken out after cooling, the metal catalyst is filtered to remove the metal catalyst, the treated oil sample is obtained, the acid value and resistivity of the oil sample are detected, and the stability of the phosphate fire-resistant oil is evaluated.

[0049] Example 6

[0050] A total of 1.8 g of a mixture of copper sulfate and manganese sulfate is dissolved in 30.0 g of deionized water, mixed and stirred to fully dissolve, and then a total of 1.8 g of a mixture of diatomaceous earth and kaolin is added to the solution, fully mixed, and then evaporated and dried to remove water to obtain a diatomaceous earth-kaolin catalyst loaded with copper sulfate and manganese sulfate; 3 g of the diatomaceous earth-kaolin catalyst loaded with copper sulfate and manganese sulfate, 2.0 g of deionized water and 100.0 g of phosphate fire-resistant oil are added to a reaction container, the reaction container is placed in a variable frequency microwave reactor, the microwave reactor and the stirring device are turned on, oxygen is continuously introduced at a rate of 300 ml / min, microwave catalysis is performed for 45 minutes at a power of 600 W, the reactor is closed, the oil sample is taken out after cooling, the metal catalyst is filtered to remove, the treated oil sample is obtained, the acid value and resistivity of the oil sample are detected, and the stability of the phosphate fire-resistant oil is evaluated.

[0051] Example 7

[0052] A total of 0.8 g of a mixture of copper sulfate and cobalt sulfate is dissolved in 30.0 g of deionized water, mixed and stirred to fully dissolve, and then a total of 4.0 g of a mixture of kaolin and molecular sieve is added to the solution, fully mixed, and then evaporated and dried to remove water to obtain a kaolin-molecular sieve catalyst loaded with copper sulfate and cobalt sulfate; 4 g of the kaolin-molecular sieve catalyst loaded with copper sulfate and cobalt sulfate, 3.0 g of deionized water and 100.0 g of phosphate fire-resistant oil are added to a reaction container, the reaction container is placed in a variable frequency microwave reactor, the microwave reactor and the stirring device are turned on, oxygen is continuously introduced at a rate of 400 ml / min, microwave catalysis is performed at a power of 700 W for 50 minutes, the reactor is closed, the oil sample is taken out after cooling, the metal catalyst is filtered to remove the treated oil sample, the acid value and resistivity of the oil sample are detected, and the stability of the phosphate fire-resistant oil is evaluated.

[0053] Example 8

[0054] A total of 0.8 g of a mixture of manganese sulfate and cobalt sulfate is dissolved in 30.0 g of deionized water, mixed and stirred to fully dissolve, and then a total of 8.0 g of a mixture of diatomaceous earth and molecular sieve is added to the solution, fully mixed, and then evaporated and dried to remove water to obtain a diatomaceous earth-molecular sieve catalyst loaded with manganese sulfate and cobalt sulfate; 4 g of the diatomaceous earth-molecular sieve catalyst loaded with manganese sulfate and cobalt sulfate, 1.0 g of deionized water and 100.0 g of phosphate fire-resistant oil are added to a reaction container, the reaction container is placed in a variable frequency microwave reactor, the microwave reactor and the stirring device are turned on, oxygen is continuously introduced at a rate of 500 ml / min, microwave catalysis is performed for 55 minutes at a power of 800 w, the reactor is closed, the oil sample is taken out after cooling, the metal catalyst is filtered to remove the treated oil sample, the acid value and resistivity of the oil sample are detected, and the stability of the phosphate fire-resistant oil is evaluated.

[0055] Example 9

[0056] A total of 0.8 g of a mixture of copper sulfate, manganese sulfate and cobalt sulfate is dissolved in 30.0 g of deionized water, mixed and stirred to fully dissolve, and then a total of 8.0 g of a mixture of diatomaceous earth, clay and molecular sieve is added to the solution, fully mixed, and then evaporated and dried to remove water to obtain a diatomaceous earth-clay-molecular sieve catalyst loaded with copper sulfate, manganese sulfate and cobalt sulfate; 5 g of the diatomaceous earth-clay-molecular sieve catalyst loaded with copper sulfate, manganese sulfate and cobalt sulfate, 2.0 g of deionized water and 100.0 g of phosphate fire-resistant oil are added to a reaction container, the reaction container is placed in a variable frequency microwave reactor, the microwave reactor and the stirring device are turned on, oxygen is continuously introduced at a rate of 300 ml / min, microwave catalysis is performed at a power of 900 W for 60 minutes, the reactor is closed, the oil sample is taken out after cooling, the metal catalyst is filtered to remove the treated oil sample, the acid value and resistivity of the oil sample are detected, and the stability of the phosphate fire-resistant oil is evaluated.

[0057] Example 10

[0058] 0.8 g of copper sulfate is dissolved in 30.0 g of deionized water, mixed and stirred to fully dissolve, and then a mixture of 8.0 g of diatomaceous earth, kaolin and molecular sieve is added to the solution, fully mixed, and then evaporated and dried to remove water to obtain a diatomaceous earth-kaolin-molecular sieve catalyst loaded with copper sulfate; 5 g of diatomaceous earth-kaolin-molecular sieve catalyst loaded with copper sulfate, 3.0 g of deionized water and 100.0 g of phosphate fire-resistant oil are added to a reaction container, the reaction container is placed in a variable frequency microwave reactor, the microwave reactor and the stirring device are turned on, oxygen is continuously introduced at a rate of 400 ml / min, microwave catalysis is performed for 40 minutes at a power of 1000 w, the reactor is closed, the oil sample is taken out after cooling, the metal catalyst is filtered to remove the metal catalyst, the treated oil sample is obtained, the acid value and resistivity of the oil sample are detected, and the stability of the phosphate fire-resistant oil is evaluated.

[0059] Embodiment 11

[0060] 0.8 g of manganese sulfate was dissolved in 30.0 g of deionized water, mixed and stirred to fully dissolve, and then a mixture of 8.0 g of diatomaceous earth, kaolin and molecular sieve was added to the solution, fully mixed, and then evaporated and dried to remove water to obtain a diatomaceous earth-kaolin-molecular sieve catalyst loaded with copper sulfate; 5 g of diatomaceous earth-kaolin-molecular sieve catalyst loaded with copper sulfate, 3.0 g of deionized water and 100.0 g of phosphate fire-resistant oil were added to a reaction container, the reaction container was placed in a variable frequency microwave reactor, the microwave reactor and the stirring device were turned on, oxygen was continuously introduced at a rate of 400 ml / min, microwave catalysis was performed for 40 min at a power of 1000 w, the reactor was closed, the oil sample was taken out after cooling, the metal catalyst was filtered to remove the treated oil sample, the acid value and resistivity of the oil sample were detected, and the stability of the phosphate fire-resistant oil was evaluated.

[0061] Example 12

[0062] 0.8 g of cobalt sulfate is dissolved in 30.0 g of deionized water, mixed and stirred to fully dissolve, and then a total of 8.0 g of a mixture of diatomaceous earth, kaolin and molecular sieve is added to the solution, fully mixed, and then evaporated and dried to remove water to obtain a diatomaceous earth-kaolin-molecular sieve catalyst loaded with copper sulfate; 5 g of the diatomaceous earth-kaolin-molecular sieve catalyst loaded with copper sulfate, 3.0 g of deionized water and 100.0 g of phosphate fire-resistant oil are added to a reaction container, the reaction container is placed in a variable frequency microwave reactor, the microwave reactor and the stirring device are turned on, oxygen is continuously introduced at a rate of 400 ml / min, microwave catalysis is performed for 40 minutes at a power of 1000 w, the reactor is closed, the oil sample is taken out after cooling, the metal catalyst is filtered to remove the treated oil sample, the acid value and resistivity of the oil sample are detected, and the stability of the phosphate fire-resistant oil is evaluated.

[0063] In order to measure the accuracy of this method, the closed cup aging method was used to age the two different phosphate fire-resistant oils A and B in Examples 1 to 12 and the two different phosphate fire-resistant oils A and B before treatment, and the acid value and resistivity were tested. The specific operation process is as follows:

[0064] First, the water content of the phosphate fire-resistant oil is adjusted to 800 mg / L±50 mg / L. Then, 200.0 g of the phosphate fire-resistant oil is placed in a conical flask, the cleaned spiral copper wire is placed in the conical flask, and a ground stopper is put on the conical flask. Then, the conical flask is placed in an oven at 115°C±1°C, and aged in the oven for 164 hours. After the aging is completed, the conical flask containing the sample is taken out, and after cooling to room temperature, the acid value and resistivity of the oil sample are detected. The performance test results of the treated oil samples obtained in Examples 1 to 12 are shown in Table 1.

[0065] Table 1 Performance test data of oil samples A and B obtained in Examples 1 to 12

[0066]

[0067]

[0068] As shown in Table 1, the changes in the acid value and resistivity of oil sample A in the closed cup aging test method are smaller than those of oil sample B, indicating that the stability of sample A is better than that of sample B. The acid value and resistivity change trends of oil samples A and B in Examples 1 to 12 of the present invention are consistent with those of the closed cup aging method, that is, the acid value increases and the resistivity decreases, and the acid value and resistivity changes of oil sample A are both smaller than those of sample B, which also indicates that the stability of sample A is better than that of sample B. That is, the results obtained by the microwave catalysis method of the present invention are consistent with those obtained by the prior art method, and the detection cycle is shortened from 164h to 40min, which greatly reduces the time required for the test.

[0069] The above contents are only for explaining the technical idea of ​​the present invention and cannot be used to limit the protection scope of the present invention. Any changes made on the basis of the technical solution in accordance with the technical idea proposed by the present invention shall fall within the protection scope of the claims of the present invention.

Claims

1. A method for rapidly evaluating the performance of phosphate fire-resistant oil based on microwave catalysis. It is characterized in that The specific steps include: S1: dissolving a metal salt in water, mixing and stirring to fully dissolve; adding a carrier, fully mixing, and then evaporating and drying to remove water to obtain a metal catalyst with a porous structure; S2: Mix a metal catalyst, water and triaryl phosphate and add them into a microwave reactor for microwave catalysis and continuously introduce oxygen. After the microwave catalytic reaction is completed, the oil sample is taken out after cooling, and the metal catalyst is filtered out to obtain a treated oil sample. The acid value and resistivity of the oil sample are tested to evaluate its stability.

2. The method for rapidly evaluating the performance of phosphate fire-resistant oil based on microwave catalysis according to claim 1, It is characterized in that The metal salt is one or more of copper sulfate, manganese sulfate and cobalt sulfate.

3. The method for rapidly evaluating the performance of phosphate fire-resistant oil based on microwave catalysis according to claim 1, It is characterized in that The carrier is one or more of diatomaceous earth, white clay and molecular sieve.

4. The method for rapidly evaluating the performance of phosphate fire-resistant oil based on microwave catalysis according to claim 1, It is characterized in that The mass ratio of the metal salt to the carrier is (1-10):(1-20).

5. The method for rapidly evaluating the performance of phosphate fire-resistant oil based on microwave catalysis according to claim 1, It is characterized in that The mass of the metal catalyst in S2 is 2% to 5% of the mass of the triaryl phosphate.

6. The method for rapidly evaluating the performance of phosphate fire-resistant oil based on microwave catalysis according to claim 1, It is characterized in that The mass of the water in S2 is 1% to 3% of the mass of the triaryl phosphate.

7. The method for rapidly evaluating the performance of phosphate fire-resistant oil based on microwave catalysis according to claim 1, It is characterized in that The flow rate of the oxygen introduced is 100-500 mL / min.

8. The method for rapidly evaluating the performance of phosphate fire-resistant oil based on microwave catalysis according to claim 1, It is characterized in that The purity of the oxygen is not less than 99.9%.

9. The method for rapidly evaluating the performance of phosphate fire-resistant oil based on microwave catalysis according to claim 1, It is characterized in that The power of the microwave reactor is 100-1000W.

10. The method for rapidly evaluating the performance of phosphate fire-resistant oil based on microwave catalysis according to claim 1, It is characterized in that The microwave catalysis time is 30 to 60 minutes.

Citation Information

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