CN112542296B - Biodegradable high-ignition-point insulating fluid - Google Patents
Biodegradable high-ignition-point insulating fluid Download PDFInfo
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- CN112542296B CN112542296B CN202011414723.8A CN202011414723A CN112542296B CN 112542296 B CN112542296 B CN 112542296B CN 202011414723 A CN202011414723 A CN 202011414723A CN 112542296 B CN112542296 B CN 112542296B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F27/00—Details of transformers or inductances, in general
- H01F27/08—Cooling; Ventilating
- H01F27/10—Liquid cooling
- H01F27/12—Oil cooling
- H01F27/125—Cooling by synthetic insulating and incombustible liquid
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/20—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances liquids, e.g. oils
Abstract
The invention relates to a biodegradable high-ignition-point insulating fluid: ester compound A generated by ester exchange reaction of dibasic acid, polyhydric alcohol butyrate and small molecular organic acid under the action of ester exchange catalyst Q; ester compound B generated by ester exchange reaction of dibasic acid, polyol X alkyl butyrate and small molecular organic acid under the action of ester exchange catalyst Q; ester compound D is generated by ester exchange reaction of polyhydric alcohol butyrate and small molecular organic acid under the action of ester exchange catalyst Q; the ester compound E is generated by the ester exchange reaction of the polyhydric alcohol X alkyl butyrate and the small molecular organic acid under the action of the ester exchange catalyst Q; ester compound A, ester compound B, ester compound D and ester compound E are mixed, and antioxidant, pour point depressant and metal stabilizer are added. The invention has good compatibility, high ignition point, excellent heat conductivity and aging resistance, and meets the IEC61099 quality standard.
Description
Technical Field
The invention belongs to the technical field of insulating fluids, and relates to a biodegradable high-ignition-point insulating fluid.
Background
In the long-distance transmission process of high-voltage power and the electricity utilization process of cities, rural areas, industry and civil use, the transformer is indispensable equipment. The transformer generates heat in the distribution and conversion processes of electric energy, and in order to ensure the normal work of the transformer, the heat needs a good heat-conducting heat carrier to be transferred to the environment, and the heat carrier simultaneously has good insulating property.
Early electric power industry has widely used vegetable oils such as sunflower oil, rapeseed oil, tea tree oil, soybean oil, etc. as transformer oils. However, these vegetable oils are easily oxidized and have poor stability during use.
Mineral oil and synthetic silicone oil are also widely used for transformer oil from the economic aspect, but mineral oil and synthetic silicone oil have poor biodegradability and cause potential pollution to the environment.
Disclosure of Invention
Object of the Invention
In order to solve the problems of poor degradation capability, easy oxidation and poor stability in the prior art, the invention provides a biodegradable high-ignition-point insulating fluid suitable for a transformer. It is an ester compound, can be biologically degraded, and can also be recycled and refined for reuse.
Technical scheme
A biodegradable high fire point insulating fluid:
ester compound A generated by ester exchange reaction of dibasic acid, polyhydric alcohol butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
ester compound B generated by ester exchange reaction of dibasic acid, polyol X alkyl butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
ester compound D is generated by ester exchange reaction of polyhydric alcohol butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
the ester compound E is generated by the ester exchange reaction of the polyhydric alcohol X alkyl butyrate and the small molecular organic acid under the action of the ester exchange catalyst Q;
the ester compound A, the ester compound B, the ester compound D and the ester compound E are mixed according to a certain proportion, and an antioxidant, a pour point depressant and a metal stabilizer are added to form the biodegradable high-ignition-point insulating fluid.
Preferably, the dibasic acid comprises a mixture of one or both of glutaric acid and adipic acid; the polyhydric alcohol butyrate ester comprises pentaerythritol tetrabutyrate and pentaerythritol tetraisobutyrate, or a mixture of both; polyol X alkyl butyrate includes either or both of trimethylol X alkyl tri-n-butyrate and trimethylol X alkyl isobutyrate.
Preferably, the ester compound A comprises compound A1Or compound A2Or compound A1And a compound A2A mixture of (a);
the compound A1The structural formula of (A) is:
Z1and Z2May have the same molecular structural group or different molecular structural groups, Z1And Z2The structural formula of (A) is:
in the formula R1Has the structural formula C2To C12The linear alkyl or branched alkyl groups of (a), wherein the linear alkyl or branched alkyl groups may have the same molecular group, may have different molecular groups;
the compound A2The structural formula of (A) is:
Z3and Z4May have the same molecular structural group or different molecular structural groups, Z3And Z4The structural formula of (A) is:
wherein X is C1To C12Linear or branched alkyl of R1Has the structural formula C2To C12The linear alkyl group or the branched alkyl group of (2), wherein the linear alkyl group or the branched alkyl group may have the same molecular structural group or may have different molecular structural groups.
Preferably, the ester compound B comprises a compound B1Or compound B2Or compound B1And a compound B2A mixture of (a);
the ester compound B1The structural formula of (A) is:
wherein R is1Has the structural formula C2To C12Wherein the linear alkyl or branched alkyl groups may have the same molecular group or may have different molecular groups;
the ester compound B2The structural formula of (A) is:
wherein X is C1To C12Linear or branched alkyl of R1Has the structural formula C2To C12The linear alkyl group or the branched alkyl group of (1), wherein the linear alkyl group or the branched alkyl group may have a molecular group of the same structure or may have a group of a different molecular structure.
Preferably, the transesterification catalyst Q is prepared by reacting stannous oxalate with dimethyl glutarate or dimethyl adipate or a mixture of dimethyl glutarate and dimethyl adipate in a molar ratio of 1:2 to 1:10 at a temperature of 80-200 ℃ and a vacuum pressure of 200-20mmHg for 3-5 hours, evaporating a side reaction product dimethyl oxalate, cooling to room temperature to obtain a uniform suspension liquid catalyst Q containing stannous glutarate and dimethyl glutarate or a uniform suspension liquid catalyst Q containing stannous adipate and dimethyl adipate, or a uniform suspension liquid catalyst Q containing stannous glutarate and dimethyl glutarate plus a uniform suspension liquid catalyst Q containing stannous adipate and dimethyl adipate, wherein the molecular structural formula of the transesterification catalyst Q is as follows:
Preferably, the preparation reaction of the ester compound A is carried out by the steps of enabling the molar ratio of the needed dibasic acid, the small molecular organic acid and the polyhydric alcohol butyrate to be (0.01-0.3) - (3-4) - (1-2), enabling the reaction temperature to be 100-;
the preparation reaction of the ester compound B is carried out by the molar ratio of the dibasic acid, the micromolecular organic acid and the polyol X alkyl butyrate being (0.01-0.3) to (3-4) to (1-2), the reaction temperature being 100-260 ℃, the vacuum degree being 300-20mmHg, the reaction time being 3-6 hours, evaporating off the by-product butyric acid generated in the reaction, cooling the reaction product to room temperature, filtering to remove the ester exchange catalyst Q, obtaining the esterification reaction product B, wherein the filling proportion of the ester exchange catalyst Q in the reaction process is 5-1 ten thousandths of the total mass of the reaction mixture of the dibasic acid, the micromolecular organic acid and the polyol X alkyl butyrate;
the preparation reaction of the ester compound D is carried out by the steps of enabling the molar ratio of the small molecular organic acid to the polyhydric alcohol butyrate to be (3-4) to (1-2), enabling the reaction temperature to be 100-200 ℃ and the vacuum degree to be 300-20mmHg, reacting for 3-6 hours, evaporating out by-product butyric acid generated in the reaction, cooling the reactant to room temperature, filtering to remove the ester exchange catalyst Q, and obtaining an esterification reaction product D, wherein the addition proportion of the ester exchange catalyst Q in the reaction process is 5-1 ten thousand parts of the total mass of the reaction mixture of the small molecular organic acid and the polyhydric alcohol butyrate;
the preparation reaction of the ester compound E is carried out by the steps of enabling the molar ratio of the small molecular organic acid to the polyol X alkyl butyrate to be (2-4) to (1-2), enabling the reaction temperature to be 100-200 ℃, enabling the vacuum degree to be 300-20mmHg, reacting for 3-6 hours, evaporating out by-product butyric acid generated in the reaction, cooling reactants to room temperature, filtering to remove ester exchange catalyst Q, and obtaining esterification reaction product E, wherein the adding proportion of the ester exchange catalyst Q in the reaction process is 5-1 ten thousand of the total mass of the reaction mixture of the small molecular organic acid and the polyol X alkyl butyrate.
Preferably, the antioxidant is a 2-alkyl imidazoline compound, and the structural formula of the 2-alkyl imidazoline compound is as follows:
wherein R is C9To C17The antioxidant accounts for 0.01 to 0.5 percent of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E.
Preferably, the antioxidant can also be one or a mixture of two or more of dodecyl dihydroxy benzene, dodecyl catechol, hydroquinone, naphthol, phenyl-naphthylamine, diphenylamine and diphenyl sulfide, and the antioxidant mass accounts for 0.01-0.5% of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E;
the metal stabilizer is one or a mixture of two or more of 2-alkyl imidazoline compound, dodecyl benzene triazole, triazole and dimercapto thiadiazole, and the mass of the metal stabilizer accounts for 0.01-0.5% of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E;
the pour point depressant is polymethyl methacrylate high-carbon alcohol ester, average addition number (average polymerization degree)
Preferably, the small-molecule organic acid is C2To C13Linear or branched alkyl organic acids of the general formula
R is C1To C12A linear or branched alkyl group of (a);
the structural formula of the polyol X alkyl butyrate is as follows:
wherein X is C1To C12Straight chain alkyl ofBranched alkyl radical, R3The molecular structural group of (A) is an n-propyl group or the molecular structural group of R3 is an isopropyl group.
Preferably, the ester compound A, the ester compound B, the ester compound D and the ester compound E respectively account for 2% -90%, 2% -90% and 2% -90% of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E.
Advantages and effects
The biodegradable high-ignition-point insulating fluid disclosed by the invention is an ester compound synthesized by adopting dibasic acid, polyol butyrate, small-molecular organic acid and polyol X alkyl butyrate, and simultaneously the antioxidant pour point depressant and the metal stabilizer are added, so that the compatibility is good, the ignition point is high, the heat conductivity is excellent, and the aging resistance is high.
The transformer oil provided by the invention is detected according to IEC61099 quality indexes, and all the quality indexes meet the standard and meet the market requirements.
Detailed Description
A biodegradable high fire point insulating fluid:
ester compound A generated by ester exchange reaction of dibasic acid, polyhydric alcohol butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
ester compound B generated by ester exchange reaction of dibasic acid, polyol X alkyl butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
ester compound D is generated by ester exchange reaction of polyhydric alcohol butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
the ester compound E is generated by the ester exchange reaction of the polyhydric alcohol X alkyl butyrate and the small molecular organic acid under the action of the ester exchange catalyst Q;
ester compound A, ester compound B, ester compound D and ester compound E are mixed, and ester compound A, ester compound B, ester compound D and ester compound E respectively account for 2% -90%, 2% -90% and 2% of the total mass of the mixture of ester compound A, ester compound B, ester compound D and ester compound E90 percent to 2 percent to 90 percent, adding an antioxidant, a pour point depressant and a metal stabilizer to form a biodegradable high-ignition-point insulating fluid, wherein the ignition point of the biodegradable high-ignition-point insulating fluid is more than or equal to 300 ℃, and the viscosity of the biodegradable high-ignition-point insulating fluid is less than 23mm at 40 DEG C2(vii)/S for a dielectric insulating liquid for transformers.
The dibasic acid comprises one or a mixture of glutaric acid and adipic acid; the polyhydric alcohol butyrate ester comprises pentaerythritol tetrabutyrate and pentaerythritol tetraisobutyrate, or a mixture of both; polyol X alkyl butyrate includes either or both of trimethylol X alkyl tri-n-butyrate and trimethylol X alkyl isobutyrate.
The ester compound A comprises a compound A1Or compound A2Or compound A1And a compound A2A mixture of (a);
compound A1The structural formula of (A) is:
Z1and Z2May have the same molecular structural group or different molecular structural groups, Z1And Z2The structural formula of (A) is:
in the formula R1Has the structural formula C2To C12The linear alkyl or branched alkyl groups of (a), wherein the linear alkyl or branched alkyl groups may have the same molecular group, may have different molecular groups;
compound A2The structural formula of (A) is:
Z3and Z4Can have the same molecular structural group or different molecular structural groups,Z3and Z4The structural formula of (A) is:
wherein X is C1To C12Linear or branched alkyl of R1Has the structural formula C2To C12The linear alkyl group or the branched alkyl group of (2), wherein the linear alkyl group or the branched alkyl group may have the same molecular structural group or may have different molecular structural groups.
The ester compound B comprises a compound B1Or compound B2Or compound B1And a compound B2A mixture of (a);
ester compound B1The structural formula of (A) is:
wherein R is1Has the structural formula C2To C12Wherein the linear alkyl or branched alkyl groups may have the same molecular group or may have different molecular groups;
ester compound B2The structural formula of (A) is:
wherein X is C1To C12Linear or branched alkyl of R1Has the structural formula C2To C12The linear alkyl group or the branched alkyl group of (1), wherein the linear alkyl group or the branched alkyl group may have a molecular group of the same structure or may have a group of a different molecular structure.
The ester exchange catalyst Q is prepared by reacting stannous oxalate with dimethyl glutarate or dimethyl adipate or a mixture of dimethyl glutarate and dimethyl adipate in a molar ratio of 1:2 to 1:10 at the temperature of 80-200 ℃ and the vacuum pressure of 200-20mmHg for 3-5 hours, evaporating a side reaction product dimethyl oxalate, cooling to room temperature to obtain a uniform suspension liquid catalyst Q containing stannous glutarate and dimethyl glutarate or a uniform suspension liquid catalyst Q containing stannous adipate and dimethyl adipate, or a uniform suspension liquid catalyst Q containing stannous glutarate and dimethyl glutarate plus a uniform suspension liquid catalyst Q containing stannous adipate and dimethyl adipate, wherein the molecular structural formula of the ester exchange catalyst Q is as follows:
The preparation reaction of the ester compound A comprises the steps of distilling off a by-product butyric acid generated in the reaction at the reaction temperature of 100-;
the preparation reaction of the ester compound B comprises the steps of enabling the molar ratio of the needed dibasic acid, the small molecular organic acid and the polyol X alkyl butyrate to be (0.01-0.3) - (3-4) - (1-2), enabling the reaction temperature to be 100-;
the preparation reaction of the ester compound D is carried out by the steps of reacting for 3-6 hours at 100-200 ℃ and 300-20mmHg for 3-4 mol ratio of the small molecular organic acid and the polyhydric alcohol butyrate, evaporating by-product butyric acid generated by the reaction, cooling the reactant to room temperature, filtering to remove ester exchange catalyst Q, and obtaining esterification reaction product D, wherein the addition ratio of the ester exchange catalyst Q is 5-1 ten thousandth of the total mass of the reaction mixture of the small molecular organic acid and the polyhydric alcohol butyrate in the reaction process;
the ester compound E is prepared by the steps of enabling the molar ratio of the needed small molecular organic acid to the polyol X alkyl butyrate to be (2-4) - (1-2), enabling the reaction temperature to be 100-200 ℃ and the vacuum degree to be 300-20mmHg, reacting for 3-6 hours, evaporating out the by-product butyric acid generated in the reaction, cooling the reactant to room temperature, filtering and removing the ester exchange catalyst Q to obtain the esterification reaction product E, wherein the addition proportion of the ester exchange catalyst Q in the reaction process is 5-1 ten thousand of the total mass of the reaction mixture of the small molecular organic acid and the polyol X alkyl butyrate.
The antioxidant is a 2-alkyl imidazoline compound, and the structural formula of the 2-alkyl imidazoline compound is as follows:
wherein R is C9To C17The antioxidant accounts for 0.01 to 0.5 percent of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E.
The antioxidant is one or a mixture of two or more of dodecyl dihydroxy benzene, dodecyl catechol, hydroquinone, naphthol, phenyl-naphthylamine, diphenylamine and diphenyl sulfide, and the antioxidant accounts for 0.01-0.5 percent of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E; the metal stabilizer is one or a mixture of two or more of 2-alkyl imidazoline compound, dodecyl benzene triazole, triazole and dimercapto thiadiazole, and the mass of the metal stabilizer accounts for 0.01-0.5% of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E;
the pour point depressant is commercially available poly (high carbon alcohol) methacrylate, and the average addition number (average polymerization degree)
The small molecular organic acid is C2To C13Linear or branched alkyl organic acids of the general formula
R is C1To C12Linear or branched alkyl groups of (a).
The structural formula of the polyol X alkyl butyrate is as follows:
wherein X is C1To C12Linear or branched alkyl of R3The molecular structural group of (A) is an n-propyl group or the molecular structural group of R3 is an isopropyl group.
Example 1
A biodegradable high fire point insulating fluid:
the preparation reaction of the ester compound A comprises the steps of distilling off by-product butyric acid generated by the reaction at the molar ratio of 0.01:3:1 of dibasic acid, micromolecular organic acid and polyhydric alcohol butyrate, wherein the reaction temperature is 200 ℃, the vacuum degree is 180mmHg, the reaction time is 5 hours, the reaction product is cooled to room temperature, and the ester exchange catalyst Q is filtered to remove, so as to obtain the esterification reaction product A, wherein the addition proportion of the ester exchange catalyst Q in the reaction process is 0.1 percent of the total mass of the reaction mixture of the dibasic acid, the micromolecular organic acid and the polyhydric alcohol butyrate;
the preparation reaction of the ester compound B comprises the steps of distilling off by-product butyric acid generated by the reaction at the molar ratio of 0.01:3:1 of dibasic acid, micromolecular organic acid and polyhydric alcohol X alkyl butyrate, wherein the reaction temperature is 200 ℃, the vacuum degree is 180mmHg, the reaction time is 5 hours, the reaction product is cooled to room temperature, and the ester exchange catalyst Q is filtered to remove, so as to obtain the esterification reaction product B, wherein the addition proportion of the ester exchange catalyst Q in the reaction process is 0.1 percent of the total mass of the reaction mixture of the dibasic acid, the micromolecular organic acid and the polyhydric alcohol X alkyl butyrate;
the preparation reaction of the ester compound D is carried out by the steps of enabling the molar ratio of the needed small molecular organic acid to the needed polyhydric alcohol butyrate to be 2:1, enabling the reaction temperature to be 150 ℃ and the vacuum degree to be 150mmHg, reacting for 5 hours, evaporating out by-product butyric acid generated in the reaction, cooling reactants to room temperature, filtering to remove ester exchange catalyst Q, and obtaining an esterification reaction product D, wherein the addition ratio of the ester exchange catalyst Q in the reaction process is 0.1% of the total mass of the reaction mixture of the small molecular organic acid and the polyhydric alcohol butyrate;
the ester compound E is prepared by the steps of reacting a required micromolecular organic acid with a polyalcohol X alkyl butyrate according to the mol ratio of 4:1 at the reaction temperature of 150 ℃ and the vacuum degree of 180mmHg for 5 hours, evaporating by-product butyric acid generated in the reaction, cooling reactants to room temperature, and filtering to remove an ester exchange catalyst Q to obtain an esterification reaction product E, wherein the addition ratio of the ester exchange catalyst Q in the reaction process is 0.1 percent of the total mass of the reaction mixture of the micromolecular organic acid and the polyalcohol X alkyl butyrate.
The ester exchange catalyst Q is a uniform suspension liquid catalyst Q containing stannous glutarate and dimethyl glutarate obtained by reacting stannous oxalate with dimethyl glutarate at 140 ℃ and vacuum pressure of 120mmHg in a molar ratio of 1:5 for 4 hours, evaporating out the dimethyl oxalate as a side reaction product, and cooling to room temperature.
Ester compound A generated by ester exchange reaction of dibasic acid, polyhydric alcohol butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
ester compound B generated by ester exchange reaction of dibasic acid, polyol X alkyl butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
ester compound D is generated by ester exchange reaction of polyhydric alcohol butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
the ester compound E is generated by the ester exchange reaction of the polyhydric alcohol X alkyl butyrate and the small molecular organic acid under the action of the ester exchange catalyst Q;
ester compound A,Ester compound B, ester compound D and ester compound E are mixed, the ester compound A, ester compound B, ester compound D and ester compound E respectively account for 2%, 6% and 90% of the total mass of the mixture of ester compound A, ester compound B, ester compound D and ester compound E, antioxidant, pour point depressant and metal stabilizer are added to form biodegradable high-ignition-point insulating fluid, and the ignition point of the biodegradable high-ignition-point insulating fluid is that of the biodegradable high-ignition-point insulating fluid>Viscosity at 300 deg.C and 40 deg.C is less than 23mm2(vii)/S for a dielectric insulating liquid for transformers. The mass of the antioxidant accounts for 0.2 percent of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E.
The mass of the metal stabilizer accounts for 0.2 percent of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E;
average sum of pour point depressants (average degree of polymerization)
The mass of the pour point depressant accounts for 0.03 percent of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E.
The insulating fluid index is detected:
physical properties: color 153HU, clear appearance, volume at 20 ℃ 0.9685g/m3Kinematic viscosity at 40 ℃ of 31.3mm2(s) a kinematic viscosity at-20 ℃ of 690mm2The temperature of the material is controlled by the following formula I, wherein the temperature is 295 ℃, the flash point is 309 ℃, no crystal exists, and the pour point is-50 ℃;
chemical characteristics: the water content is 120mg/kg, the neutralization value is 0.02mgKOH/g, the total acid content is 0.2mgKOH/g, and the total sediment mass accounts for 0.005 percent;
electrical characteristics: breakdown voltage 60kV, dielectric loss factor 0.023 at 90 ℃/50Hz, and DC resistance 6 ohm at 90 ℃.
Example 2
A biodegradable high fire point insulating fluid:
the preparation reaction of the ester compound A comprises the steps of distilling off by-product butyric acid generated in the reaction when the molar ratio of the needed dibasic acid, the small molecular organic acid and the polyol butyrate is 0.1:3.5:2, the reaction temperature is 100 ℃, the vacuum degree is 300mmHg, the reaction time is 3 hours, cooling the reaction product to room temperature, and filtering to remove the ester exchange catalyst Q to obtain an esterification reaction product A, wherein the addition proportion of the ester exchange catalyst Q in the reaction process is 5 ten-thousandth of the total mass of the reaction mixture of the dibasic acid, the small molecular organic acid and the polyol butyrate;
the preparation reaction of the ester compound B is that the molar ratio of the needed dibasic acid, the small molecular organic acid and the polyol X alkyl butyrate is 0.1:3.5:2, the reaction temperature is 100 ℃, the vacuum degree is 300mmHg, the reaction time is 3-6 hours, the by-product butyric acid generated by the reaction is evaporated, the reaction product is cooled to room temperature, the ester exchange catalyst Q is filtered to remove, and the esterification reaction product B is obtained, wherein the addition proportion of the ester exchange catalyst Q in the reaction process is 5 ten-thousandth of the total mass of the reaction mixture of the dibasic acid, the small molecular organic acid and the polyol X alkyl butyrate;
the preparation reaction of the ester compound D is carried out by the steps of reacting for 3 hours at 200 ℃ and 300mmHg for 4:1 molar ratio of the needed micromolecular organic acid to the polyhydric alcohol butyrate, evaporating out by-product butyric acid generated in the reaction, cooling the reactant to room temperature, filtering to remove ester exchange catalyst Q to obtain esterification reaction product D, wherein the addition ratio of the ester exchange catalyst Q is 5 ten-thousandth of the total mass of the reaction mixture of the micromolecular organic acid and the polyhydric alcohol butyrate in the reaction process;
the ester compound E is prepared by the steps of enabling the molar ratio of the needed small molecular organic acid to the polyol X alkyl butyrate to be 1:1, enabling the reaction temperature to be 100 ℃, enabling the vacuum degree to be 300mmHg, reacting for 3 hours, evaporating out by-product butyric acid generated in the reaction, cooling reactants to room temperature, and filtering to remove the ester exchange catalyst Q to obtain an esterification reaction product E, wherein the addition ratio of the ester exchange catalyst Q in the reaction process is 5 ten-thousandth of the total mass of the reaction mixture of the small molecular organic acid and the polyol X alkyl butyrate.
The ester exchange catalyst Q is a uniform suspension liquid catalyst Q containing stannous adipate and dimethyl adipate, which is obtained by reacting stannous oxalate with dimethyl adipate in a molar ratio of 1:2 for 3 hours at the temperature of 80 ℃ and the vacuum pressure of 200mmHg, evaporating a side reaction product dimethyl oxalate, and cooling to room temperature.
Ester compound A generated by ester exchange reaction of dibasic acid, polyhydric alcohol butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
ester compound B generated by ester exchange reaction of dibasic acid, polyol X alkyl butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
ester compound D is generated by ester exchange reaction of polyhydric alcohol butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
the ester compound E is generated by the ester exchange reaction of the polyhydric alcohol X alkyl butyrate and the small molecular organic acid under the action of the ester exchange catalyst Q;
ester compound A, ester compound B, ester compound D and ester compound E are mixed, the ester compound A, ester compound B, ester compound D and ester compound E respectively account for 10%, 20%, 30% and 40% of the total mass of the mixture of ester compound A, ester compound B, ester compound D and ester compound E, antioxidant, pour point depressant and metal stabilizer are added to form biodegradable high-ignition-point insulating fluid, and the ignition point of the biodegradable high-ignition-point insulating fluid is that of the biodegradable high-ignition-point insulating fluid>Viscosity at 300 deg.C and 40 deg.C is less than 23mm2(vii)/S for a dielectric insulating liquid for transformers.
The mass of the antioxidant accounts for 0.01 percent of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E.
The mass of the metal stabilizer accounts for 0.01 percent of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E;
average sum of pour point depressants (average degree of polymerization)
The mass of the pour point depressant accounts for 0.01 percent of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E.
The insulating fluid index is detected:
physical properties: color 155HU, clear appearance, volume 0.9650g/m at 20 ℃3Kinematic viscosity at 40 ℃ of 31.8mm2(s) kinematic viscosity at-20 ℃ of 700mm2The temperature is 290 ℃ in ignition point, 310 ℃ in flash point, no crystal and 50 ℃ below zero in pour point;
chemical characteristics: the water content is 120mg/kg, the neutralization value is 0.02mgKOH/g, the total acid content is 0.2mgKOH/g, and the total sediment mass accounts for 0.004 percent;
electrical characteristics: breakdown voltage 60kV, dielectric loss tangent 0.022 at 90 ℃/50Hz, and DC resistance 6.2 ohm at 90 ℃.
Example 3
A biodegradable high fire point insulating fluid:
the preparation reaction of the ester compound A comprises the steps of distilling off by-product butyric acid generated by the reaction at the molar ratio of 0.3:4:1 of dibasic acid, micromolecular organic acid and polyhydric alcohol butyrate, at the reaction temperature of 260 ℃ and the vacuum degree of 20mmHg for 6 hours, cooling the reaction product to room temperature, and filtering to remove the ester exchange catalyst Q to obtain an esterification reaction product A, wherein the addition proportion of the ester exchange catalyst Q in the reaction process is 1 percent of the total mass of the reaction mixture of the dibasic acid, the micromolecular organic acid and the polyhydric alcohol butyrate;
the preparation reaction of the ester compound B is that the mole ratio of the needed dibasic acid, the small molecular organic acid and the polyol X alkyl butyrate is 0.3:4:1, the reaction temperature is 260 ℃, the vacuum degree is 20mmHg, the reaction time is 6 hours, the by-product butyric acid generated by the reaction is evaporated, the reaction product is cooled to room temperature, the ester exchange catalyst Q is filtered to remove, and the esterification reaction product B is obtained, wherein the adding proportion of the ester exchange catalyst Q in the reaction process is 1 percent of the total mass of the reaction mixture of the dibasic acid, the small molecular organic acid and the polyol X alkyl butyrate;
the preparation reaction of the ester compound D is carried out by the steps of distilling off by-product butyric acid generated in the reaction when the molar ratio of the small molecular organic acid to the polyhydric alcohol butyrate is 3:2, the reaction temperature is 100 ℃, the vacuum degree is 20mmHg and reacting for 6 hours, cooling the reactant to room temperature, and filtering to remove the ester exchange catalyst Q to obtain an esterification reaction product D, wherein the addition ratio of the ester exchange catalyst Q is 1 percent of the total mass of the reaction mixture of the small molecular organic acid and the polyhydric alcohol butyrate in the reaction process;
the ester compound E is prepared by the steps of enabling the molar ratio of the needed small molecular organic acid to the polyol X alkyl butyrate to be 2:1, enabling the reaction temperature to be 200 ℃, enabling the vacuum degree to be 20mmHg, reacting for 6 hours, evaporating out by-product butyric acid generated in the reaction, cooling reactants to room temperature, and filtering to remove the ester exchange catalyst Q to obtain an esterification reaction product E, wherein the addition ratio of the ester exchange catalyst Q in the reaction process is 1% of the total mass of the reaction mixture of the small molecular organic acid and the polyol X alkyl butyrate.
The ester exchange catalyst Q is prepared by reacting stannous oxalate with a mixture of dimethyl glutarate and dimethyl adipate in a molar ratio of 1:10 at 200 ℃ and a vacuum pressure of 20mmHg for 5 hours, evaporating out a side reaction product dimethyl oxalate, and cooling to room temperature to obtain a uniform suspension liquid catalyst Q containing stannous glutarate and dimethyl glutarate and a uniform suspension liquid catalyst Q containing stannous adipate and dimethyl adipate. Ester compound A generated by ester exchange reaction of dibasic acid, polyhydric alcohol butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
ester compound B generated by ester exchange reaction of dibasic acid, polyol X alkyl butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
ester compound D is generated by ester exchange reaction of polyhydric alcohol butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
the ester compound E is generated by the ester exchange reaction of the polyhydric alcohol X alkyl butyrate and the small molecular organic acid under the action of the ester exchange catalyst Q;
ester compound A, ester compound B, ester compound D and ester compound E are mixed, the ester compound A, ester compound B, ester compound D and ester compound E respectively account for 90%, 4%, 2% and 4% of the total mass of the mixture of ester compound A, ester compound B, ester compound D and ester compound E, antioxidant, pour point depressant and metal stabilizer are added to form biodegradable high-ignition-point insulating fluid, and the ignition point of the biodegradable high-ignition-point insulating fluid is that of the biodegradable high-ignition-point insulating fluid>Viscosity at 300 deg.C and 40 deg.C is less than 23mm2(vii)/S for a dielectric insulating liquid for transformers. The mass of the antioxidant accounts for the ester compound A and the ester0.5 percent of the total mass of the mixture of the ester compound B, the ester compound D and the ester compound E.
The mass of the metal stabilizer accounts for 0.5 percent of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E;
average sum of pour point depressants (average degree of polymerization)
The mass of the pour point depressant accounts for 0.05 percent of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E.
The insulating fluid index is detected:
physical properties: color 154HU, clear appearance, volume at 20 ℃ 0.9622g/m3Kinematic viscosity at 40 ℃ of 31.5mm2The kinematic viscosity at-20 ℃ is 695mm2The temperature is higher than that of the molten steel, and the temperature is lower than that of the molten steel, wherein the burning point is 297 ℃, the flash point is 306 ℃, and the molten steel is free of crystals and has a pour point of-50 ℃;
chemical characteristics: the water content is 121mg/kg, the neutralization value is 0.02mgKOH/g, the total acid content is 0.2mgKOH/g, and the total sediment mass accounts for 0.006%;
electrical characteristics: breakdown voltage 62kV, dielectric loss factor 0.024 at 90 deg.C/50 Hz, and DC resistance 6.1 ohm at 90 deg.C.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that various changes and modifications can be made on the basis of the above description, and all embodiments cannot be exhaustive, and obvious changes and modifications included in the technical solutions of the present invention are within the scope of the present invention.
Claims (8)
1. A biodegradable high ignition point insulating fluid characterized by:
ester compound A generated by ester exchange reaction of dibasic acid, polyhydric alcohol butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
ester compound B generated by ester exchange reaction of dibasic acid, polyol X alkyl butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
ester compound D is generated by ester exchange reaction of polyhydric alcohol butyrate and small molecular organic acid under the action of ester exchange catalyst Q;
the ester compound E is generated by the ester exchange reaction of the polyhydric alcohol X alkyl butyrate and the small molecular organic acid under the action of the ester exchange catalyst Q;
ester compound A, ester compound B, ester compound D and ester compound E are mixed according to a certain proportion, and antioxidant, pour point depressant and metal stabilizer are added to form biodegradable high-ignition-point insulating fluid;
the ester compound A, the ester compound B, the ester compound D and the ester compound E respectively account for 2% -90%, 2% -90% and 2% -90% of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E;
the dibasic acid comprises one or a mixture of glutaric acid and adipic acid; the polyhydric alcohol butyrate ester comprises pentaerythritol tetrabutyrate and pentaerythritol tetraisobutyrate, or a mixture of both; polyol X alkyl butyrate includes either or both of trimethylol X alkyl tri-n-butyrate and trimethylol X alkyl isobutyrate.
2. The biodegradable high fire point insulating fluid of claim 1, wherein: the ester compound A comprises a compound A1Or compound A2Or compound A1And a compound A2A mixture of (a); the compound A1The structural formula of (A) is:
Z1and Z2May have the same molecular structural group or different molecular structural groups, Z1And Z2The structural formula of (A) is:
in the formula R1Has the structural formula C2To C12The linear alkyl or branched alkyl groups of (a), wherein the linear alkyl or branched alkyl groups may have the same molecular group, may have different molecular groups;
the compound A2The structural formula of (A) is:
Z3and Z4May have the same molecular structural group or different molecular structural groups, Z3And Z4The structural formula of (A) is:
wherein X is C1To C12Linear or branched alkyl of R1Has the structural formula C2To C12The linear alkyl group or the branched alkyl group of (2), wherein the linear alkyl group or the branched alkyl group may have the same molecular structural group or may have different molecular structural groups.
3. The biodegradable high fire point insulating fluid of claim 1, wherein: the ester compound B comprises a compound B1Or compound B2Or compound B1And a compound B2A mixture of (a);
the ester compound B1The structural formula of (A) is:
wherein R is1Has the structural formula C2To C12Wherein the linear alkyl or branched alkyl groups may have the same molecular group or may have different molecular groups;
the ester compound B2The structural formula of (A) is:
wherein X is C1To C12Linear or branched alkyl of R1Has the structural formula C2To C12The linear alkyl group or the branched alkyl group of (1), wherein the linear alkyl group or the branched alkyl group may have a molecular group of the same structure or may have a group of a different molecular structure.
4. The biodegradable high fire point insulating fluid of claim 1, wherein: the ester exchange catalyst Q is prepared by reacting stannous oxalate with dimethyl glutarate or dimethyl adipate or a mixture of dimethyl glutarate and dimethyl adipate in a molar ratio of 1:2 to 1:10 at the temperature of 80-200 ℃ and the vacuum pressure of 200-20mmHg for 3-5 hours, evaporating a side reaction product dimethyl oxalate, cooling to room temperature to obtain a uniform suspension liquid catalyst Q containing stannous glutarate and dimethyl glutarate, or a uniform suspension liquid catalyst Q containing stannous adipate and dimethyl adipate, or a uniform suspension liquid catalyst Q containing stannous glutarate and dimethyl glutarate plus a uniform suspension liquid catalyst Q containing stannous adipate and dimethyl adipate, wherein the molecular structural formula of the ester exchange catalyst Q is as follows:
5. The biodegradable high fire point insulating fluid of claim 1, wherein: the preparation reaction of the ester compound A is carried out by the steps of enabling the molar ratio of the needed dibasic acid, the small molecular organic acid and the polyol butyrate to be (0.01-0.3) - (3-4) - (1-2), enabling the reaction temperature to be 100-260 ℃, enabling the vacuum degree to be 300-20mmHg, enabling the reaction time to be 3-6 hours, evaporating out by-product butyric acid generated in the reaction, cooling the reaction product to room temperature, and filtering to remove the ester exchange catalyst Q to obtain the esterification reaction product A, wherein the filling proportion of the ester exchange catalyst Q in the reaction process is 5-1 ten thousandths of the total mass of the reaction mixture of the dibasic acid, the small molecular organic acid and the polyol butyrate;
the preparation reaction of the ester compound B is carried out by the molar ratio of the dibasic acid, the micromolecular organic acid and the polyol X alkyl butyrate being (0.01-0.3) to (3-4) to (1-2), the reaction temperature being 100-260 ℃, the vacuum degree being 300-20mmHg, the reaction time being 3-6 hours, evaporating off the by-product butyric acid generated in the reaction, cooling the reaction product to room temperature, filtering to remove the ester exchange catalyst Q, obtaining the esterification reaction product B, wherein the filling proportion of the ester exchange catalyst Q in the reaction process is 5-1 ten thousandths of the total mass of the reaction mixture of the dibasic acid, the micromolecular organic acid and the polyol X alkyl butyrate;
the preparation reaction of the ester compound D is carried out by the steps of enabling the molar ratio of the small molecular organic acid to the polyhydric alcohol butyrate to be (3-4) to (1-2), enabling the reaction temperature to be 100-200 ℃ and the vacuum degree to be 300-20mmHg, reacting for 3-6 hours, evaporating out by-product butyric acid generated in the reaction, cooling the reactant to room temperature, filtering to remove the ester exchange catalyst Q, and obtaining an esterification reaction product D, wherein the addition proportion of the ester exchange catalyst Q in the reaction process is 5-1 ten thousand parts of the total mass of the reaction mixture of the small molecular organic acid and the polyhydric alcohol butyrate;
the preparation reaction of the ester compound E is carried out by the steps of enabling the molar ratio of the small molecular organic acid to the polyol X alkyl butyrate to be (2-4) to (1-2), enabling the reaction temperature to be 100-200 ℃, enabling the vacuum degree to be 300-20mmHg, reacting for 3-6 hours, evaporating out by-product butyric acid generated in the reaction, cooling reactants to room temperature, filtering to remove ester exchange catalyst Q, and obtaining esterification reaction product E, wherein the adding proportion of the ester exchange catalyst Q in the reaction process is 5-1 ten thousand of the total mass of the reaction mixture of the small molecular organic acid and the polyol X alkyl butyrate.
6. The biodegradable high fire point insulating fluid of claim 1, wherein: the antioxidant is a 2-alkyl imidazoline compound, and the structural formula of the 2-alkyl imidazoline compound is as follows:
wherein R is C9To C17The antioxidant accounts for 0.01 to 0.5 percent of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E.
7. The biodegradable high fire point insulating fluid of claim 1, wherein: the antioxidant is one or a mixture of two or more of dodecyl dihydroxy benzene, dodecyl catechol, hydroquinone, naphthol, phenyl-naphthylamine, diphenylamine and diphenyl sulfide, and the antioxidant accounts for 0.01-0.5 percent of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E;
the metal stabilizer is one or a mixture of two or more of 2-alkyl imidazoline compound, dodecyl benzene triazole, triazole and dimercapto thiadiazole, and the mass of the metal stabilizer accounts for 0.01-0.5% of the total mass of the mixture of the ester compound A, the ester compound B, the ester compound D and the ester compound E;
the pour point depressant is polymethyl methacrylate high-carbon alcohol ester, average addition number (average polymerization degree)
8. According to claim1 the biodegradable high ignition point type insulating fluid is characterized in that: the small molecular organic acid is C2To C13Linear or branched alkyl organic acids of the general formula
R is C1To C12A linear or branched alkyl group of (a);
the structural formula of the polyol X alkyl butyrate is as follows:
wherein X is C1To C12Linear or branched alkyl of R3The molecular structural group of (A) is an n-propyl group or the molecular structural group of R3 is an isopropyl group.
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