CN106635432A - Method for preparing vegetable insulating oil by utilizing swill oil - Google Patents
Method for preparing vegetable insulating oil by utilizing swill oil Download PDFInfo
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- CN106635432A CN106635432A CN201611055278.4A CN201611055278A CN106635432A CN 106635432 A CN106635432 A CN 106635432A CN 201611055278 A CN201611055278 A CN 201611055278A CN 106635432 A CN106635432 A CN 106635432A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
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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
- C10M109/00—Lubricating compositions characterised by the base-material being a compound of unknown or incompletely defined constitution
- C10M109/02—Reaction products
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
- C11C1/10—Refining by distillation
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/10—Ester interchange
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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
- C10N2040/14—Electric or magnetic purposes
- C10N2040/16—Dielectric; Insulating oil or insulators
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Abstract
The invention relates to the technical field of swill oil utilization, and particularly discloses a method for preparing vegetable insulating oil by utilizing swill oil. According to the preparation method, interesterification is carried out on swill oil and ethanol by adopting refined swill oil as a main raw material, ethanol as a reacting raw material, KOH or NaOH as a catalyst and phosphoric acid as a neutralizing agent to reduce the viscosity of swill oil and remove impurities in the swill oil so as to obtain high-purity fatty acid ethyl ester; then, fatty acid ethyl ester serving as a main raw material reacts with a reaction raw material neopentylene glycol by using monobutyltin oxide as a catalyst, diatomite, carclazyte and activated carbon as filtering agents and nitrogen as a protective gas to prepare high-quality vegetable insulating oil through a refining process. The method has the advantages that the insulating oil is prepared by utilizing swill oil, waste resources are reasonably utilized, energy can be furthest utilized, the environment can be protected, and the production cost can be reduced. The performance of the vegetable insulating oil synthesized by the method has remarkable advantages in comparison with that of mineral oil and imported vegetable insulating oil.
Description
Technical field
The present invention relates to swill oil utilizes technical field, the side that a kind of utilization swill oil produces vegetable insulating oil is particularly related to
Method.
Background technology
Insulating oil is a kind of important liquid insulating material, is mainly used in various reactors, transformer, oil-immersed type power and becomes
In the power equipments such as depressor, by impregnating and filling the air gap in abatement apparatus, play a part of to improve insulation electrical intensity, together
When can improve the heat dispersion of equipment, have directly impact on the safe operation of power system.
At present insulating oil widest used in various countries' power equipment is mineral insulating oil, mineral insulating oil be mainly by
Natural oil refining.The electric insulating quality and cooling performance of mineral insulating oil is good, and cost is not also high, therefore in oil immersion
There is the applicating history of more than 100 years in insulating power equipment.But with the raising to the various performance requirements of insulating oil, mineral insulation
Also there are many shortcomings in oil, such as：Flash-point is relatively low, and fire protecting performance is poor；Biodegradability is poor, pollutes the environment during leakage；Can not
Regeneration etc..
Under the situation of petroleum resources worsening shortages, developing a kind of green, the novel insulating oil of environmental protection becomes everybody concern
Focus.Wherein, the insulating oil with vegetable oil as raw material because its environment friendly and recyclability cause again many science works
The attention of author.
At present major part is all processing insulating oil, equally to consume resource with vegetable oil as raw material, and high cost is limited
Its application prospect.Nowadays it is more and more to the investigative technique of swill oil, the technical value that swill oil is converted into new product must be ground
Study carefully, waste resource is rationally utilized.
The content of the invention
The present invention is intended to provide a kind of method that utilization swill oil produces vegetable insulating oil, by entering with ethanol to swill oil
Row ester exchange, obtains high-purity fatty-acid ethyl ester, by fatty-acid ethyl ester and season pentanediol reaction, through refining step height is obtained
The vegetable insulating oil of quality, performance is with the obvious advantage compared with mineral oil and imported plants insulating oil.
To achieve these goals, present invention employs following technical scheme：One kind is exhausted using swill oil production plant
The method of edge oil, comprises the steps of：
A () prepares fatty-acid ethyl ester by main material of swill oil；
B () prepares vegetable insulating oil by main material of fatty-acid ethyl ester.
Above-mentioned steps a are specifically comprised the steps of：
1) raw material is chosen：With refined swill oil as main material, reaction raw materials are ethanol, catalyst is KOH or NaOH, neutralization
Reagent is phosphoric acid；
2) above-mentioned raw materials are added in fatty-acid ethyl ester reactor, ethanol addition account for the 10% of water from washing rice weight of oil to
15%, catalyst loading accounts for the 0.1% to 0.15% of water from washing rice weight of oil, and temperature is adjusted to 65 DEG C, quick stirring, in fatty acid
Ethyl ester reaction kettle for reaction 1 hour, precipitation stands 2 hours, partial glycerol under releasing in fatty-acid ethyl ester reactor, retains
Upper strata；
3) ethanol and catalyst are added again：Ethanol addition accounts for the 10% to 15% of water from washing rice weight of oil, catalyst addition
Amount accounts for the 0.05% to 0.15% of water from washing rice weight of oil, and temperature is 65 DEG C, quick stirring, in fatty-acid ethyl ester reaction kettle for reaction
Between be 1-2 hours；
4) phosphoric acid is added in fatty-acid ethyl ester reactor, fine setting PH to 7 (neutrality), precipitation stands 5 hours, under releasing
Layer glycerol and alcohol mixture, retain upper strata, and upper strata is the croude fatty acids ethyl ester containing ethanol；
5) ethanol in the croude fatty acids ethyl ester containing ethanol is removed：By the thick fat containing ethanol of fatty-acid ethyl ester reactor
Fat acetoacetic ester is pumped in flash tank, continuous circulation, is 100 DEG C in temperature, and pressure is under the vacuum state of -0.1MPa, to maintain 1
Individual hour, the gas flashed off from flash tank filters out impurity through filter, that is, obtain croude fatty acids ethyl ester；
6) croude fatty acids ethyl ester distillation：Croude fatty acids ethyl ester is through gassing tank, bubbing impurity, subsequently into distillation column
In, vacuum is 50Pa～60Pa, takes distillation i.e. fatty-acid ethyl ester.
Above-mentioned steps b are specifically comprised the steps of：
1) raw material is chosen：With fatty-acid ethyl ester as main material, reaction raw materials are season pentanediol, and catalyst is monobutyl oxidation
Stannum, filtering agent is kieselguhr, hargil, activated carbon；
2) with nitrogen as shielding gas, first it is passed through in nitrogen displacement season pentanediol di fatty acid ester reactor, pipeline and line
Air on road in equipment, makes the air in equipment, pipeline thoroughly replace；
3) fatty-acid ethyl ester, season pentanediol, catalyst, filtering agent are added to into season pentanediol di fatty acid ester reactor
In, season pentanediol addition account for the 14% of fatty-acid ethyl ester weight, holding is passed through nitrogen as shielding gas, and temperature adjusts 185 to 190
DEG C, under vacuum conditions, quick stirring makes each component in season 3 hours of pentanediol di fatty acid ester reaction kettle for reaction；
4) material in above-mentioned season pentanediol di fatty acid ester reactor is pumped in removing impurities tank, holding is passed through nitrogen
Used as shielding gas, temperature is 190 DEG C, and vacuum is 30Pa or so, steam fatty-acid ethyl ester, season pentanediol monoesters, catalyst with
And season pentanediol, lower the temperature and obtain thick season pentanediol di fatty acid ester；
5) thick season pentanediol di fatty acid ester obtained above enters the first Hi-mixer, while phosphoric acid is added, control
In 3-5, subsequently into acid reaction kettle, temperature is 85 DEG C to pH value, and a hour is reacted in acid reaction kettle；
6) into the second Hi-mixer, while 10% sig water for accounting for fatty-acid ethyl ester weight is added, it is high through second
After effect blender mixing, into alkali reaction kettle, the alkali liquor that concentration is 1%～2% is added, temperature is 85 DEG C, quick stirring, in alkali
One hour of reaction kettle for reaction, through centrifuge water, colloid, soap and impurity are removed；
7) through the 3rd Hi-mixer, addition accounts for 10% deionized water of fatty-acid ethyl ester weight, and temperature is 85 DEG C, soon
Speed stirring, in one hour of water reaction kettle for reaction, through centrifuge water and impurity is removed；
8) subsequently into flash tank, temperature is upgraded to into 100 DEG C, vacuum is -0.1MPa, and through flash tank moisture content is removed；
9) material in flash tank is pumped in filtration mixing kettle, quick stirring, addition accounts for fatty-acid ethyl ester weight
1% hargil, 1% activated carbon, 1% kieselguhr, temperature is adjusted to 85 DEG C, adsorption reaction half an hour, filters through filter
Obtain season pentanediol di fatty acid ester；
10) superheated steam is passed through, is warmed up to 210 DEG C, vacuum is 200Pa or so, and the air stripping in stripping tower removes low-carbon (LC)
Even impurity, abnormal smells from the patient, through filter colourless, tasteless season pentanediol di fatty acid ester is obtained, and obtains vegetable insulating oil.
Further, steam it has been passed through in the acid reaction kettle, alkali reaction kettle, water reactor.
Further, the step 9) repeatedly.
Wherein, the acid value of the refined swill oil is anhydrous without miscellaneous within 1mgKOH/g.
The beneficial effects of the present invention is：The insulating oil of this method production is refined by swill oil and obtained, without noxious substance,
Environment and human body will not be damaged, can be rapidly biodegradable, be a kind of environment-friendly type insulated liquid；
Insulating oil is produced using swill oil, rationally using waste resource, the energy is maximally utilized, while also protecting
Environment, reduces production cost；
The vegetable insulating oil synthesized by this method is lower than mineral oil viscosity, only 0.6 times of mineral oil；Compare mineral
The flash-point of oil is higher, is 1.2 times of mineral oil；The close insulating paper of relative dielectric constant, can expect by adjust dielectric constant come
Improve the special energy of insulation.
Specific embodiment
Below in conjunction with embodiments of the invention, the technical scheme in the embodiment of the present invention is clearly and completely retouched
State, it is clear that described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.Based on the present invention
In embodiment, the every other enforcement that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example, belongs to the scope of protection of the invention.
Embodiment 1
A kind of method that utilization swill oil produces vegetable insulating oil, comprises the steps of：
A () prepares fatty-acid ethyl ester by main material of swill oil：
1) raw material is chosen：With refined swill oil (acid value is anhydrous without miscellaneous within 1mgKOH/g) for main material, reaction raw materials
For ethanol, catalyst be KOH, neutralization reagent be phosphoric acid；
2) above-mentioned raw materials are added in fatty-acid ethyl ester reactor, ethanol addition accounts for 10%, KOH of water from washing rice weight of oil
Addition accounts for the 0.1% of water from washing rice weight of oil, and temperature is adjusted to 65 DEG C, is stirred with 60 revs/min of mixing speed, makes each component in fat
Fat acetoacetic ester reaction kettle for reaction 1 hour, precipitation stands 2 hours, partial glycerol under releasing in fatty-acid ethyl ester reactor,
Retain upper strata；
3) ethanol and catalyst are added again：Ethanol addition accounts for 10%, the KOH additions of water from washing rice weight of oil and accounts for swill oil
The 0.05% of weight, temperature is adjusted to 65 DEG C, is stirred with 60 revs/min of mixing speed, each raw material is reacted in fatty-acid ethyl ester
The response time is 1 hour in kettle；
4) in fatty-acid ethyl ester reactor, micro phosphoric acid adjustment PH to 7 (neutrality), precipitation is added to stand 5 hours, put
Go out lower floor's glycerol and alcohol mixture, retain upper strata, upper strata is the croude fatty acids ethyl ester containing ethanol；
5) ethanol in the croude fatty acids ethyl ester containing ethanol is removed：By the thick fat containing ethanol of fatty-acid ethyl ester reactor
Fat acetoacetic ester is pumped in flash tank, continuous circulation, is 100 DEG C in temperature, and pressure is under the vacuum state of -0.1MPa, to maintain 1
Individual hour, the gas flashed off from flash tank filters out trace impurity through filter, that is, obtain croude fatty acids ethyl ester；
6) croude fatty acids ethyl ester distillation：Croude fatty acids ethyl ester separates out minimum gas impurity, subsequently into steaming through gassing tank
In evaporating tower, pressure is adjusted to 50Pa, takes distillation i.e. fatty-acid ethyl ester.
Front-end volatiles, bottom of towe dirty oil are side-product, and we only take midbarrel product, this product index：Appearance colorless, depletion of QI
Taste, acid value 0.17mgKOH/g or so, ester content are more than 99%.
By carrying out ester exchange to swill oil and ethanol, the viscosity of swill oil is reduced, remove the impurity in swill oil, obtained
High-purity fatty-acid ethyl ester, for future use.
As preferred：Catalyst can also be adopted as NaOH, measure identical with KOH.
B () prepares vegetable insulating oil by main material of fatty-acid ethyl ester：
1) raw material is chosen：With fatty-acid ethyl ester as main material, reaction raw materials are season pentanediol, and catalyst is monobutyl oxidation
Stannum, filtering agent is kieselguhr, hargil, activated carbon；
2) with nitrogen as shielding gas, first it is passed through in a large amount of nitrogen displacement season pentanediol di fatty acid ester reactors, pipeline
And the air on circuit in equipment, the air in equipment, pipeline is thoroughly replaced；
3) fatty-acid ethyl ester, season pentanediol, catalyst, filtering agent are added to into season pentanediol di fatty acid ester reactor
In, season pentanediol addition account for the 14% of fatty-acid ethyl ester weight, holding is passed through extremely trace nitrogen gas as shielding gas, and temperature is adjusted
185 DEG C, vacuum is micro-vacuum, is stirred with 60 revs/min of mixing speed, makes each component in season pentanediol di fatty acid ester reaction
3 hours are reacted in kettle；
4) material in above-mentioned season pentanediol di fatty acid ester reactor is pumped in removing impurities tank, holding is passed through extremely micro-
Used as shielding gas, temperature is adjusted to 190 DEG C to amount nitrogen, and vacuum is micro-vacuum, and vacuum is 30Pa or so, steams excess fatty acids
Ethyl ester, a small amount of season pentanediol monoesters, and micro catalyst, season pentanediol, cooling obtains thick season pentanediol difatty acid
Ester；
5) by thick season pentanediol di fatty acid ester obtained above through the first Hi-mixer, micro phosphoric acid, control are added
PH value processed enters acid reaction kettle after 3-5, mixing, and temperature is 85 DEG C, and a hour is reacted in acid reaction kettle；
6) 10% sig water for accounting for fatty-acid ethyl ester weight is added, through the second Hi-mixer, addition concentration is 1% alkali
Liquid, enters alkali reaction kettle after mixing, temperature is 85 DEG C, is stirred with 40 revs/min of mixing speed, and one is reacted in alkali reaction kettle
Hour, remove water, colloid, soap and impurity through centrifuge；
7) through the 3rd Hi-mixer, addition accounts for 10% deionized water of fatty-acid ethyl ester weight, and water is entered after mixing
Reactor, temperature is 85 DEG C, is stirred with 60 revs/min of mixing speed, in one hour of water reaction kettle for reaction, through centrifuge
Remove water and impurity；
8) flash tank is entered, temperature is upgraded to into 100 DEG C, vacuum is -0.1MPa, and through flash tank moisture content is removed；
9) material in flash tank is pumped in filtration mixing kettle, is stirred with 60 revs/min of mixing speed, addition accounts for fat
The hargil of the 1% of fat acetoacetic ester weight, 1% activated carbon, 1% kieselguhr, temperature is adjusted to 85 DEG C, little half of adsorption reaction
When, it is filtrated to get season pentanediol di fatty acid ester through filter；
10) micro superheated steam 1.0MPa is passed through, 210 DEG C are warmed up to, vacuum is 200Pa or so, in stripping tower
Air stripping, goes out except low-carbon (LC) connects impurity, abnormal smells from the patient, and polished bag filter obtains that finished product is colourless, tasteless season pentanediol difatty acid
Ester, obtains vegetable insulating oil.
Embodiment 2
A kind of method that utilization swill oil produces vegetable insulating oil, comprises the steps of：
A () prepares fatty-acid ethyl ester by main material of swill oil：
1) raw material is chosen：With refined swill oil (acid value is anhydrous without miscellaneous within 1mgKOH/g) for main material, reaction raw materials
For ethanol, catalyst be KOH, neutralization reagent be phosphoric acid；
2) above-mentioned raw materials are added in fatty-acid ethyl ester reactor, ethanol addition accounts for 15%, KOH of water from washing rice weight of oil
Addition accounts for the 0.15% of water from washing rice weight of oil, and temperature is adjusted to 65 DEG C, is stirred with 60 revs/min of mixing speed, makes each component exist
Fatty-acid ethyl ester reaction kettle for reaction 1 hour, precipitation stands 2 hours, and part is sweet under releasing in fatty-acid ethyl ester reactor
Oil, retains upper strata；
3) ethanol and catalyst are added again：Ethanol addition accounts for 15%, the KOH additions of water from washing rice weight of oil and accounts for swill oil
The 0.15% of weight, temperature is adjusted to 65 DEG C, is stirred with 60 revs/min of mixing speed, each raw material is reacted in fatty-acid ethyl ester
The response time is 2 hours in kettle；
4) in fatty-acid ethyl ester reactor, micro phosphoric acid adjustment PH to 7 (neutrality), precipitation is added to stand 5 hours, put
Go out lower floor's glycerol and alcohol mixture, retain upper strata, upper strata is the croude fatty acids ethyl ester containing ethanol；
5) ethanol in the croude fatty acids ethyl ester containing ethanol is removed：By the thick fat containing ethanol of fatty-acid ethyl ester reactor
Fat acetoacetic ester is pumped in flash tank, continuous circulation, is 100 DEG C in temperature, and pressure is under the vacuum state of -0.1MPa, to maintain 1
Individual hour, the gas flashed off from flash tank filters out trace impurity through filter, that is, obtain croude fatty acids ethyl ester；
6) croude fatty acids ethyl ester distillation：Croude fatty acids ethyl ester separates out minimum gas impurity, subsequently into steaming through gassing tank
In evaporating tower, pressure is adjusted to 60Pa, takes distillation i.e. fatty-acid ethyl ester.
Front-end volatiles, bottom of towe dirty oil are side-product, and we only take midbarrel product, this product index：Appearance colorless, depletion of QI
Taste, acid value 0.17mgKOH/g or so, ester content are more than 99%.
By carrying out ester exchange to swill oil and ethanol, the viscosity of swill oil is reduced, remove the impurity in swill oil, obtained
High-purity fatty-acid ethyl ester, for future use.
As preferred：Catalyst can also be adopted as NaOH, measure identical with KOH.
B () prepares vegetable insulating oil by main material of fatty-acid ethyl ester：
1) raw material is chosen：With fatty-acid ethyl ester as main material, reaction raw materials are season pentanediol, and catalyst is monobutyl oxidation
Stannum, filtering agent is kieselguhr, hargil, activated carbon；
2) with nitrogen as shielding gas, first it is passed through in a large amount of nitrogen displacement season pentanediol di fatty acid ester reactors, pipeline
And the air on circuit in equipment, the air in equipment, pipeline is thoroughly replaced；
3) fatty-acid ethyl ester, season pentanediol, catalyst, filtering agent are added to into season pentanediol di fatty acid ester reactor
In, season pentanediol addition account for the 14% of fatty-acid ethyl ester weight, holding is passed through extremely trace nitrogen gas as shielding gas, and temperature is adjusted
190 DEG C, vacuum is micro-vacuum, is stirred with 60 revs/min of mixing speed, makes each component in season pentanediol di fatty acid ester reaction
3 hours are reacted in kettle；
4) material in above-mentioned season pentanediol di fatty acid ester reactor is pumped in removing impurities tank, holding is passed through extremely micro-
Used as shielding gas, temperature is adjusted to 190 DEG C to amount nitrogen, and vacuum is micro-vacuum, and vacuum is 30Pa or so, steams excess fatty acids
Ethyl ester, a small amount of season pentanediol monoesters, and micro catalyst, season pentanediol, cooling obtains thick season pentanediol difatty acid
Ester；
5) by thick season pentanediol di fatty acid ester obtained above through the first Hi-mixer, micro phosphoric acid, control are added
PH value processed enters acid reaction kettle after 3-5, mixing, and temperature is 85 DEG C, and a hour is reacted in acid reaction kettle；
6) 10% sig water for accounting for fatty-acid ethyl ester weight is added, through the second Hi-mixer, addition concentration is 2% alkali
Liquid, enters alkali reaction kettle after mixing, temperature is 85 DEG C, is stirred with 40 revs/min of mixing speed, and one is reacted in alkali reaction kettle
Hour, remove water, colloid, soap and impurity through centrifuge；
7) through the 3rd Hi-mixer, addition accounts for 10% deionized water of fatty-acid ethyl ester weight, and water is entered after mixing
Reactor, temperature is 85 DEG C, is stirred with 60 revs/min of mixing speed, in one hour of water reaction kettle for reaction, through centrifuge
Remove water and impurity；
8) flash tank is entered, temperature is upgraded to into 100 DEG C, vacuum is -0.1MPa, and through flash tank moisture content is removed；
9) material in flash tank is pumped in filtration mixing kettle, is stirred with 60 revs/min of mixing speed, addition accounts for fat
The hargil of the 1% of fat acetoacetic ester weight, 1% activated carbon, 1% kieselguhr, temperature is adjusted to 85 DEG C, little half of adsorption reaction
When, it is filtrated to get season pentanediol di fatty acid ester through filter；
11) micro superheated steam 1.0MPa is passed through, 210 DEG C are warmed up to, vacuum is 200Pa or so, in stripping tower
Air stripping, goes out except low-carbon (LC) connects impurity, abnormal smells from the patient, and polished bag filter obtains that finished product is colourless, tasteless season pentanediol difatty acid
Ester, obtains vegetable insulating oil.
Step 9) repeatedly, i.e., repeatedly through filtering mixing kettle and filter process, in order to filter more abundant.
This section obtains the vegetable insulating oil of high-quality by fatty-acid ethyl ester and season pentanediol reaction through refining step,
Performance is with the obvious advantage compared with mineral oil and imported plants insulating oil.
The vegetable insulating oil synthesized by this method is lower than mineral oil viscosity, only 0.6 times of mineral oil；Compare mineral
The flash-point of oil is higher, is 1.2 times of mineral oil；The close insulating paper of relative dielectric constant, can expect by adjust dielectric constant come
The special energy of insulation is improved, the vegetable insulating oil performance advantage processed by the visible this method of this table is obvious.
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (6)
1. a kind of method that utilization swill oil produces vegetable insulating oil, it is characterised in that comprise the steps of：
（a）Fatty-acid ethyl ester is prepared by main material of swill oil；
（b）Vegetable insulating oil is prepared by main material of fatty-acid ethyl ester.
2. utilization swill oil according to claim 1 into produce vegetable insulating oil method, it is characterised in that above-mentioned steps a
Specifically comprise the steps of：
1）Choose raw material：With refined swill oil as main material, reaction raw materials are ethanol, catalyst is KOH or NaOH, neutralization examination
Agent is phosphoric acid；
2）Above-mentioned raw materials are added in fatty-acid ethyl ester reactor, ethanol addition accounts for the 10% to 15% of water from washing rice weight of oil,
Catalyst loading accounts for the 0.1% to 0.15% of water from washing rice weight of oil, and temperature is adjusted to 65 DEG C, quick stirring, in fatty-acid ethyl ester
Reaction kettle for reaction 1 hour, precipitation stands 2 hours, partial glycerol under releasing in fatty-acid ethyl ester reactor, in reservation
Layer；
3）Add ethanol and catalyst again：Ethanol addition accounts for the 10% to 15% of water from washing rice weight of oil, and catalyst loading is accounted for
The 0.05% to 0.15% of water from washing rice weight of oil, temperature is 65 DEG C, quick stirring, is in the fatty-acid ethyl ester reaction kettle for reaction time
1-2 hours；
4）Phosphoric acid is added in fatty-acid ethyl ester reactor, PH to 7 is finely tuned（It is neutral）, precipitate and stand 5 hours, release lower floor sweet
Oil and alcohol mixture, retain upper strata, and upper strata is the croude fatty acids ethyl ester containing ethanol；
5）Ethanol in croude fatty acids ethyl ester containing ethanol is removed：By the croude fatty acids containing ethanol of fatty-acid ethyl ester reactor
Ethyl ester is pumped in flash tank, continuous circulation, is 100 DEG C in temperature, and pressure is that under the vacuum state of -0.1MPa, maintenance 1 is little
When, the gas flashed off from flash tank filters out impurity through filter, that is, obtain croude fatty acids ethyl ester；
6）Croude fatty acids ethyl ester distills：Croude fatty acids ethyl ester through gassing tank, bubbing impurity, subsequently into distillation column in,
Vacuum is 50Pa ~ 60Pa, takes distillation i.e. fatty-acid ethyl ester.
3. utilization swill oil according to claim 1 and 2 into produce vegetable insulating oil method, it is characterised in that above-mentioned step
Rapid b is specifically comprised the steps of：
1）Choose raw material：With fatty-acid ethyl ester as main material, reaction raw materials are season pentanediol, and catalyst is Mono-n-butyltin,
Filtering agent is kieselguhr, hargil, activated carbon；
2）With nitrogen as shielding gas, first it is passed through in nitrogen displacement season pentanediol di fatty acid ester reactor, on pipeline and circuit
Air in equipment, makes the air in equipment, pipeline thoroughly replace；
3）Fatty-acid ethyl ester, season pentanediol, catalyst, filtering agent are added in season pentanediol di fatty acid ester reactor, season
Pentanediol addition accounts for the 14% of fatty-acid ethyl ester weight, and holding is passed through nitrogen as shielding gas, and temperature adjusts 185 to 190 DEG C,
Under vacuum state, quick stirring makes each component in season 3 hours of pentanediol di fatty acid ester reaction kettle for reaction；
4）Material in above-mentioned season pentanediol di fatty acid ester reactor is pumped in removing impurities tank, holding is passed through nitrogen as guarantor
Shield gas, temperature is 190 DEG C, and vacuum is 25-30Pa, steams fatty-acid ethyl ester, season pentanediol monoesters, catalyst and season penta 2
Alcohol, cooling obtains thick season pentanediol di fatty acid ester；
5）Thick season pentanediol di fatty acid ester obtained above enters the first Hi-mixer, while adding phosphoric acid, controls pH value
In 3-5, subsequently into acid reaction kettle, temperature is 85 DEG C, and a hour is reacted in acid reaction kettle；
6）Into the second Hi-mixer, while 10% sig water for accounting for fatty-acid ethyl ester weight is added, it is efficiently mixed through second
After clutch mixing, into alkali reaction kettle, the alkali liquor that concentration is 1% ~ 2% is added, temperature is 85 DEG C, quick stirring, in alkali reaction
A hour is reacted in kettle, through centrifuge water, colloid, soap and impurity are removed；
7）Through the 3rd Hi-mixer, addition accounts for 10% deionized water of fatty-acid ethyl ester weight, and temperature is 85 DEG C, is quickly stirred
Mix, in one hour of water reaction kettle for reaction, through centrifuge water and impurity are removed；
8）Subsequently into flash tank, temperature is upgraded to into 100 DEG C, vacuum is -0.1MPa, and through flash tank moisture content is removed；
9）Filter：Material in flash tank is pumped in filtration mixing kettle, quick stirring, addition accounts for fatty-acid ethyl ester weight
1% hargil, 1% activated carbon, 1% kieselguhr, temperature is adjusted to 85 DEG C, adsorption reaction half an hour, filters through filter
Obtain season pentanediol di fatty acid ester；
10）Superheated steam is passed through, 210 DEG C are warmed up to, vacuum is 180-210Pa, the air stripping in stripping tower, removed low-carbon (LC) and connect miscellaneous
Matter, abnormal smells from the patient, through filter colourless, tasteless season pentanediol di fatty acid ester is obtained, and obtains vegetable insulating oil.
4. utilization swill oil according to claim 3 into produce vegetable insulating oil method, it is characterised in that the acid reaction
Steam has been passed through in kettle, alkali reaction kettle, water reactor.
5. utilization swill oil according to claim 3 into produce vegetable insulating oil method, it is characterised in that the step 9）
Repeatedly.
6. utilization swill oil according to claim 2 into produce vegetable insulating oil method, it is characterised in that the refined water from washing rice
The acid value of water oil is anhydrous without miscellaneous within 1mgKOH/g.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113186031A (en) * | 2020-11-11 | 2021-07-30 | 广东电网有限责任公司 | Pour point depressing process for preparing kitchen waste grease-based natural ester insulating oil |
| CN113528236A (en) * | 2021-06-29 | 2021-10-22 | 江西尊创新能源有限公司 | Method for removing colloid in hogwash oil |
| CN113817525A (en) * | 2021-09-22 | 2021-12-21 | 西安交通大学 | Preparation method of natural ester insulating oil |
-
2016
- 2016-11-25 CN CN201611055278.4A patent/CN106635432A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113186031A (en) * | 2020-11-11 | 2021-07-30 | 广东电网有限责任公司 | Pour point depressing process for preparing kitchen waste grease-based natural ester insulating oil |
| CN113528236A (en) * | 2021-06-29 | 2021-10-22 | 江西尊创新能源有限公司 | Method for removing colloid in hogwash oil |
| CN113817525A (en) * | 2021-09-22 | 2021-12-21 | 西安交通大学 | Preparation method of natural ester insulating oil |
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