CN113736535A - Natural ester base oil and preparation method thereof, and natural ester insulating oil and application thereof - Google Patents
Natural ester base oil and preparation method thereof, and natural ester insulating oil and application thereof Download PDFInfo
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/32—Esters
- C10M105/38—Esters of polyhydroxy compounds
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/045—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution and non-macromolecular compounds
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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
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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
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/32—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes natural resins
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/04—Ethers; Acetals; Ortho-esters; Ortho-carbonates
- C10M2207/046—Hydroxy ethers
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/283—Esters of polyhydroxy compounds
- C10M2207/2835—Esters of polyhydroxy compounds used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/22—Heterocyclic nitrogen compounds
- C10M2215/223—Five-membered rings containing nitrogen and carbon only
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/48—Slushing oils
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Abstract
The invention provides natural ester base oil and a preparation method thereof, natural ester insulating oil and application thereof, belongs to the technical field of insulating oil, and comprises the following steps: and (3) distilling and concentrating the wood pulp floating oil to obtain sulfate soap, mixing the sulfate soap with phosphoric acid, acidifying, performing vacuum rectification, and performing esterification reaction to obtain the natural ester base oil. The invention adopts phosphoric acid acidification partAnd (3) treating sulfate soap, separating unsaponifiable matters, and performing esterification to prepare the natural ester base oil, wherein the main component of the prepared natural ester base oil is triolein and/or triolein and has lower pour point and kinematic viscosity. The results of the examples show that the natural ester insulating oil provided by the invention has the kinematic viscosity of 7.735mm at 100 DEG C2A kinematic viscosity at 40 ℃ of 32.01 mm/s2And the pour point is-25 ℃, and in addition, the wood pulp floating oil is adopted as the raw material, so that the waste can be changed into valuable, the resources are saved, and the additional economic value is generated.
Description
Technical Field
The invention belongs to the technical field of insulating oil, and particularly relates to natural ester base oil and a preparation method thereof, and natural ester insulating oil and application thereof.
Background
The insulating oil is widely applied to various electric equipment, particularly transformers, and generally plays roles in insulation and heat dissipation. Most of the traditional insulating oil is mineral insulating oil, the main component of the traditional insulating oil is a mixture of various hydrocarbons, and the traditional insulating oil has the advantages of low price and good physical and chemical dielectric properties, but the traditional insulating oil has lower burning point, poorer fire resistance, low biodegradation degree and poorer environmental protection. The natural ester insulating oil has the characteristics of higher ignition point, better fire resistance, high biodegradability and better environmental protection, and is widely applied.
The natural ester insulating oil prepared by the method contains stearic acid, so that the natural ester insulating oil has higher pour point and is difficult to apply in low-temperature areas, and meanwhile, the natural ester insulating oil has higher kinematic viscosity and poorer fluidity, is not beneficial to heat dissipation of power equipment, is easy to cause fire, and harms society and personal safety.
Therefore, how to reduce the pour point and kinematic viscosity of the natural ester insulating oil becomes a difficult point in the prior art.
Disclosure of Invention
The invention aims to provide natural ester base oil and a preparation method thereof, and natural ester insulating oil and application thereof. The natural ester insulating oil provided by the invention has lower pour point and kinematic viscosity.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of natural ester base oil, which comprises the following steps:
(1) distilling and concentrating the wood pulp oil slick to obtain sulfate soap;
(2) mixing the sulfate soap obtained in the step (1) with phosphoric acid, and carrying out acidification treatment to obtain an acidification product;
(3) performing vacuum rectification on the acidified product obtained in the step (2) to obtain a rectified product;
(4) and (4) mixing the rectification product obtained in the step (3) with glycerol, a catalyst and water, and carrying out esterification reaction to obtain the natural ester base oil.
Preferably, the temperature of distillation and concentration in the step (1) is 80-100 ℃, and the time of distillation and concentration is 1-3 h.
Preferably, the mass ratio of the phosphoric acid to the sulfate soap in the step (2) is (3-6): 100.
preferably, the temperature of vacuum rectification in the step (3) is 98-102 ℃, 108-112 ℃ or 118-122 ℃.
Preferably, the volume ratio of the glycerol to the rectification product in the step (4) is (1-3): 1.
preferably, the catalyst in the step (4) is lipase; the mass ratio of the catalyst to the rectification product is (1-3): 100.
preferably, the mass ratio of the water to the rectification product in the step (4) is (3-7): 100.
the invention provides the natural ester base oil prepared by the preparation method in the technical scheme, which comprises triolein and/or trilinolein.
The invention also provides natural ester insulating oil which comprises one or more of an antioxidant, a metal deactivator, a pour point depressant, traditional natural ester insulating oil, mineral insulating oil and synthetic ester insulating oil and the natural ester base oil in the technical scheme.
The invention also provides application of the natural ester insulating oil in the technical scheme in power equipment. The invention provides a preparation method of natural ester base oil, which comprises the following steps: distilling and concentrating the wood pulp oil slick to obtain sulfate soap; mixing the obtained sulfate soap with phosphoric acid, and carrying out acidification treatment to obtain an acidification product; performing vacuum rectification on the obtained acidified product to obtain a rectified product; and mixing the obtained rectification product with glycerol, a catalyst and water, and carrying out esterification reaction to obtain the natural ester base oil. The sulfate soap is acidized by phosphoric acid, unsaponifiable matters are separated, esterification is carried out after rectification to prepare the natural ester base oil, and the main components of the prepared natural ester base oil are triolein and/or triolein and have lower pour point and kinematic viscosity. The results of the examples show that the kinematic viscosity at 100 ℃ of the natural ester insulating oil prepared using the natural ester base oil prepared according to the present invention is 7.735mm2A kinematic viscosity at 40 ℃ of 32.01 mm/s2The pour point is-25 ℃.
In addition, the wood pulp floating oil is used as the raw material, so that waste can be changed into valuable, resources are saved, and additional economic value is generated.
Detailed Description
The invention provides a preparation method of natural ester base oil, which comprises the following steps:
(1) distilling and concentrating the wood pulp oil slick to obtain sulfate soap;
(2) mixing the sulfate soap obtained in the step (1) with phosphoric acid, and carrying out acidification treatment to obtain an acidification product;
(3) performing vacuum rectification on the acidified product obtained in the step (2) to obtain a rectified product;
(4) and (4) mixing the rectification product obtained in the step (3) with glycerol, a catalyst and water, and carrying out esterification reaction to obtain the natural ester base oil.
In the present invention, the sources of the components are not particularly limited, unless otherwise specified, and commercially available products known to those skilled in the art may be used.
According to the invention, the wood pulp oil slick is distilled and concentrated to obtain the sulfate soap.
In the present invention, the tall oil is preferably derived from a by-product in the paper industry, and more preferably: with NaOH and Na2During the process of cooking pine wood chips by the mixed solution of S, fatty acid and resin acid in the pine wood are saponified by alkali to form sodium salt of the fatty acid and the resin acid and black liquor formed by dissolving neutral substances.
In the present invention, the tall oil is preferably washed with water and filtered in this order before concentration by distillation.
The operation of the washing and filtering is not particularly limited in the present invention, and the technical solution of the washing and filtering operation known to those skilled in the art can be adopted. In the invention, the water washing and filtering can remove insoluble cellulose in the wood pulp oil slick, thereby avoiding influencing the product performance.
In the invention, the temperature of the distillation concentration is preferably 80-100 ℃, and more preferably 90 ℃; the distillation and concentration time is preferably 1-3 h, and more preferably 2 h. In the invention, most of water in the wood pulp oil slick is removed in the distillation concentration process, so that the sulfate soap is crystallized and separated out. In the present invention, the sulfate soap contains, as main components, a resinate, a fatty acid salt and an unsaponifiable matter.
After the sulfate soap is obtained, the sulfate soap is mixed with phosphoric acid for acidification treatment to obtain an acidification product.
In the present invention, the mass fraction of phosphoric acid is preferably 33%. In the invention, the mass ratio of the phosphoric acid to the sulfate soap is preferably (3-6): 100, more preferably (4-5): 100. the invention limits the mass ratio of the phosphoric acid to the sulfate soap to be in the range, can fully acidify the fatty acid salt and the resin acid salt in the sulfate soap, forms the fatty acid and the resin acid to enter the water phase, and removes unsaponifiable matters insoluble in the water phase.
In the invention, the temperature of the acidification treatment is preferably 20-30 ℃; the time of the acidification treatment is preferably 10-60 min, and more preferably 20-40 min. The present invention limits the temperature and time of the acidification treatment within the above range, and can make the acidification treatment more complete.
In the present invention, the reaction equation during the acidification treatment is as follows:
3RCOONa+H3PO4→Na3PO4+3RCOOH。
after the acidification treatment is finished, the invention preferably carries out water washing and phase separation on the product after the acidification treatment in sequence to obtain the acidified product.
In the present invention, the water used in the washing is preferably high purity water; the volume of the water is preferably 15-30% of that of the product after the acidification treatment, and more preferably 20-25%; the washing temperature is preferably 70-90 ℃, and more preferably 80 ℃. In the present invention, the water washing is preferably performed first under stirring and then left to stand. In the invention, the stirring time is preferably 20-40 min, and more preferably 30 min; the stirring speed is preferably 200-400 rpm, and more preferably 300 rpm; the standing time is preferably 1.5-2.5 h, and more preferably 2 h. In the present invention, the water washing is used to remove phosphoric acid from the acidified product.
The operation of the phase separation is not particularly limited in the present invention, and the technical scheme of phase separation known to those skilled in the art can be adopted. In the invention, the split phase is used for separating out the water phase for subsequent rectification and removing the unsaponifiable matter which is not dissolved in water, thereby avoiding influencing the performance of the product. In the invention, the unsaponifiable matter can be used in the field of medicines by extracting phytosterol and the like in the unsaponifiable matter again.
After the acidified product is obtained, the acidified product is rectified in vacuum to obtain a rectified product.
In the invention, the vacuum degree of the vacuum rectification is preferably 7-9 Pa, and more preferably 8 Pa; the temperature of the vacuum rectification is preferably 98-102 ℃ or 108-112 ℃ or 118-122 ℃, and more preferably 100 ℃ or 110 ℃ or 120 ℃. When the vacuum rectification temperature is 98-102 ℃, the distillation product is oleic acid; when the vacuum rectification temperature is 108-112 ℃, the distillation product is a mixture of oleic acid and linoleic acid; when the vacuum rectification temperature is 118-122 ℃, the distillation product is linoleic acid. In the present invention, the vacuum distillation time is not particularly limited, and no distillation fraction is distilled.
After the rectification product is obtained, the rectification product is mixed with glycerin, a catalyst and water for esterification reaction to obtain the natural ester base oil.
In the invention, the volume ratio of the glycerol to the rectification product is preferably (1-3): 1, more preferably 2: 1. In the present invention, the glycerol is reacted with oleic acid and/or linoleic acid in the rectified product to form an ester. The volume ratio of the glycerol to the rectification product is limited in the range, so that the rectification product can be esterified more fully.
In the present invention, the catalyst is preferably a lipase; the mass ratio of the catalyst to the rectification product is preferably (1-3): 100, more preferably 2: 100. The invention limits the mass ratio of the catalyst to the rectification product within the range, and can catalyze the esterification reaction to be carried out more fully.
In the invention, the mass ratio of the water to the rectification product is preferably (3-7): 100, more preferably (4-6): 100, most preferably 5: 100. The present invention limits the mass ratio of water to the rectification product within the above range, and enables the esterification reaction to proceed more sufficiently.
The operation of mixing the rectification product with the glycerol, the catalyst and the water is not particularly limited in the invention, and the technical scheme of material mixing which is well known to the person skilled in the art can be adopted.
In the present invention, the esterification reaction is preferably carried out under stirring conditions; the stirring speed is preferably 200-400 rpm, and more preferably 300 rpm. In the invention, the temperature of the esterification reaction is preferably 50-70 ℃, and more preferably 60 ℃; the time of the esterification reaction is preferably 10-14 h, and more preferably 12 h. The invention limits the temperature and time of the esterification reaction in the range, can ensure that the esterification reaction is more sufficient, and improves the conversion rate.
In the present invention, the equation of the esterification reaction is as follows:
after the esterification reaction is finished, the product of the esterification reaction is preferably refined to obtain the natural ester base oil.
In the present invention, the refining preferably includes washing with water, decoloring, alkali refining and drying, which are sequentially performed.
The operation of the water washing is not particularly limited in the present invention, and a technical scheme of water washing known to those skilled in the art may be adopted.
In the present invention, the decolorization is preferably performed by mixing clay and activated carbon. In the invention, the mass of the argil is preferably 1-3% of that of the esterification product, and more preferably 2%; the mass of the activated carbon is preferably 1-3% of that of the esterification product, and more preferably 2%; the decolorizing temperature is preferably 80-100 ℃, and more preferably 90 ℃; the decoloring time is preferably 0.5-1.5 h, and more preferably 1 h; the degree of vacuum of the decolorization is preferably 7-9 Pa, and more preferably 8 Pa. The parameters of the decolorant, such as temperature, time and the like, for decoloring are limited in the range, so that the decoloring can be more complete.
After the decoloring is completed, the decolored product is preferably filtered in the present invention.
The operation of the filtration is not particularly limited in the present invention, and a filtration technical scheme known to those skilled in the art may be adopted. In the present invention, the filtration is used to remove clay and activated carbon.
In the present invention, the alkali refining is preferably performed by adding an alkali solution. In the present invention, the alkali solution is preferably a sodium hydroxide solution; the mass concentration of the alkali liquor is preferably 30%; the volume of the alkali liquor is preferably 20% of the volume of the decolorized product; the alkali refining is preferably carried out for 3h at 45 ℃ and then for 2h at 85 ℃. In the present invention, the alkali refining is preferably performed under stirring conditions; the stirring speed is preferably 200-400 rpm, and more preferably 300 rpm. In the present invention, the alkali refining is used to remove impurities in the product. The invention limits the parameters of alkali refining such as temperature, time and the like in the range, can fully remove impurities and improve the purity of the product.
In the invention, the drying temperature is preferably 60-80 ℃, and more preferably 70 ℃; the drying time is preferably 1-3 h, and more preferably 2 h; the degree of vacuum for drying is preferably 7-9 Pa, and more preferably 8 Pa. The invention limits the drying temperature and time in the above range, can fully remove the water in the product, and improve the product purity.
The sulfate soap is treated by phosphoric acid acidification, simultaneously unsaponifiable matters are separated, and then esterification is carried out to prepare the natural ester base oil, the main components of the prepared natural ester base oil are triolein and/or triolein, the process parameters such as the dosage of each component, the reaction temperature, the reaction time and the like are controlled, the product purity is improved, and in addition, the wood pulp floating oil is used as the raw material, so that the waste can be changed into valuable, the resources are saved, and the additional economic value is generated.
The invention provides the natural ester base oil prepared by the preparation method in the technical scheme, which comprises triolein and/or trilinolein.
The natural ester base oil provided by the invention has lower pour point and kinematic viscosity.
The invention also provides natural ester insulating oil which comprises one or more of an antioxidant, a metal deactivator, a pour point depressant, traditional natural ester insulating oil, mineral insulating oil and synthetic ester insulating oil and the natural ester base oil in the technical scheme.
In the present invention, the antioxidant preferably comprises butylhydroquinone, 2, 6-di-tert-butyl-4-methylphenol, propyl gallate, butylated hydroxyanisole or tocopherol; the mass fraction of the antioxidant is preferably less than or equal to 5%. In the present invention, the antioxidant is used to improve the antioxidant property of the natural ester insulating oil.
In the present invention, the metal deactivator preferably includes benzotriazole, 5-methylbenzotriazole, N- [2- (2-ethylhexyl) -aminomethyl ] -methylbenzotriazole or Irgamet 39; the mass fraction of the metal passivator is preferably less than or equal to 0.01 percent. In the present invention, the metal deactivator is used to improve the corrosion resistance of the natural ester insulating oil.
In the present invention, the pour point depressant includes long chain alkyl naphthalene, polymethacrylate or polyalpha-olefin; the mass fraction of the pour point depressant is preferably less than or equal to 0.02 percent. In the present invention, the pour point depressant is used to lower the freezing point of natural ester insulating oil.
The present invention is not particularly limited to specific types of the conventional natural ester insulating oil, mineral insulating oil and synthetic ester insulating oil, and may be commercially available products well known to those skilled in the art. In the invention, the mass fraction of the traditional natural ester insulating oil, the mineral insulating oil and the synthetic ester insulating oil is preferably 0-100%.
The natural ester insulating oil provided by the invention has lower pour point and kinematic viscosity.
The preparation method of the natural ester insulating oil is not particularly limited, and the technical scheme of material mixing, which is well known to a person skilled in the art, can be adopted.
The invention also provides application of the natural ester insulating oil in the technical scheme in power equipment.
The operation of the application of the natural ester insulating oil in the power equipment is not particularly limited, and the technical scheme of the application of the natural ester insulating oil in the power equipment, which is well known to those skilled in the art, can be adopted.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Washing and filtering the wood pulp oil slick in sequence, and then distilling and concentrating for 2h at 90 ℃ to obtain sulfate soap;
(2) mixing the sulfate soap with 33% phosphoric acid (the mass ratio of phosphoric acid to sulfate soap is 5:100), carrying out acidification treatment at 25 ℃ for 30min, then adding high-purity water accounting for 20% of the volume of the product, stirring at 80 ℃ for 30min, standing for 2h, and separating out a water phase to obtain an acidified product;
(3) vacuum rectifying the acidified product at 100 ℃ under the condition of 8Pa to obtain a rectified product oleic acid;
(4) mixing the rectified product oleic acid with glycerol (the volume ratio of glycerol to the rectified product is 2:1), lipase (the mass ratio of lipase to the rectified product is 2:100) and water (the mass ratio of water to the rectified product is 5:100), stirring and reacting for 12h at 60 ℃ (the oleic acid conversion rate is 96%), then washing the product with water, adding clay accounting for 2% of the product mass and activated carbon accounting for 2% of the product mass, decoloring in vacuum at 90 ℃ and 8Pa, filtering, then adding sodium hydroxide solution accounting for 20% of the product volume (the mass fraction is 30%), stirring for 3h at 45 ℃ and then stirring for 2h at 85 ℃ for alkali refining, and finally drying in vacuum at 70 ℃ and 8Pa for 2h to obtain the natural ester base oil, wherein the main component of the natural ester base oil is triolein.
Example 2
To the natural ester base oil prepared in example 1, butylated hydroxyanisole 0.3 mass% and metal deactivator Irgamet39 0.01 mass% were added and mixed uniformly to obtain a natural ester insulating oil.
Example 3
(1) Washing and filtering the wood pulp oil slick in sequence, and then distilling and concentrating for 2h at 90 ℃ to obtain sulfate soap;
(2) mixing the sulfate soap with 33% phosphoric acid (the mass ratio of phosphoric acid to sulfate soap is 5:100), carrying out acidification treatment at 25 ℃ for 30min, then adding high-purity water accounting for 20% of the volume of the product, stirring at 80 ℃ for 30min, standing for 2h, and separating out a water phase to obtain an acidified product;
(3) vacuum rectifying the acidified product at 120 ℃ under 8Pa to obtain a rectified product linoleic acid;
(4) mixing the rectified product linoleic acid with glycerol (the volume ratio of glycerol to the rectified product is 2:1), lipase (the mass ratio of lipase to the rectified product is 2:100) and water (the mass ratio of water to the rectified product is 5:100), stirring and reacting for 12h at 60 ℃ (the linoleic acid conversion rate is 96%), then washing the product with water, adding clay accounting for 2% of the product mass and activated carbon accounting for 2% of the product mass, decoloring in vacuum at 90 ℃ and 8Pa, filtering, then adding sodium hydroxide solution accounting for 20% of the product volume (the mass fraction is 30%), stirring for 3h at 45 ℃ and then stirring for 2h at 85 ℃ for alkali refining, and finally drying in vacuum at 70 ℃ and 8Pa for 2h to obtain the natural ester base oil, wherein the main component of the natural ester base oil is triolein.
Example 4
To the natural ester base oil prepared in example 2, butylated hydroxyanisole was added in an amount of 0.3 mass%, a metal deactivator Irgamet39 was added in an amount of 0.01 mass%, and a pour point depressant polymethyl methacrylate was added in an amount of 0.01 mass%, and the mixture was mixed uniformly to obtain a natural ester insulating oil.
Example 5
(1) Washing and filtering the wood pulp oil slick in sequence, and then distilling and concentrating for 2h at 90 ℃ to obtain sulfate soap;
(2) mixing the sulfate soap with 33% phosphoric acid (the mass ratio of phosphoric acid to sulfate soap is 5:100), carrying out acidification treatment at 25 ℃ for 30min, then adding high-purity water accounting for 20% of the volume of the product, stirring at 80 ℃ for 30min, standing for 2h, and separating out a water phase to obtain an acidified product;
(3) vacuum rectifying the acidified product at 110 ℃ under the condition of 8Pa to obtain a mixture of rectified products oleic acid and linoleic acid;
(4) mixing the rectification product with glycerol (the volume ratio of the glycerol to the rectification product is 2:1), lipase (the mass ratio of the lipase to the rectification product is 2:100) and water (the mass ratio of the water to the rectification product is 5:100), stirring and reacting for 12h at 60 ℃ (the conversion rate of oleic acid and linoleic acid is 96%), then washing the product with water, adding carclazyte accounting for 2 percent of the mass of the product and active carbon accounting for 2 percent of the mass of the product, decoloring in vacuum at 90 ℃ under the condition of 8Pa, filtering, then adding sodium hydroxide solution (mass fraction is 30%) whose volume is 20% of product volume, stirring at 45 deg.C for 3h, stirring at 85 deg.C for 2h to make alkali refining, finally vacuum drying at 70 deg.C under 8Pa for 2h to obtain natural ester base oil, the main component of the oil-in-water emulsion is a mixture of triolein and trilinolein (the mass ratio of triolein to trilinolein is 2: 8).
Example 6
To the natural ester base oil prepared in example 3, butylated hydroxyanisole 0.3 mass% and metal deactivator Irgamet39 0.01 mass% were added and mixed uniformly to obtain a natural ester insulating oil.
The natural ester insulating oils prepared in examples 2, 4, and 6 were tested for their biodegradability, and the results showed that the natural ester insulating oils prepared in examples 2, 4, and 6 had a biodegradability of > 90% in 28 days.
The natural ester insulating oils prepared in examples 2, 4 and 6 and the conventional natural ester insulating oil (FR3) were subjected to performance tests, and the respective test standards and data are shown in table 1.
Table 1 properties of the natural ester insulating oils and the conventional natural ester insulating oils prepared in examples 2, 4 and 6
As can be seen from Table 1, the natural ester insulating oil prepared by the invention has lower kinematic viscosity, is beneficial to equipment heat dissipation, has lower pour point, and is more beneficial to being applied to low-temperature areas.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of natural ester base oil comprises the following steps:
(1) distilling and concentrating the wood pulp oil slick to obtain sulfate soap;
(2) mixing the sulfate soap obtained in the step (1) with phosphoric acid, and carrying out acidification treatment to obtain an acidification product;
(3) performing vacuum rectification on the acidified product obtained in the step (2) to obtain a rectified product;
(4) and (4) mixing the rectification product obtained in the step (3) with glycerol, a catalyst and water, and carrying out esterification reaction to obtain the natural ester base oil.
2. The preparation method according to claim 1, wherein the temperature of the distillation concentration in the step (1) is 80-100 ℃, and the time of the distillation concentration is 1-3 h.
3. The preparation method according to claim 1, wherein the mass ratio of phosphoric acid to sulfate soap in the step (2) is (3-6): 100.
4. the method according to claim 1, wherein the temperature of the vacuum distillation in the step (3) is 98-102 ℃, 108-112 ℃ or 118-122 ℃.
5. The preparation method according to claim 1, wherein the volume ratio of the glycerol to the rectification product in the step (4) is (1-3): 1.
6. the method according to claim 1, wherein the catalyst in the step (4) is a lipase; the mass ratio of the catalyst to the rectification product is (1-3): 100.
7. the preparation method according to claim 1, wherein the mass ratio of water to rectification products in the step (4) is (3-7): 100.
8. the natural ester base oil produced by the production method according to any one of claims 1 to 7, comprising glycerol trioleate and/or glycerol trilinoleate.
9. A natural ester insulating oil comprising one or more of an antioxidant, a metal deactivator, a pour point depressant, a conventional natural ester insulating oil, a mineral insulating oil and a synthetic ester insulating oil and the natural ester base oil of claim 8.
10. Use of the natural ester insulating oil of claim 9 in electrical equipment.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101456813A (en) * | 2007-12-13 | 2009-06-17 | 中国科学院兰州化学物理研究所 | Method for synthesizing polyatomic alcohol fatty acid ester |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456813A (en) * | 2007-12-13 | 2009-06-17 | 中国科学院兰州化学物理研究所 | Method for synthesizing polyatomic alcohol fatty acid ester |
Non-Patent Citations (1)
| Title |
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| 傅国秀: "我国木浆浮油的提取和加工特点", 《林产化工通讯》 * |
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