CN105219480B - A kind of pentaerythrite ester base oil and its synthetic method - Google Patents
A kind of pentaerythrite ester base oil and its synthetic method Download PDFInfo
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Abstract
The invention provides a kind of pentaerythrite ester base oil and its synthetic method.Specific synthetic method comprises the following steps:Using pentaerythrite as reaction raw materials, catalyst A is added, carries out auto polymerization reaction, pentaerythrite of the generation rich in dimer;Aliphatic acid or aryl carboxylic acid are added into the pentaerythrite rich in dimer, esterification is carried out, obtains crude product;The crude product depickling is decolourized, obtains product.The present invention improves viscosity, the viscosity temperature characteristic of base oil, reduces the condensation point of base oil, obtained base oil is particularly suitable for fields such as aviation engine lubricating oil, gear oils by the dimer for introducing pentaerythritol ester in the mixture and its corresponding ester.
Description
Technical field
The present invention relates to lube base oil field, in particular to a kind of pentaerythrite ester base oil and its synthesis
Method.
Background technology
Lubricating oil runs indispensable material as machine, for maintaining mechanical normal operation, improves mechanical efficiency, prolongs
Long mechanical service life plays vital effect.With the development of contemporary industry, the environment of machine operation is more harsh, right
The service life of machine proposes higher requirement, and former mineral base oil is non-renewable, has pollution to environment, is gradually backed out
Use.And there is the shortcomings of poor heat endurance, oxidation stability and hydrolytic stability difference in vegetable and animals oils as lubricating base oil.
Therefore, sight has been turned to synthetic lubricant fluid by people.The lubricating oil of chemical synthesis, its combination property is far above mineral oil and dynamic plant
Thing oil, can meet different performance requirements, be developed rapidly.
Synthetic lubricant base oil is divided into organic hydrocarbon, organosilane ester and other synthesis and moistened by American Society Testing and Materials
The three major types such as lubricating oil class.Wherein Esters oil is one kind important in synthetic lubricant fluid, is occupied an important position and sizable ratio
Weight.Esters oil is that organic acid and alcohol is obtained by dehydration esterification reaction.During the Second World War, because the pour point of mineral oil is compared with high and low temperature
Poor fluidity so that German aircraft can not start, so as to accelerate the research of synthetic ester lubricant.Nineteen forty-three, Zorn are established
Industrialized dibasic acid esters production line, largely produces various Esters oils, and product is mainly used in compound with polyolefin or mineral oil, makes
It is adapted to the low condensation point lubricating oil used in aircraft, vehicle, locomotive etc..1940-1942, Germany, Britain, the U.S. produce in succession
Diester-type lubricating oil.Before and after 1958, dibasic acid esters oil is replaced by the more preferable polyol ester of antioxygenic property.Neopentyl polyol ester
(neopentyl polyol ester is the product for having trimethylolpropane, pentaerythrite, dimethyltrimethylene glycol etc. to be obtained with fatty acid response)
Due to not having hydrogen atom on the β positions carbon atom of alcohol part, there is more excellent heat endurance.Now, with neopentyl polyol ester
Based on oily synthesis aeroengine oil be widely used in aeroengine oil, compressor oil and flame resistance hydraulic oil, high temperature chain
The fields such as bar oil.
In existing known synthesis technique, generally require to add substantial amounts of different nonyl during synthesis of pentaerythritol ester base oil
Acid or aryl carboxylic acid obtain preferable cryogenic property and higher viscosity, but reduce viscosity index (VI) (such as patent
US4826633, US5503761, US20030153471 etc.).
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of synthetic method of pentaerythrite ester base oil, described synthetic method
By the dimer for introducing pentaerythritol ester in the mixture and its corresponding ester, viscosity, the viscosity temperature characteristic of base oil are improved,
The condensation point of base oil is reduced, the base oil for synthesizing to obtain is particularly suitable for fields such as aviation engine lubricating oil, gear oils.
The second object of the present invention is to provide a kind of pentaerythrite ester base oil, and not only cryogenic property is excellent for the base oil
It is different, and viscosity index (VI) is high, and condensation point is low, particularly suitable for fields such as aviation engine lubricating oil, gear oils, compared to existing
Significant performance advantage be present in base oil.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme:
A kind of synthetic method of pentaerythrite ester base oil, comprises the following steps:
Using pentaerythrite as reaction raw materials, catalyst is added, carries out auto polymerization reaction, Ji Wusi of the generation rich in dimer
Alcohol;
Aliphatic acid or aryl carboxylic acid are added into the pentaerythrite rich in dimer, carries out esterification, is obtained thick
Product;
The crude product depickling is decolourized, obtains product.
The auto polymerization reaction response that above-mentioned synthetic method first passes through pentaerythrite introduces dipentaerythritol, then need not
Separation is directly added into acid and carries out esterification, obtains corresponding ester, most decolourizes to get product through depickling afterwards, end properties tool
There are following characteristics:In colourless or lurid grease, the viscosity at 40 DEG C can reach 20-30mm2/ s, the viscosity at 100 DEG C
It can reach 5mm2/ more than s, viscosity index (VI) is more than 132, and for condensation point below -41 DEG C, acid number is respectively less than 0.1mgKOH/g.
As can be seen here, compared with existing synthetic method there is following advantage in above-mentioned synthetic method:First, base oil is not only
Possess relatively low condensation point and acid number, also possess higher viscosity and viscosity index (VI);Although the 2, introducing single step reaction more,
Front and rear two-step reaction without separation, thus can not complicate integrated artistic with accessible linking completely.
Above-mentioned synthetic method can make following improve:
Preferably, in the pentaerythrite rich in dimer, the weight ratio of dipentaerythritol and pentaerythrite is:5-
22:95-78。
Both in base oil with this ratio in the presence of, the viscosity of base oil, viscosity index (VI) and condensation point are more excellent, performance
It is more excellent.
Preferably, the catalyst can be sour (sulfuric acid, phosphoric acid, phosphorous acid, p-methyl benzenesulfonic acid etc.) or alkali (such as hydroxide
Potassium, potassium carbonate, saleratus, sodium acid carbonate, sodium hydroxide, sodium carbonate etc.) or molecular sieve, sulfate, montmorillonite etc. in
One or more of compound, one or more preferably in phosphoric acid, phosphorous acid, sulfuric acid, the high catalytic efficiency of these three catalyst,
Reaction time can be greatly shortened, its quality dosage is preferably the 0.5%-5% of pentaerythrite (relative to the weight of reactant
Than), further preferred 1-3%.
Preferably, the auto polymerization reaction is carried out at negative pressure, 100-260 DEG C, and negative pressure is easy to the removing of water, from reaction
Further promote the positive progress of auto polymerization reaction in balance, and reaction time is short at 100-260 DEG C, more preferably 150-250
DEG C, more preferably 180-240 DEG C.
Preferably, the time of the auto polymerization reaction is 2-10 hours, preferably 2-6 hours.The rationally control reaction time
To avoid the degree of polymerization excessive, have a negative impact to the performance of base oil.
Preferably, the aliphatic acid is one or more of mixing in C4-C12 saturated acids, oleic acid, isostearic acid, and this is several
The performance of base oil obtained by after kind aliphatic acid esterification is more preferable, and the aliphatic acid can be C2-C20 saturated fatty acids
(such as valeric acid, caproic acid, enanthic acid, octanoic acid, n-nonanoic acid, capric acid) or unrighted acid (such as oleic acid, linoleic acid, leukotrienes
Deng), it can be straight-chain acid (positive valeric acid, n-caproic acid, positive enanthic acid, caprylic acid, pelargonic acid etc.), can also be branched acids (such as isoamyl
Acid, isooctyl acid, different n-nonanoic acid, isostearic acid etc.).
Preferably, the pentaerythrite rich in dimer and aliphatic acid mol ratio are preferably 3-6:1.Using this mol ratio not only
Reaction time is short, and yield is high, more preferably 4-5:1.
Preferably, it is additionally added following catalyst when carrying out the esterification:Phosphoric acid, phosphorous acid, butyl titanate, phosphoric acid
One or more of mixing in tributyl.The speed of esterification can be improved by adding catalyst, phosphoric acid, phosphorous acid, butyl titanate,
Reaction time used in this several catalyst of tributyl phosphate is short, and crude product color is shallower.It is of course also possible to use other catalysis
Agent, such as sulfuric acid, p-methyl benzenesulfonic acid, solid super-strong acid, molecular sieve, organotin, tributyl phosphite, tetraisopropyl titanate.
Preferably, the esterification is that 2-15 hours are reacted at negative pressure, 100-260 DEG C.
It is beneficial under same negative pressure except the water of dereaction generation, promotes esterification is positive to carry out, improve yield, shorten reaction
Cycle, reaction temperature and time are preferable to react 2-15 hours at 100-260 DEG C, are further 150-250 DEG C, further
To react 6-12 hours at 160-240 DEG C.
Preferably, the method for the depickling decolouring is:Addition at least one of alkali and complexing agent is mixed with atlapulgite
Compound, carry out composite adsorption processing.Compared to the technique of traditional alkali cleaning, washing deacidification, composite adsorption handling process of the invention letter
It is single, waste water will not be produced, it is free from environmental pollution.
Preferably, the complexing agent is one in sodium ammonium triacetate, edetate, diethylenetriamine pentacarboxylic acid salt
Kind is a variety of, and total addition of the complexing agent and the atlapulgite is the 1%-10% of the crude product quality, is obtained more preferable
Deacidification effect, and if alkali or the mass ratio of complexing agent and atlapulgite better, more preferably 1/1- when being 2/1-0.5/1
0.8/1。
The temperature of the composite adsorption processing is 50-150 DEG C, and the time is 0.5-2 hours.Handle, deacidify on this condition
Time is short, and clearance is high.
Preferably, deacidification is first evaporated under reduced pressure before composite adsorption processing, can so reduces follow-up composite adsorption
Required amount of reagent, both organically combine acquisition more preferably clearance and remove speed.
A kind of pentaerythrite ester base oil, it is made using the synthetic method of pentaerythrite ester base oil described above.
Compared to traditional pentaerythrite ester base oil, above-mentioned base oil also contains dimerization in addition to containing pentaerythritol ester
Pentaerythritol ester, these compositions, which combine to show, preferably is used for high perofmrnace lubricating oils (aeroengine oil, compressor
Oil and flame resistance hydraulic oil, high-temperature chain oil etc.) physico-chemical property:Viscosity under low temperature and high temperature is all higher, and viscosity index (VI) is high,
Condensation point is low, and acid number is low, therefore it will have broader industrial prospect.
Compared with prior art, beneficial effects of the present invention are:
(1) chemical composition of existing monopentaerythritol ester base oil is changed, is referred to so as to improve its viscosity and viscosity
Number, reduces its condensation point.
(2) condition of polymerisation and esterification in synthesis is optimized, so as to improve yield, shortens reaction time.
(3) ratio of dimer and monomer in base oil is optimized, so as to further improve the performance of base oil.
(4) deacidifying process is improved, the depickling by way of a variety of adsorbent composite adsorptions, avoids washing, alkali cleaning institute
The problems such as pollution that brings is big, water consumption is big, complex process.
(5) it will be evaporated under reduced pressure and be combined with adsorption deacidification, reduce cost of material and technology difficulty.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted specific in embodiment
Condition person, the condition suggested according to normal condition or manufacturer are carried out.Agents useful for same or the unreceipted production firm person of instrument, it is
The conventional products that can be obtained by commercially available purchase.
Embodiment 1
The synthesis of pentaerythrite 1 rich in dimer
500g monopentaerythritols and the phosphoric acid of 5g 85% are added in 5L reactors, the air led in nitrogen displacement kettle, are repeated
4 times.Temperature programming, after temperature is raised to 160 DEG C, -0.05MPa is evacuated down to, is maintained the temperature between 200-240 DEG C, reaction 2
Hour.Sampling, bipentaerythrite and single cropping penta 4 in product are detected by the high performance liquid chromatography with Composition distribution
The ratio of alcohol is 5/95.
The synthesis of pentaerythritol fatty ester 1 rich in dimer
After above-mentioned reacting liquid temperature drops to 100 DEG C, the positive valeric acids of 406g, the positive enanthic acid of 994g, 676g are added into reactor
Pelargonic acid, reactor is closed, led to nitrogen to pressure 0.5MPa, then vacuumize.Repeat this operation 4 times.Then program liter
Temperature maintains the temperature at 160-180 DEG C and reacted 6 hours to 160 DEG C.After the completion of reaction, 200 DEG C are increased the temperature to, vacuum distillation removes
Unreacted acid is removed, sample acid number is treated in sampling detection<When 1, stop depickling.After reaction solution drops to room temperature, material, Ran Houjia are released
Enter the EDTA and atlapulgite (mass ratio 1/1) of 3% mass, be heated to 110 DEG C, stirred under nitrogen atmosphere 1 hour.After the completion of,
It is filtrated to get lube base oil.
Properties of product:Viscosity (40 DEG C, mm2/ s) 25.1, viscosity (100 DEG C, mm2/ s) 5.05, viscosity index (VI) 132, condensation point<-
50 DEG C, acid number 0.05mgKOH/g.
Embodiment 2
The synthesis of pentaerythrite 2 rich in dimer
450g monopentaerythritols and 4.5g p-methyl benzenesulfonic acid are added in 5L reactors, the air led in nitrogen displacement kettle,
It is repeated 4 times.Temperature programming, after temperature is raised to 160 DEG C, -0.05MPa is evacuated down to, is maintained the temperature between 200-240 DEG C,
Reaction 2.5 hours.Sampling, bipentaerythrite and list in product are detected by the high performance liquid chromatography with Composition distribution
The ratio of pentaerythrite is 13/87.
The synthesis of pentaerythritol fatty ester 2 rich in dimer
When above-mentioned reacting liquid temperature drops to 100 DEG C, the positive valeric acids of 455g, 169g n-caproic acids, 189g are added into reactor
Positive enanthic acid, 629g caprylic acids, 460g pelargonic acids, 4g tributyl phosphites, reactor is closed, logical nitrogen to pressure 0.5MPa,
Then vacuumize.Repeat this operation 4 times.Then temperature programming is to 160 DEG C, maintains the temperature at 160-200 DEG C, and pressure-
Reacted 7 hours under 0.03MPa to -0.05MPa.After the completion of reaction, 200 DEG C are maintained the temperature at, it is unreacted to be evaporated under reduced pressure removing
Sample acid number is treated in acid, sampling detection<When 1, stop depickling.After reaction solution drops to room temperature, material is released, then adds 5% mass
Sodium carbonate and atlapulgite (mass ratio 1/1), be heated to 110 DEG C, stirred under nitrogen atmosphere 1 hour.After the completion of, it is filtrated to get
Lube base oil.
Properties of product:Viscosity (40 DEG C, mm2/ s) 27.3, viscosity (100 DEG C, mm2/ s) 5.38, viscosity index (VI) 135, condensation point<-
50 DEG C, acid number 0.07mgKOH/g.
Embodiment 3
The synthesis of pentaerythrite 3 rich in dimer
475g monopentaerythritols and 7.13g potassium carbonate are added in 5L reactors, the air led in nitrogen displacement kettle, are repeated
4 times.Temperature programming, after temperature is raised to 200 DEG C, it is evacuated down to -0.07MPa, between 240-250 DEG C of keeping temperature, reaction 5 is small
When.Sampling, bipentaerythrite and monopentaerythritol in product are detected by the high performance liquid chromatography with Composition distribution
Ratio be 22/78.
The synthesis of pentaerythritol fatty ester 3 rich in dimer
When above-mentioned reacting liquid temperature drops to 100 DEG C, 1230g n-caproic acids, 218g caprylic acids, 521g are added into reactor
N-capric acid, reactor is closed, led to nitrogen to pressure 0.2MPa, then vacuumize.Repeat this operation 4 times.Then program liter
Temperature maintains the temperature at 220-240 DEG C and reacted 10 hours, reaction pressure is arrived in -0.02MPa between -0.04MPa to 220 DEG C.Reaction
After the completion of, 200 DEG C are maintained the temperature at, is evaporated under reduced pressure and removes unreacted acid, until no acid steams.Reaction solution drops to room temperature
Afterwards, material is released, then adds the DPTA and atlapulgite (mass ratio 1/1) of 5% mass, is heated to 110 DEG C, under nitrogen protection
Stirring 1.5 hours.After the completion of, it is filtrated to get lube base oil.
Properties of product:Viscosity (40 DEG C, mm2/ s) 29.4, viscosity (100 DEG C, mm2/ s) 5.73, viscosity index (VI) 140, condensation point<-
50 DEG C, acid number 0.06mgKOH/g.
Embodiment 4
The synthesis of pentaerythrite 4 rich in dimer
420g monopentaerythritols and 4.2g phosphorous acid are added in 5L reactors, the air led in nitrogen displacement kettle, repeat 4
It is secondary.Temperature programming, after temperature is raised to 170 DEG C, it is evacuated down to -0.05MPa, between 200-240 DEG C of keeping temperature, reaction 1.5
Hour.Sampling, bipentaerythrite and single cropping penta 4 in product are detected by the high performance liquid chromatography with Composition distribution
The ratio of alcohol is 9.5/90.5.
The synthesis of pentaerythritol fatty ester 4 rich in dimer
When above-mentioned reacting liquid temperature drops to 100 DEG C, 566g oleic acid is added into reactor, 466g n-caproic acids, 609g is just
Enanthic acid, 193g caprylic acids, 212g pelargonic acids, 10g butyl titanates, reactor is closed, led to nitrogen to pressure 0.3MPa, then take out
Vacuum.Repeat this operation 4 times.Then temperature programming maintains the temperature at 200-220 DEG C and reacted 10 hours to 200 DEG C, reaction pressure
Power is arrived in -0.03MPa between -0.04MPa.After the completion of reaction, 200 DEG C are maintained the temperature at, is evaporated under reduced pressure and removes unreacted acid,
Until no acid steams.After reaction solution drops to room temperature, material is released, then adds the EDTA and atlapulgite (quality of 4% mass
Than 1/1), being heated to 110 DEG C, stirred under nitrogen atmosphere 1 hour.After the completion of, it is filtrated to get lube base oil.
Properties of product:Viscosity (40 DEG C, mm2/ s) 28.9, viscosity (100 DEG C, mm2/ s) 5.96, viscosity index (VI) 158, condensation point<-
41 DEG C, acid number 0.08mgKOH/g.
Embodiment 5
The synthesis of pentaerythrite 5 rich in dimer
420g monopentaerythritols and 2.1g phosphorous acid are added in 5L reactors, the air led in nitrogen displacement kettle, repeat 4
It is secondary.Temperature programming, after temperature is raised to 100 DEG C, it is evacuated down to -0.05MPa, between 150-180 DEG C of keeping temperature, reaction 10 is small
When.Sampling, bipentaerythrite and monopentaerythritol in product are detected by the high performance liquid chromatography with Composition distribution
Ratio be 9.0/91.0.
The synthesis of pentaerythritol fatty ester 5 rich in dimer
When above-mentioned reacting liquid temperature drops to 100 DEG C, 566g oleic acid is added into reactor, 466g n-caproic acids, 609g is just
Enanthic acid, 193g caprylic acids, 212g pelargonic acids, 10g butyl titanates, reactor is closed, led to nitrogen to pressure 0.3MPa, then take out
Vacuum.Repeat this operation 4 times.Then temperature programming maintains the temperature at 120-150 DEG C and reacted 15 hours to 100 DEG C, reaction pressure
Power is arrived in -0.03MPa between -0.04MPa.After the completion of reaction, 200 DEG C are maintained the temperature at, is evaporated under reduced pressure and removes unreacted acid,
Until no acid steams.After reaction solution drops to room temperature, material is released, then adds the EDTA and atlapulgite (quality of 4% mass
Than 1/1), being heated to 110 DEG C, stirred under nitrogen atmosphere 1 hour.After the completion of, it is filtrated to get lube base oil.
Properties of product:Viscosity (40 DEG C, mm2/ s) 29.1, viscosity (100 DEG C, mm2/ s) 5.94, viscosity index (VI) 155, condensation point<-
41 DEG C, acid number 0.06mgKOH/g.
Embodiment 6
The synthesis of pentaerythrite 6 rich in dimer
420g monopentaerythritols and 21g phosphorous acid are added in 5L reactors, the air led in nitrogen displacement kettle, repeat 4
It is secondary.Temperature programming, after temperature is raised to 170 DEG C, it is evacuated down to -0.05MPa, between 200-240 DEG C of keeping temperature, reaction 1 is small
When.Sampling, bipentaerythrite and monopentaerythritol in product are detected by the high performance liquid chromatography with Composition distribution
Ratio be 8.5/91.5.
The synthesis of pentaerythritol fatty ester 6 rich in dimer
When above-mentioned reacting liquid temperature drops to 100 DEG C, 566g oleic acid is added into reactor, 466g n-caproic acids, 609g is just
Enanthic acid, 193g caprylic acids, 212g pelargonic acids, 10g tributyl phosphates, reactor is closed, logical nitrogen to pressure 0.3MPa, then
Vacuumize.Repeat this operation 4 times.Then temperature programming maintains the temperature at 200-260 DEG C and reacted 2 hours to 200 DEG C, reaction
Pressure is arrived in -0.03MPa between -0.04MPa.After the completion of reaction, 200 DEG C are maintained the temperature at, it is unreacted to be evaporated under reduced pressure removing
Acid, until no acid steams.After reaction solution drops to room temperature, material is released, then adds the EDTA and atlapulgite of 8% mass
(mass ratio 1/1), 150 DEG C are heated to, stirred under nitrogen atmosphere 0.5 hour.After the completion of, it is filtrated to get lube base oil.
Properties of product:Viscosity (40 DEG C, mm2/ s) 28.6, viscosity (100 DEG C, mm2/ s) 5.87, viscosity index (VI) 155, condensation point<-
41 DEG C, acid number 0.08mgKOH/g.
Embodiment 7
The synthesis of pentaerythrite 7 rich in dimer
420g monopentaerythritols and 12.6g phosphorous acid are added in 5L reactors, the air led in nitrogen displacement kettle, are repeated
4 times.Temperature programming, after temperature is raised to 170 DEG C, it is evacuated down to -0.05MPa, between 200-240 DEG C of keeping temperature, reaction 1.5
Hour.Sampling, bipentaerythrite and single cropping penta 4 in product are detected by the high performance liquid chromatography with Composition distribution
The ratio of alcohol is 12/88.
The synthesis of pentaerythritol fatty ester 7 rich in dimer
When above-mentioned reacting liquid temperature drops to 100 DEG C, 566g oleic acid is added into reactor, 466g n-caproic acids, 609g is just
Enanthic acid, 193g caprylic acids, 212g pelargonic acids, 10g butyl titanates, reactor is closed, led to nitrogen to pressure 0.3MPa, then take out
Vacuum.Repeat this operation 4 times.Then temperature programming maintains the temperature at 200-240 DEG C and reacted 6 hours to 150 DEG C, reaction pressure
Power is arrived in -0.03MPa between -0.04MPa.After the completion of reaction, 200 DEG C are maintained the temperature at, is evaporated under reduced pressure and removes unreacted acid,
Until no acid steams.After reaction solution drops to room temperature, material is released, then adds the EDTA and atlapulgite (quality of 4% mass
Than 1/1), being heated to 50 DEG C, stirred under nitrogen atmosphere 2 hours.After the completion of, it is filtrated to get lube base oil.
Properties of product:Viscosity (40 DEG C, mm2/ s) 29.5, viscosity (100 DEG C, mm2/ s) 5.96, viscosity index (VI) 153, condensation point<-
43 DEG C, acid number 0.08mgKOH/g.
Although illustrate and describing the present invention with specific embodiment, but will be appreciated that without departing substantially from the present invention's
Many other change and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (7)
1. a kind of synthetic method of pentaerythrite ester base oil, it is characterised in that comprise the following steps:
Using pentaerythrite as reaction raw materials, catalyst is added, carries out auto polymerization reaction, pentaerythrite of the generation rich in dimer;
In the pentaerythrite rich in dimer, the weight ratio of dipentaerythritol and pentaerythrite is:5-22:95-78;It is described to urge
Agent is phosphoric acid, phosphorous acid, the one or more in sulfuric acid, and quality dosage is the 0.5%-5% of pentaerythrite, the auto polymerization
Reaction is carried out at negative pressure, 100-260 DEG C;
Aliphatic acid or aryl carboxylic acid are added into the pentaerythrite rich in dimer, esterification is carried out, obtains crude product;
The crude product depickling is decolourized, obtains product;
Above-mentioned all reactions are carried out under anaerobic.
2. the synthetic method of pentaerythrite ester base oil according to claim 1, it is characterised in that the auto polymerization reaction
Time be 2-10 hours.
3. the synthetic method of pentaerythrite ester base oil according to claim 1, it is characterised in that the aliphatic acid is
One or more of mixing in C4-C12 saturated acids, oleic acid, isostearic acid, pentaerythrite and aliphatic acid mole rich in dimer
Than being preferably 3-6:1.
4. the synthetic method of pentaerythrite ester base oil according to claim 1, it is characterised in that carrying out the esterification
The one or more of mixing being additionally added during reaction in phosphoric acid, phosphorous acid, butyl titanate, tributyl phosphate.
5. the synthetic method of pentaerythrite ester base oil according to claim 1, it is characterised in that the esterification is
2-15 hours are reacted at negative pressure, 100-260 DEG C.
6. the synthetic method of pentaerythrite ester base oil according to claim 1, it is characterised in that what the depickling was decolourized
Method is:The mixture of at least one of alkali and complexing agent and atlapulgite is added, carries out composite adsorption processing.
7. the synthetic method of pentaerythrite ester base oil according to claim 6, it is characterised in that the complexing agent is ammonia
One or more in triacetic acid sodium, edetate, diethylenetriamine pentacarboxylic acid salt, the complexing agent and the activity
Total addition of carclazyte is the 1%-10% of the crude product quality;The temperature of the composite adsorption processing is 50-150 DEG C, the time
For 0.5-2 hours.
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CN115449418B (en) * | 2022-09-29 | 2023-12-01 | 国网湖南省电力有限公司 | Fireproof insulating oil |
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