CN113201387A - Low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance and preparation method thereof - Google Patents
Low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance and preparation method thereof Download PDFInfo
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Abstract
The invention discloses low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance and a preparation method thereof, and the environment-friendly natural ester mixed insulating oil consists of an insulating oil mixture, zinc diamyldithiocarbamate accounting for 1.3-1.5% of the weight of the oil, antimony dialkyldithiocarbamate accounting for 1.1-1.3% of the weight of the oil, 4' -methylenebis (2, 6-di-tert-butylphenol) accounting for 0.5-0.7% of the weight of the oil, polymethacrylate accounting for 0.8-1.0% of the weight of the oil and poly alpha olefin accounting for 12-15% of the weight of the oil, wherein the insulating oil mixture is formed by mixing natural ester insulating oil, epoxidized insulating oil and high-oleic acid insulating oil according to the volume ratio of 4-5: 1.5-2: 3-4. The natural ester mixed insulating oil prepared by the invention has excellent oxidation resistance and low temperature resistance, good physical, chemical and electrical properties, can meet the use conditions at low temperature, and effectively expands the application range of the natural ester insulating oil.
Description
Technical Field
The invention belongs to the technical field of insulating oil, and particularly relates to low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance and a preparation method thereof.
Background
The oil-immersed transformer has been used for more than 100 years by adopting mineral insulating oil as a cooling insulating medium, but the biodegradability of the mineral insulating oil is poor, leakage often occurs in the using process to pollute the environment, and particularly in areas such as agriculture, forestry, water sources and buildings, the difficult problem of recycling waste mineral insulating oil and the fire and large-area power failure accidents caused by overload of the mineral insulating oil transformer seriously affect the life of people. Compared with mineral insulating oil, the dielectric constants of the natural ester insulating oil and the insulating paper are closer, and the electric field distribution of the insulating oil and the insulating paper in an alternating current electric field in a natural ester oil paper insulating system is more uniform; the natural ester insulating oil can effectively delay the aging rate of insulating paper and prolong the insulating life of the paper, the service life of the insulating paper in the natural ester insulating oil transformer is 5-8 times that of the insulating paper in the mineral oil transformer, and the life cycle cost of the natural ester insulating oil transformer can be effectively reduced. Because the natural ester insulating oil has the characteristics of reproducibility, high ignition point, easy biodegradation, paper insulation aging delay and the like, the natural ester insulating oil is considered to be a good liquid dielectric medium for developing an energy-saving oil-immersed transformer with overload capacity. Therefore, with the increasing shortage of petroleum resources and the gradual enhancement of environmental awareness of people, the natural ester insulating oil as a green, environment-friendly and renewable resource is inevitably a future development direction in the field of insulating oil, and at present, more than 200 tens of thousands of natural ester insulating oil transformers are in net hanging operation globally.
The natural ester insulating oil has the following defects while having excellent performance: 1) poor oxidation resistance, mainly caused by the large number of unsaturated double bonds in the fatty acid chains of the triglycerides and the glyceryl groups in the triglycerides; 2) the poor low temperature fluidity is mainly caused by the large molecular weight of triglycerides. It is generally considered that monounsaturated fatty acids have good oxidation stability and low-temperature fluidity, so that natural ester insulating oil needs to select natural ester having a high content of monounsaturated fatty acids as a raw material oil. The content of monounsaturated fatty acid in camellia seed oil and olive oil can reach more than 70 percent, but the production cost is high, the content of monounsaturated fatty acid in soybean oil is relatively high, the planting range is wide, and the production cost is low, so that the soybean oil is mostly adopted at home and abroad to process and produce the natural ester insulating oil by taking the soybean oil as base oil.
Modifications or additives may be used to improve the oxidation resistance and low temperature fluidity of natural ester insulating oils in general. However, the oxidation resistance and low-temperature fluidity of the natural ester insulating oil are improved by using the additive alone, and the obtained oxidation resistance and low-temperature fluidity cannot meet related performance requirements under normal conditions; the double bonds of triglyceride in the natural ester insulating oil can be eliminated by adopting an epoxidation modification mode, so that the natural ester insulating oil has better oxidation resistance, the tendency of forming oil sludge is obviously reduced, and the antioxidant also has very good sensitivity, but the saturation degree of the natural ester insulating oil is increased, and further the low-temperature fluidity is further deteriorated; hydrogenation can completely convert unsaturated fatty acids in the natural ester insulating oil into saturated fatty acids, but improves the oxidation resistance of the natural ester insulating oil and simultaneously reduces the low-temperature fluidity of the natural ester insulating oil.
To further improve the properties of natural ester insulating oils, there are currently a number of studies reporting the combination of modification and the use of additives. Chinese patent CN101538500A discloses a method for preparing insulating oil from vegetable oil as raw material, which comprises the steps of alkali neutralization, reduced pressure distillation, hydrogenation, deep refining, etc. of vegetable oil, and finally adding additives to prepare the insulating oil from vegetable oil as raw material. Chinese patent CN102682869A discloses a vegetable insulating oil and a preparation method thereof, wherein the vegetable insulating oil is prepared by carrying out ester exchange, reduced pressure distillation, decoloration, deacidification, filtration, deep dehydration and other processes on refined vegetable oil, and finally adding an additive.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance and a preparation method thereof. The preparation method has the advantages of short period, environmental protection, economy and high efficiency, can obviously improve the oxidation resistance and low temperature resistance of the natural ester mixed insulating oil, and effectively enlarges the application range of the natural ester mixed insulating oil.
In order to achieve the purpose, the invention adopts the following technical scheme:
the low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance is characterized by comprising an insulating oil mixture, zinc diamyldithiocarbamate accounting for 1.3-1.5% of the weight of the oil, antimony dialkyldithiocarbamate accounting for 1.1-1.3% of the weight of the oil, 4' -methylenebis (2, 6-di-tert-butylphenol) accounting for 0.5-0.7% of the weight of the oil, polymethacrylate accounting for 0.8-1.0% of the weight of the oil and poly alpha olefin accounting for 12-15% of the weight of the oil.
Further, the insulating oil mixture is composed of a natural ester insulating oil, an epoxidized insulating oil and a high oleic acid insulating oil, all of which are based on soybean oil.
Furthermore, the volume ratio of the natural ester insulating oil to the epoxidized insulating oil to the high oleic acid insulating oil is 4-5: 1.5-2: 3-4.
Furthermore, the high oleic acid insulating oil is refined from high oleic acid soybean oil or prepared by selective hydrogenation modification of soybean oil, and the oleic acid content in the obtained high oleic acid insulating oil is more than 70%.
Further, the preparation method of the low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance comprises the following steps:
(1) under stirring and vacuum conditions, heating natural ester insulating oil, epoxidized insulating oil and high oleic acid insulating oil respectively, then performing vacuum dehydration, mixing according to corresponding proportions, performing short-time ultrasonic dispersion treatment, and continuously stirring for 15-18 min;
(2) and (2) sequentially adding zinc diamyldithiocarbamate, antimony dialkyldithiocarbamate, 4' -methylenebis (2, 6-di-tert-butylphenol), polymethacrylate and poly-alpha-olefin in corresponding mass proportion into the insulating oil mixture subjected to ultrasonic treatment in the step (1), performing short-time ultrasonic dispersion treatment again, continuously stirring for 25-30 min, and then cooling the natural ester mixed insulating oil to room temperature in vacuum to obtain the product of the invention.
Further, in the step (1), the stirring speed is 80-100 r/min, and the vacuum degree is 30-50 Pa; the heating temperature is 65-68 ℃.
Further, the short-time ultrasonic dispersion treatment conditions in the step (1) are as follows: the ultrasonic power is 120-160W, the ultrasonic frequency is 16-30 kHz, the ultrasonic treatment time is 8-10 min, and a circulation mode of ultrasonic dispersion for 90-120 s and stopping for 90-120 s is adopted.
Further, the short-time ultrasonic dispersion treatment conditions in the step (2) are as follows: the ultrasonic power is 100-120W, the ultrasonic frequency is 16-20 kHz, the ultrasonic treatment time is 8-10 min, and a circulation mode of ultrasonic dispersion for 60-90 s and stopping for 90-120 s is adopted.
The weight of the oil is the weight of the environment-friendly natural ester mixed insulating oil.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the invention, by adding the quantitative epoxidized insulating oil, the saturation of the natural ester mixed insulating oil is improved to a certain extent, and the oxidation resistance and the sensitivity to an antioxidant of the natural ester mixed insulating oil are effectively improved; on the basis, the antioxidant synergistic performance of the antioxidants is perfectly combined, the antioxidant performance of the natural ester mixed insulating oil is greatly improved, the tendency of forming oil sludge is reduced, and the problem of poor low-temperature fluidity caused by excessive addition of the epoxidized insulating oil is effectively avoided.
(2) The addition of the high-oleic-acid insulating oil improves the content of monounsaturated fatty acid in the natural ester mixed insulating oil, effectively improves the oxidation resistance and low-temperature fluidity of the natural ester mixed insulating oil, combines the excellent low-temperature characteristic and oxidation stability of the poly-alpha-olefin, and can effectively improve the low-temperature performance of the natural ester mixed insulating oil by being compounded with the pour point depressant.
(3) The strong vibration and stirring effect generated by the ultrasonic secondary effect can effectively improve the uniform dispersion degree of each component in the natural ester mixed insulating oil, and is more favorable for improving the oxidation resistance and low-temperature fluidity of the natural ester mixed insulating oil; by accurately controlling the ultrasonic dispersion power, frequency and time, the problems of additive failure caused by excessive ultrasonic dispersion energy and C produced by cracking of natural ester insulating oil can be effectively avoided2H6、C2H2And the performance is deteriorated due to the combustible organic gas and polar substances such as aldehyde and ketone.
(4) The natural ester mixed insulating oil prepared by the preparation method has excellent oxidation resistance and low temperature resistance, the pour point is less than-27.5 ℃, the total acid value after 48-hour oxidation stability test is less than 0.31mgKOH/g, the dielectric loss factor (90 ℃) is less than 8.1 percent, the performance stability is good, the technical advantage is obvious, and the application range of the natural ester insulating oil is effectively expanded.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited to the scope of the examples. These examples are intended to illustrate the invention only and are not intended to limit the scope of the invention.
Example 1
The low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance comprises an insulating oil mixture, zinc diamyldithiocarbamate accounting for 1.3 percent of the weight of the oil, antimony dialkyldithiocarbamate accounting for 1.3 percent of the weight of the oil, 4' -methylenebis (2, 6-di-tert-butylphenol) accounting for 0.7 percent of the weight of the oil, polymethacrylate accounting for 1.0 percent of the weight of the oil and poly-alpha-olefin accounting for 13 percent of the weight of the oil, wherein the insulating oil mixture comprises natural ester insulating oil, epoxidized insulating oil and high-oleic acid insulating oil which all use soybean oil as base oil according to the volume ratio of 5:1.5:3.5, the high-oleic acid insulating oil is refined by the high-oleic acid soybean oil, and the content of oleic acid reaches 72 percent.
The preparation method of the low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance comprises the following steps:
(1) respectively heating natural ester insulating oil, epoxidized insulating oil and high oleic acid insulating oil to 68 ℃ under the conditions of 100r/min and 50Pa, then performing vacuum dehydration, then mixing according to the volume ratio of 5:1.5:3.5, and performing short-time ultrasonic dispersion treatment by adopting a circulation mode of ultrasonic dispersion for 100s and stopping for 120s, wherein the ultrasonic power is 160W, the ultrasonic frequency is 22kHz, the ultrasonic treatment is 10min, and continuously stirring for 15min after the ultrasonic treatment is finished;
(2) and (2) sequentially adding zinc diamyldithiocarbamate, antimony dialkyldithiocarbamate, 4' -methylenebis (2, 6-di-tert-butylphenol), polymethacrylate and poly-alpha-olefin in corresponding weight ratios into the insulating oil mixture subjected to ultrasonic treatment in the step (1), performing short-time ultrasonic dispersion treatment again in a circulation mode of ultrasonic dispersion for 60s and stopping for 90s, wherein the ultrasonic power is 100W, the ultrasonic frequency is 20kHz, the ultrasonic treatment is performed for 10min, continuously stirring for 30min after the ultrasonic treatment is finished, and performing vacuum cooling to room temperature to obtain the low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance.
Example 2
The low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance is composed of an insulating oil mixture, zinc diamyldithiocarbamate accounting for 1.5 percent of the weight of the oil, antimony dialkyldithiocarbamate accounting for 1.2 percent of the weight of the oil, 4' -methylenebis (2, 6-di-tert-butylphenol) accounting for 0.5 percent of the weight of the oil, polymethacrylate accounting for 0.8 percent of the weight of the oil and poly-alpha-olefin accounting for 15 percent of the weight of the oil, wherein the insulating oil mixture is composed of natural ester insulating oil, epoxidized insulating oil and high-oleic acid insulating oil which all use soybean oil as base oil according to a volume ratio of 4:2:4, the high-oleic acid insulating oil is prepared by selectively hydrogenating and modifying the soybean oil, and the content of oleic acid reaches 78 percent.
The preparation method of the low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance comprises the following steps:
(1) respectively heating natural ester insulating oil, epoxidized insulating oil and high oleic acid insulating oil to 65 ℃ under the conditions of 80r/min and 35Pa, then performing vacuum dehydration, then mixing according to the volume ratio of 4:2:4, performing short-time ultrasonic dispersion treatment by adopting a circulation mode of ultrasonic dispersion for 120s and stopping for 120s, wherein the ultrasonic power is 160W, the ultrasonic frequency is 16kHz, the ultrasonic treatment is 8min, and continuously stirring for 18min after the ultrasonic treatment is finished;
(2) and (2) sequentially adding zinc diamyldithiocarbamate, antimony dialkyldithiocarbamate, 4' -methylenebis (2, 6-di-tert-butylphenol), polymethacrylate and poly-alpha-olefin in corresponding weight ratios into the insulating oil mixture subjected to ultrasonic treatment in the step (1), performing short-time ultrasonic dispersion treatment again in a circulation mode of ultrasonic dispersion for 90s and stopping for 120s, wherein the ultrasonic power is 120W, the ultrasonic frequency is 16kHz, the ultrasonic treatment is performed for 8min, continuously stirring for 25min after the ultrasonic treatment is finished, and performing vacuum cooling to room temperature to obtain the low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance.
Example 3
The low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance comprises an insulating oil mixture, zinc diamyldithiocarbamate accounting for 1.5 percent of the weight of the oil, antimony dialkyldithiocarbamate accounting for 1.1 percent of the weight of the oil, 4' -methylenebis (2, 6-di-tert-butylphenol) accounting for 0.7 percent of the weight of the oil, polymethacrylate accounting for 0.85 percent of the weight of the oil and poly-alpha-olefin accounting for 15 percent of the weight of the oil, wherein the insulating oil mixture comprises natural ester insulating oil, epoxidized insulating oil and high-oleic acid insulating oil which all use soybean oil as base oil according to the volume ratio of 4.5:1.5:4, the high-oleic acid insulating oil is refined by the high-oleic acid soybean oil, and the content of oleic acid reaches 72 percent.
The preparation method of the low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance comprises the following steps:
(1) respectively heating natural ester insulating oil, epoxidized insulating oil and high oleic acid insulating oil to 66 ℃ under the conditions of 100r/min and 30Pa, then performing vacuum dehydration, then mixing according to the volume ratio of 4.5:1.5:4, performing short-time ultrasonic dispersion treatment by adopting a circulation mode of ultrasonic dispersion for 90s and stopping for 90s, wherein the ultrasonic power is 120W, the ultrasonic frequency is 26kHz, the ultrasonic treatment is 10min, and continuously stirring for 15min after the ultrasonic treatment is finished;
(2) and (2) sequentially adding zinc diamyldithiocarbamate, antimony dialkyldithiocarbamate, 4' -methylenebis (2, 6-di-tert-butylphenol), polymethacrylate and poly-alpha-olefin in corresponding weight ratios into the insulating oil mixture subjected to ultrasonic treatment in the step (1), performing short-time ultrasonic dispersion treatment again in a circulation mode of ultrasonic dispersion for 75s and stopping for 90s, wherein the ultrasonic power is 120W, the ultrasonic frequency is 18kHz, the ultrasonic treatment is performed for 8min, continuously stirring for 30min after the ultrasonic treatment is finished, and performing vacuum cooling to room temperature to obtain the low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance.
Comparative example 1
A natural ester-based mixed insulating oil was prepared by removing epoxidized insulating oil from the components, and then mixing the other components and preparing the same as in example 1.
Comparative example 2
A natural ester blend insulating oil having a volume ratio of natural ester insulating oil, epoxidized insulating oil and high oleic acid insulating oil in the insulating oil blend of 3.5:3.5:3, the other ingredients and preparation were the same as in example 1.
Comparative example 3
A natural ester mixed insulating oil is prepared by removing high oleic acid insulating oil from the components, and the other components and preparation method are the same as example 2.
Comparative example 4
A natural ester-based mixed insulating oil was prepared in the same manner as in example 3 except that short-time ultrasonic dispersion treatment was not performed in steps (1) and (2).
The main performance parameters of the natural ester mixed insulating oils prepared in examples 1 to 3 of the present invention and comparative examples 1 to 4 are shown in tables 1 and 2.
As can be seen from the comparison of the data in tables 1 and 2, the oxidation resistance of the natural ester-based hybrid insulating oil is significantly reduced compared to that of example 1 after the epoxidized insulating oil component in the insulating oil mixture is removed in comparative example 1; comparative example 2 the proportion of the epoxidized insulating oil in the insulating oil mixture was increased to 35%, and although the natural ester-based mixed insulating oil had good oxidation resistance, its low temperature performance was deteriorated and its pour point could only reach-23.5 ℃; comparative example 3 after the high oleic acid insulating oil component in the insulating oil mixture was removed, the monounsaturated fatty acid content in the natural ester-based mixed insulating oil was reduced, and both the low temperature fluidity and the oxidation resistance were reduced; comparative example 4 in the preparation process, short-time ultrasonic dispersion treatment is not used, which affects the uniform dispersion degree of each component in the natural ester mixed insulating oil and is not beneficial to the improvement of the oxidation resistance and the low-temperature fluidity of the natural ester mixed insulating oil.
Table 1 main performance parameters of natural ester-based hybrid insulating oils prepared in examples 1-3
Table 2 main performance parameters of the natural ester-based hybrid insulating oils prepared in comparative examples 1 to 4
In conclusion, the comprehensive performance of the natural ester mixed insulating oil prepared in the embodiments 1 to 3 of the present invention is superior to that of the comparative examples 1 to 4, which shows that the composition of the component proportions of the natural ester mixed insulating oil and the preparation process parameters thereof directly affect the performance of the product, and the oxidation resistance and the low temperature fluidity of the natural ester mixed insulating oil are greatly improved by the precise blending of the component proportions and the precise control of the preparation parameters.
It should be noted that the above-mentioned embodiments are only detailed descriptions of the present invention, and are not intended to limit the protection scope of the present invention. Modifications and equivalents of the present invention may be made without departing from the spirit and scope of the invention and are intended to be covered by the appended claims.
Claims (8)
1. The low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance is characterized by comprising an insulating oil mixture, zinc diamyldithiocarbamate accounting for 1.3-1.5% of the weight of the oil, antimony dialkyldithiocarbamate accounting for 1.1-1.3% of the weight of the oil, 4' -methylenebis (2, 6-di-tert-butylphenol) accounting for 0.5-0.7% of the weight of the oil, polymethacrylate accounting for 0.8-1.0% of the weight of the oil and poly alpha olefin accounting for 12-15% of the weight of the oil.
2. The low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance as claimed in claim 1, wherein the insulating oil mixture is composed of a natural ester insulating oil, an epoxidized insulating oil and a high oleic acid insulating oil, all of which are based on soybean oil.
3. The low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance as claimed in claim 2, wherein the volume ratio of the natural ester insulating oil to the epoxidized insulating oil to the high oleic acid insulating oil is 4-5: 1.5-2: 3-4.
4. The low temperature resistant environment-friendly natural ester blended insulating oil with good oxidation resistance as claimed in claim 2 or 3, wherein the high oleic acid insulating oil is refined from high oleic acid soybean oil or is selectively hydrogenated and modified from soybean oil, and the oleic acid content in the obtained high oleic acid insulating oil is more than 70%.
5. A method for preparing the low temperature resistant environment friendly natural ester based blend insulating oil with good oxidation resistance as claimed in any one of claims 1 to 4, comprising the steps of:
(1) under stirring and vacuum conditions, heating natural ester insulating oil, epoxidized insulating oil and high oleic acid insulating oil respectively, then performing vacuum dehydration, mixing according to corresponding proportions, performing short-time ultrasonic dispersion treatment, and continuously stirring for 15-18 min;
(2) and (2) sequentially adding zinc diamyldithiocarbamate, antimony dialkyldithiocarbamate, 4' -methylenebis (2, 6-di-tert-butylphenol), polymethacrylate and poly-alpha-olefin in corresponding mass proportion into the insulating oil mixture subjected to ultrasonic treatment in the step (1), performing short-time ultrasonic dispersion treatment again, continuously stirring for 25-30 min, and then cooling the natural ester mixed insulating oil to room temperature in vacuum to obtain the product of the invention.
6. The preparation method of the low-temperature-resistant environment-friendly natural ester mixed insulating oil with good oxidation resistance as claimed in claim 5, wherein in the step (1), the stirring speed is 80-100 r/min, and the vacuum degree is 30-50 Pa; the heating temperature is 65-68 ℃.
7. The method for preparing the low temperature resistant environment-friendly natural ester blended insulating oil with good oxidation resistance as claimed in claim 5, wherein the short-time ultrasonic dispersion treatment conditions in the step (1) are as follows: the ultrasonic power is 120-160W, the ultrasonic frequency is 16-30 kHz, the ultrasonic treatment time is 8-10 min, and a circulation mode of ultrasonic dispersion for 90-120 s and stopping for 90-120 s is adopted.
8. The method for preparing the low temperature resistant environment-friendly natural ester blended insulating oil with good oxidation resistance as claimed in claim 5, wherein the short-time ultrasonic dispersion treatment conditions in the step (2) are as follows: the ultrasonic power is 100-120W, the ultrasonic frequency is 16-20 kHz, the ultrasonic treatment time is 8-10 min, and a circulation mode of ultrasonic dispersion for 60-90 s and stopping for 90-120 s is adopted.
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| CN116731773A (en) * | 2023-06-13 | 2023-09-12 | 上海江天高分子材料有限公司 | Degradable soybean-based natural ester insulating oil and preparation method and application thereof |
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