CN114045186A - Illegal cooking oil base insulating oil and preparation method thereof - Google Patents
Illegal cooking oil base insulating oil and preparation method thereof Download PDFInfo
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- CN114045186A CN114045186A CN202111272096.3A CN202111272096A CN114045186A CN 114045186 A CN114045186 A CN 114045186A CN 202111272096 A CN202111272096 A CN 202111272096A CN 114045186 A CN114045186 A CN 114045186A
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- oil
- illegal cooking
- cooking oil
- heating
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- 239000008162 cooking oil Substances 0.000 title claims abstract description 224
- 239000003921 oil Substances 0.000 title claims abstract description 169
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 65
- 239000003513 alkali Substances 0.000 claims abstract description 62
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000010438 heat treatment Methods 0.000 claims abstract description 54
- 238000003756 stirring Methods 0.000 claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 27
- 238000005406 washing Methods 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 20
- 239000004927 clay Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 230000018044 dehydration Effects 0.000 claims abstract description 15
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 15
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000002585 base Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 37
- 239000000126 substance Substances 0.000 claims description 31
- 238000004332 deodorization Methods 0.000 claims description 29
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 12
- 230000002378 acidificating effect Effects 0.000 claims description 11
- 230000003472 neutralizing effect Effects 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 abstract description 21
- 238000009413 insulation Methods 0.000 abstract 1
- 235000019198 oils Nutrition 0.000 description 136
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 26
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 26
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 26
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 26
- 239000005642 Oleic acid Substances 0.000 description 26
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 26
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 26
- 238000009874 alkali refining Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- 230000000694 effects Effects 0.000 description 8
- 239000012535 impurity Substances 0.000 description 7
- 239000002699 waste material Substances 0.000 description 7
- 238000011160 research Methods 0.000 description 6
- 238000004821 distillation Methods 0.000 description 4
- 235000021190 leftovers Nutrition 0.000 description 4
- 238000007670 refining Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000004042 decolorization Methods 0.000 description 3
- 230000001877 deodorizing effect Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 208000034699 Vitreous floaters Diseases 0.000 description 2
- 239000010775 animal oil Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 238000001935 peptisation Methods 0.000 description 2
- 235000015277 pork Nutrition 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 description 2
- 239000008158 vegetable oil Substances 0.000 description 2
- 210000001835 viscera Anatomy 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 235000019484 Rapeseed oil Nutrition 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003225 biodiesel Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000002781 deodorant agent Substances 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000010696 ester oil Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 235000019387 fatty acid methyl ester Nutrition 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000021281 monounsaturated fatty acids Nutrition 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
- C11B3/14—Refining fats or fatty oils by distillation with the use of indifferent gases or vapours, e.g. steam
-
- 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- 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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/40—Fatty vegetable or animal oils
- C10M2207/401—Fatty vegetable or animal oils used as base material
-
- 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
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/08—Resistance to extreme temperature
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
- Lubricants (AREA)
- Edible Oils And Fats (AREA)
Abstract
The invention provides a trench oil-based insulating oil and a preparation method thereof, wherein the preparation method comprises the following steps: mixing the illegal cooking oil with phosphoric acid, heating, stirring, reacting, standing, separating out water phase, taking out oil phase, and removing water; heating the illegal cooking oil to 108-115 ℃ under vacuum, and introducing steam for stripping for 25-30 min; then heating the illegal cooking oil to 205-210 ℃, and carrying out steam stripping for 25-35 min; then heating the illegal cooking oil to 220-230 ℃, and continuously carrying out steam stripping for 50-60 min; cooling the trench oil under vacuum; mixing the illegal cooking oil with active carbon and activated clay, stirring and decoloring in vacuum, and filtering; heating the illegal cooking oil, mixing the illegal cooking oil with alkali liquor, stirring and reacting for 2-3 h, then heating to 70-90 ℃, standing for 8-10 h, separating out a water phase, and taking an oil phase to obtain an alkali refined oil sample; and (3) washing the alkali refined oil sample with water, performing vacuum dehydration and performing heat filtration in sequence. The illegal cooking oil base insulation oil disclosed by the invention is low in acid value, low in pour point, low in viscosity and good in electrical performance.
Description
Technical Field
The invention relates to the technical field, in particular to a trench oil-based insulating oil and a preparation method thereof.
Background
Drainage oil can be divided into three categories: the first is narrow-sense swill oil, namely oil obtained by simply processing and refining greasy floaters in a sewer or leftovers and leftovers (generally called swill) of hotels and restaurants; second, the inferior pork, pig's viscera, pigskin process and oil produced after refining; and thirdly, the oil used for frying the food is reused after being used for a certain number of times or is reused after being added with some new oil.
At present, the comprehensive utilization of the illegal cooking oil in China mainly has three modes: firstly, the swill-cooked dirty oil is simply processed and purified and directly used as low-grade industrial oleic acid, stearic acid, industrial grease and the like; secondly, the illegal cooking oil is used for preparing the phosphorus-free washing powder; thirdly, the illegal cooking oil is alcoholyzed to prepare the biodiesel (fatty acid methyl ester).
The main component of the illegal cooking oil is fatty acid triglyceride, and the illegal cooking oil is mainly natural ester oil consisting of animal oil and vegetable oil. The illegal cooking oil has higher flash point and ignition point characteristics than mineral oil, so that the illegal cooking oil has better safety in operation, treatment, storage and transportation, and ensures the operation safety of the illegal cooking oil used as insulating oil for transformers. Therefore, illegal cooking oil is commonly used as the insulating oil of the transformer.
However, since the drainage oil is mainly used animal oil and vegetable oil, the drainage oil has the disadvantages of high pour point and high dielectric loss compared with the unused grease such as rapeseed oil and soybean oil; meanwhile, compared with mineral oil, the illegal cooking oil has higher condensation point or pour point, higher viscosity and poorer electrical performance.
Disclosure of Invention
Therefore, the illegal cooking oil-based insulating oil and the preparation method thereof are needed to solve the problems of high pour point and poor electrical performance of the illegal cooking oil.
In order to solve the problems, the invention provides the following technical scheme:
according to an aspect of the present invention, there is provided a method of preparing a trench oil-based insulating oil, comprising the steps of:
step 1): mixing the illegal cooking oil with phosphoric acid, heating, stirring, reacting, standing, separating out a water phase, and removing water from an oil phase to obtain degummed illegal cooking oil;
step 2): heating the degummed illegal cooking oil to 108-115 ℃ under a vacuum condition, and introducing steam for steam stripping for 25-30 min; heating the degummed illegal cooking oil to 205-210 ℃, and introducing steam for steam stripping for 25-35 min; then heating the degummed illegal cooking oil to 220-230 ℃, and continuously introducing steam for steam stripping for 50-60 min; cooling the degummed illegal cooking oil under a vacuum condition to obtain deodorized illegal cooking oil;
step 3): mixing the deodorized illegal cooking oil with active carbon and activated clay, stirring and decoloring in vacuum, and then filtering to obtain decolored illegal cooking oil;
step 4): heating the decolored illegal cooking oil to 40-55 ℃, mixing the decolored illegal cooking oil with alkali liquor, stirring and reacting for 2-3 hours, then heating to 70-90 ℃, standing for 8-10 hours, separating out a water phase, and taking an oil phase to obtain an alkali refined oil sample;
step 5): and sequentially carrying out water washing, vacuum dehydration and heat filtration on the alkali refined oil sample to obtain the illegal cooking oil base insulating oil.
In some embodiments, in the step 2), the steam-feeding stripping step is: heating the degummed illegal cooking oil to 110 ℃ under the vacuum condition, and introducing steam for steam stripping for 30 min; heating the degummed illegal cooking oil to 210 ℃, and introducing steam for steam stripping for 30 min; and then heating the degummed illegal cooking oil to 225 ℃, and continuously introducing steam for steam stripping for 60 min.
In some embodiments, in the step 2), the steam-feeding stripping step is: and injecting the degummed illegal cooking oil into a deodorization tower, and introducing steam from the bottom of the deodorization tower to strip the degummed illegal cooking oil.
In some embodiments, in the step 3), the amount of the activated carbon is 1.8-2% of the volume of the deodorized illegal cooking oil, the amount of the activated clay is 3.5-4% of the volume of the deodorized illegal cooking oil, and the time for vacuum stirring and decoloring is 1.8-2 h.
In some embodiments, in the step 4), the amount of the alkali substance in the alkali liquor is 5 to 10 times of the theoretical amount of alkali required for neutralizing the acidic substance in the decolorized illegal cooking oil, and the amount of the alkali liquor is 20 to 25 percent of the volume of the decolorized illegal cooking oil.
In some embodiments, in step 5), the water washing specifically includes the following steps:
heating the alkali refined oil sample to 60-80 ℃, adding water with the same temperature as the alkali refined oil sample under the stirring condition, stirring for 2-2.2 h, standing for 4-6 h for layering, removing a water phase, taking an oil phase, and obtaining a primary water washing oil sample; wherein the using amount of the water is 20-25% of the volume of the alkali refined oil sample;
and repeating the water washing steps for one time on the primary water-washed oil sample to obtain a secondary water-washed oil sample.
In some embodiments, in the step 5), the vacuum degree of the vacuum dehydration is 20-50 mmHg, and the dehydration temperature is 60-80 ℃.
In some embodiments, in step 1), the phosphoric acid is a phosphoric acid solution with a mass fraction of 70% to 80%, and the amount of the phosphoric acid solution is 2% to 3% of the volume of the illegal cooking oil.
In some embodiments, before the step 1) of mixing the illegal cooking oil with the phosphoric acid, the method further comprises the following steps: and filtering the illegal cooking oil to remove solid impurities in the illegal cooking oil.
In some embodiments, in step 1), the step of standing after the heating and stirring reaction comprises the following steps:
stirring the mixed solution of the illegal cooking oil and the phosphoric acid at 60-70 ℃ for reacting for 28-32 min, standing at 70-80 ℃ for 1.5-2 h after the reaction is finished for layering, separating out a water phase, taking out an oil phase, and removing water from the oil phase to obtain the degumming illegal cooking oil.
According to another aspect of the present invention, there is provided a illegal cooking oil-based insulating oil prepared by the above-described preparation method of the present invention.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method of the illegal cooking oil-based insulating oil, the method of removing the light oil acid and the high oleic acid in the illegal cooking oil by stepwise heating and stripping in three steps is adopted, so that the acid value, the viscosity and the pour point of the illegal cooking oil-based insulating oil are effectively reduced, the electrical property of the illegal cooking oil-based insulating oil is improved, and the insulating property of the insulating oil is effectively improved under the condition that the main components in the illegal cooking oil are not changed; the illegal cooking oil-based insulating oil can be used in a low-temperature area, and the use temperature range of the illegal cooking oil-based insulating oil is expanded.
The method has the advantages of simple preparation process flow and good process stability, and can meet the technical requirements of industrial production.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings, which illustrate embodiments of the present invention. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
One embodiment of the present invention provides a preparation method of a illegal cooking oil-based insulating oil, which includes the following steps 1) to 5):
step 1): mixing the illegal cooking oil with phosphoric acid, heating, stirring, reacting, standing, separating out a water phase, and removing water from an oil phase to obtain the degumming illegal cooking oil.
The illegal cooking oil can generate a large amount of peptization substances in the high-temperature frying process, and the peptization substances can influence the effects of the subsequent treatment processes of deodorization, decoloration, alkali refining and the like. Mixing the illegal cooking oil with phosphoric acid, stirring under a heating condition to enable peptizing substances in the illegal cooking oil to fully react with the phosphoric acid and enter a water phase, standing to enable the water phase and the oil phase to be layered, separating the water phase and taking the oil phase, and removing water from the oil phase to obtain the degummed illegal cooking oil; peptizing substances are removed from the degummed illegal cooking oil, and subsequent treatment processes such as deodorization, decoloration and alkali refining cannot be influenced.
In some embodiments, the phosphoric acid used in step 1) is a phosphoric acid solution with a mass fraction of 70% to 80%, and the amount of the phosphoric acid solution is 2% to 3% of the volume of the illegal cooking oil. According to research, the phosphate solution with the mass fraction of 70-80% and the volume of 2-3% of the illegal cooking oil is adopted to react with the illegal cooking oil by heating and stirring, so that the peptizing substances in the illegal cooking oil can be fully removed. When the use amount of the phosphoric acid solution is too low, an ideal removal effect cannot be achieved, and the degummed illegal cooking oil still contains part of peptizing substances; when the amount of the phosphoric acid solution is too large, phosphoric acid is wasted, and the amount of alkali used in the subsequent alkali refining step is increased, so that the production cost is increased.
In some embodiments, in step 1), before mixing the illegal cooking oil with the phosphoric acid, the illegal cooking oil is filtered to remove impurities in the illegal cooking oil, so as to obtain clean illegal cooking oil. Specifically, the solid impurities in the illegal cooking oil are removed by filtering the illegal cooking oil by a physical filtering method, such as a filter screen. The drainage oil is oil produced by simply processing and refining greasy floaters in a sewer or leftovers and leftovers of hotels and restaurants, or oil produced by processing and refining inferior pork, pig viscera and pigskin, or oil produced after the use times of fried food exceed certain times; the waste oil is filtered before degumming to remove solid impurities in the waste oil, so that the treatment effects of subsequent deodorization, decoloration and alkali refining steps can be further improved.
In some embodiments, the step 1), the standing after the heating, stirring and reacting specifically includes the following steps: stirring and reacting the mixed solution of the illegal cooking oil and the phosphoric acid at 60-70 ℃ for 28-32 min, standing at 70-80 ℃ for 1.5-2 h for layering after the reaction is finished, separating out a water phase, taking out an oil phase, and removing water from the oil phase to obtain the degumming illegal cooking oil. Researches show that under the condition of adopting a phosphoric acid solution with the mass fraction of 70-80% and the volume of 2-3% of the illegal cooking oil, the mixed solution of the illegal cooking oil and the phosphoric acid is stirred and reacts for 28-32 min at the temperature of 60-70 ℃, so that the removal effect on peptizing substances in the illegal cooking oil is better; standing for 1.5-2 h at the temperature of 70-80 ℃ after the reaction is finished, and fully dissolving a product obtained after the reaction of the peptizing substance and the phosphoric acid in a water phase and layering the peptizing substance and an oil phase.
Step 2): heating the degummed illegal cooking oil to 108-115 ℃ under a vacuum condition, and introducing steam for steam stripping for 25-30 min; heating the degummed illegal cooking oil to 205-210 ℃, and introducing steam for steam stripping for 25-35 min; then heating the degummed illegal cooking oil to 220-230 ℃, and continuously introducing steam for steam stripping for 50-60 min; and (3) cooling the degummed illegal cooking oil under a vacuum condition to obtain the deodorized illegal cooking oil.
The inventor researches and discovers that the reasons for causing high pour point, high dielectric loss, high viscosity and poor electrical performance of the illegal cooking oil are mainly that the illegal cooking oil contains a large amount of light oleic acid (unsaturated fatty acid with small molecular weight, which is dissociated in an oil product and affects the acid value of the oil product) and high oleic acid (monounsaturated fatty acid which is easy to saponify with alkali and has great influence on the color and the acid value of the oil product); the light oil acid and the high oleic acid in the illegal cooking oil not only can greatly improve the acid value and the pour point of the illegal cooking oil, but also can improve the viscosity of the illegal cooking oil, reduce the electrical property of the illegal cooking oil and have odor.
The degumming illegal cooking oil is stripped step by step, the degumming illegal cooking oil is firstly heated to 108-115 ℃ under the vacuum condition, and stripping is carried out for 25-30 min through steam, so that most of light oleic acid in the illegal cooking oil is removed; then heating to 205-210 ℃, introducing steam for stripping for 25-35 min, and removing the remaining light oleic acid and part of high oleic acid in the illegal cooking oil; and heating the degummed illegal cooking oil to 220-230 ℃, introducing steam for stripping for 50-60 min, and completely removing high oleic acid in the illegal cooking oil. By adopting the method of the step-by-step steam stripping, the light oil acid and the high oleic acid in the illegal cooking oil can be effectively and thoroughly removed, the pour point and the viscosity of the illegal cooking oil are reduced, and the electrical performance of the illegal cooking oil is improved. If the light oleic acid and the high oleic acid cannot be well removed, the high oleic acid has great influence on the color of the oil product, saponification reaction is easy to occur in the alkali refining step, the oil product is emulsified, and the yield of the oil product is reduced. The light oleic acid is not easy to react with alkali in the alkali refining step, so that the acid value is difficult to reduce.
Further research shows that if a one-step stripping method is adopted, the degummed illegal cooking oil is directly heated to more than 200 ℃ and even more than 220 ℃ for stripping for more than 1h, although light oil acid and high oleic acid in the illegal cooking oil can also be removed; however, the longer time of stripping at higher temperature can change the effective components contained in the illegal cooking oil, and the service performance of the illegal cooking oil as insulating oil is affected. By adopting the method of stripping in three steps and gradually raising the stripping temperature, the light oleic acid and the high oleic acid in the illegal cooking oil can be thoroughly removed, the damage of the stripping process to the effective components in the illegal cooking oil can be avoided, and the service performance of the illegal cooking oil as the insulating oil is ensured.
In one specific example, step 2) is specifically: heating the degummed illegal cooking oil to 110 ℃ under the vacuum condition, and introducing steam for steam stripping for 30 min; heating the degummed illegal cooking oil to 210 ℃, and introducing steam for steam stripping for 30 min; then heating the degummed illegal cooking oil to 225 ℃, and continuously introducing steam for steam stripping for 60 min; and (3) cooling the degummed illegal cooking oil under a vacuum condition to obtain the deodorized illegal cooking oil.
Through further research, the inventor finds that in the step stripping operation, under the preferable process parameter conditions, each step has good removal effect on light oleic acid and high oleic acid in the illegal cooking oil, and the damage to effective components in the illegal cooking oil is smaller. The present invention preferably employs the split-step stripping process parameters described above.
Specifically, the step 2) of introducing steam for stripping means that the degummed illegal cooking oil is injected into a deodorization tower, and the steam is introduced from the bottom of the deodorization tower to strip the degummed illegal cooking oil. In the deodorization tower, by utilizing the characteristic that light oleic acid and high oleic acid in the illegal cooking oil are easier to volatilize than triglyceride under the conditions of high temperature and negative pressure, steam is introduced from the bottom of the deodorization tower, and is saturated by volatilized oleic acid components and escapes from the deodorization tower, so that the aims of removing oleic acid and removing odor are fulfilled. In particular, the steam used is water vapour.
Step 3): mixing the deodorized illegal cooking oil with active carbon and activated clay, stirring and decoloring in vacuum, and then filtering to obtain the decolored illegal cooking oil.
After the illegal cooking oil is subjected to steam stripping deodorization, the deodorized illegal cooking oil is mixed with active carbon and activated clay, the mixture is stirred and decolored under the vacuum condition, and the colored substances in the illegal cooking oil can be well adsorbed and removed through the cooperation of the active carbon and the activated clay, so that the color and luster of the illegal cooking oil are improved, and meanwhile, the purity of the illegal cooking oil is improved.
In some embodiments, in step 3), the amount of the activated carbon is 1.8-2% of the volume of the deodorized waste oil, the amount of the activated clay is 3.5-4% of the volume of the deodorized waste oil, and the time for vacuum stirring and decoloring is 1.8-2 h.
Researches show that when the dosage of the active carbon is 1.8-2% of the volume of the deodorization waste oil, and the dosage of the active clay is 3.5-4% of the volume of the deodorization waste oil, good decolorization effect can be obtained. When the consumption of the activated carbon and/or the activated clay is too low, the decoloring effect is poor; when the amount of the active carbon is too large, the decoloring effect is not obviously improved, and the waste of the active carbon and the active clay is caused.
Step 4): heating the decolored illegal cooking oil to 40-55 ℃, mixing the decolored illegal cooking oil with alkali liquor, stirring and reacting for 2-3 h, then heating to 70-90 ℃, standing for 8-10 h, separating out a water phase, and taking out an oil phase to obtain an alkali refined oil sample.
The decolored illegal cooking oil after the decoloration treatment is mixed with the alkali liquor, and the mixture is stirred and reacts under the heating condition, so that acidic substances in the illegal cooking oil can be removed, and the acid value of the illegal cooking oil is reduced; and possibly oleic acid present in the illegal cooking oil which is not completely removed by the stripping step can be removed. The combination of the alkali refining step and the steam stripping step greatly reduces the acid value of the illegal cooking oil, thoroughly removes oleic acid in the illegal cooking oil, effectively reduces the viscosity and pour point of the illegal cooking oil, and improves the electrical performance of the illegal cooking oil.
Heating the decolorized illegal cooking oil to 40-55 ℃, mixing the decolorized illegal cooking oil with alkali liquor, and stirring for reacting for 2-3 hours to ensure that acidic substances in the illegal cooking oil fully react with alkali; after the reaction is finished, the temperature is raised to 70-90 ℃, standing is carried out for 8-10 hours, so that the salt generated by the reaction of the acidic substance and the alkali is fully dissolved in the water phase, and the water phase and the oil phase are well layered.
Before mixing the lye with the decolorized illegal cooking oil, the lye is preferably heated to the same temperature as the decolorized illegal cooking oil. As the neutralization reaction of the acidic substance and the alkali is an exothermic reaction, the alkali liquor is heated to the same temperature as the decolored swill-cooked dirty oil and then mixed, so that the condition of bumping caused by large local temperature difference in a solution system can be avoided. Further, preferably, the alkali liquor and the decolored swill-cooked dirty oil are mixed and stirred to react in an open reaction container, so that the heat dissipation efficiency is improved; and preferably, the alkali liquor is dropwise added into the decolored illegal cooking oil, so that the neutralization reaction is more controllable.
In some embodiments, in the step 4), the amount of alkali substances in the alkali liquor is 5-10 times of the theoretical amount of alkali required for neutralizing acidic substances in the decolorized illegal cooking oil, and the amount of the alkali liquor is 20-25% of the volume of the decolorized illegal cooking oil.
It can be understood that the theoretical amount of alkali required for neutralizing the acidic substances in the decolorized illegal cooking oil, i.e. the amount of alkali required for converting the acidic substances in the decolorized illegal cooking oil into salts by completely reacting with alkali.
When the amount of alkaline substances in the alkali liquor is 5-6 times of the theoretical amount of alkaline required for neutralizing and decoloring acidic substances in the illegal cooking oil, the thorough conversion of the acidic substances in the illegal cooking oil can be ensured, and the service performance of the illegal cooking oil as insulating oil is ensured. The dosage of the alkali liquor is 20-25% of the volume of the decolorized illegal cooking oil, and the dosage of the alkali liquor is combined with the dosage of the alkali in the alkali liquor, so that the concentration of the alkali liquor is determined.
Step 5): and (3) sequentially carrying out water washing, vacuum dehydration and heat filtration on the alkali refined oil sample to obtain the insulating oil.
The alkali refined oil sample after alkali refining treatment may also contain some water-soluble substances such as salts and alkalis which do not completely enter the water phase. The water-soluble substances can be removed by washing the alkali refined oil sample with water, so that the purity of the illegal cooking oil is higher; and after washing, carrying out vacuum dehydration on the illegal cooking oil to remove water contained in the illegal cooking oil, and then carrying out hot filtration to further remove impurities in the illegal cooking oil to obtain the insulating oil.
In some embodiments, in step 5), the water washing specifically includes the following steps: heating an alkali refined oil sample to 60-80 ℃, adding water with the same temperature as the alkali refined oil sample under the stirring condition, stirring for 2-2.2 h, standing for 4-6 h for layering, removing a water phase, and taking an oil phase to obtain a primary water-washing oil sample; wherein, the water consumption is 20-25% of the volume of the alkali refined oil sample; and repeating the water washing step for one time on the primary water-washed oil sample to obtain a secondary water-washed oil sample.
Adding water into the alkali refined oil sample under the temperature condition, stirring to fully dissolve water-soluble substances in the illegal cooking oil in the water, standing for 4-6 h to fully separate a water phase from an oil phase, removing the water phase and taking the oil phase; through the two washing steps, the water-soluble substances in the illegal cooking oil can be effectively removed.
In some embodiments, in step 5), the vacuum degree of vacuum dehydration is 20-50 mmHg, and the dehydration temperature is 60-80 ℃. The vacuum dehydration under the condition can improve the water removal rate, ensure that the water is evaporated from the illegal cooking oil as much as possible and improve the dehydration efficiency.
In another embodiment of the invention, the invention also provides the illegal cooking oil-based insulating oil prepared by the preparation method. The illegal cooking oil-based insulating oil has the advantages of low acid value, low viscosity, low pour point, good electrical property and the like, has good insulating property, and can be used in low-temperature areas.
The present invention will be further described with reference to specific examples and comparative examples, which should not be construed as limiting the scope of the present invention.
Example 1:
the preparation method of the illegal cooking oil-based insulating oil provided by the embodiment of the invention comprises the following steps:
(1) removing impurities
And (4) removing impurities from the illegal cooking oil, and filtering the illegal cooking oil by adopting a physical filtering method to obtain clean illegal cooking oil.
(2) Degumming treatment
Degumming the impurity-removed swill-cooked dirty oil obtained in the step (1), wherein the method comprises the following steps: adding a phosphoric acid solution with the mass fraction of 75% and the volume of 2% of the illegal cooking oil, stirring and reacting for 30min at the temperature of 70 ℃, standing for 2h for layering at the temperature of 80 ℃, removing a water phase, reserving an oil phase, and carrying out reduced pressure distillation on the obtained oil phase to remove water, thereby obtaining the degumming illegal cooking oil.
(3) Steam stripping deodorization
And (3) deodorizing the degummed illegal cooking oil obtained in the step (2), wherein the treatment method comprises the following steps: injecting the illegal cooking oil into a deodorization tower, circulating the oil in the deodorization tower, circularly heating the oil to 110 ℃ in vacuum, introducing steam into the bottom layer of the deodorization tower, taking out light oil acid in the illegal cooking oil by using the steam, cooling the upper layer of the illegal cooking oil, flowing into a distillation tank of the deodorization tower, and circularly stripping for 30min in the way; heating to 210 ℃, and continuously carrying out steam stripping and distillation for 30 min; raising the temperature to 225 ℃ again, taking out the high oleic acid in the swill-cooked dirty oil by using water vapor, and continuously carrying out steam stripping and recovery for 1 h; and then cooling to normal temperature under the vacuum condition to obtain the deodorant swill-cooked dirty oil.
(4) Decolorizing treatment
And (4) carrying out decoloring treatment on the deodorized illegal cooking oil obtained in the step (3), wherein the treatment method comprises the following steps: adding 2% of activated carbon and 4% of activated clay by volume of the illegal cooking oil into the deodorized illegal cooking oil, stirring in vacuum for decolorization and adsorption for 2h, and then filtering out the activated carbon and the activated clay by a physical filtration method to obtain the decolorized illegal cooking oil.
(5) Alkali refining treatment
And (3) injecting the decolored illegal cooking oil obtained in the step (4) into an open reaction container, heating to 55 ℃, dropwise adding alkali liquor with the same temperature as the illegal cooking oil and the volume of 20% oil (the alkali quantity is 5 times of the theoretical alkali quantity of acid substances in the neutralized oil, and the required pure water is 20% of the volume of the oil) under the stirring condition, stirring for reaction for 3 hours, heating to 90 ℃, standing for 10 hours for layering, removing the lower-layer aqueous solution, and taking an oil phase to obtain an alkali refined oil sample.
(6) One-time water washing
And (3) transferring the alkali refined oil sample obtained in the step (5) into an open reaction container, heating to 80 ℃, adding pure water with the same temperature as the illegal cooking oil and the volume of 20% of the oil under the stirring condition, stirring for 2 hours, standing for 6 hours for layering, removing the lower-layer aqueous solution, and taking an oil phase to obtain a primary water-washing oil sample.
(7) Second washing with water
And (5) repeating the step (6) and carrying out secondary water washing to obtain a secondary water-washed oil sample.
(8) Dewatering and filtering
And (4) carrying out vacuum dehydration treatment on the secondary washing oil sample obtained in the step (7), wherein the vacuum degree is 50mmHg, the dehydration temperature is 80 ℃, and then filtering the illegal cooking oil while the illegal cooking oil is hot by using a filter to obtain the illegal cooking oil-based insulating oil.
The viscosity, acid value, pour point, dielectric loss, insulating property, electrical property and the like of the drainage oil-based insulating oil obtained in the embodiment were measured, and the test results are shown in table 1.
Example 2:
a method for preparing a trench oil-based insulating oil, the method comprising substantially the same steps as in example 1. Compared with example 1, the difference is that: and (3) in the alkali refining treatment in the step (5), injecting the decolored illegal cooking oil obtained in the step (4) into an open reaction container, heating to 45 ℃, dropwise adding 20% of alkali liquor with the same temperature as the illegal cooking oil in oil volume (the alkali quantity is 10 times of the theoretical alkali quantity of acid substances in the neutralized oil, and the required pure water is 20% of the oil volume) under the stirring condition, stirring for reaction for 2 hours, heating to 80 ℃, standing for 10 hours for layering, removing the lower-layer aqueous solution, and taking an oil phase to obtain an alkali refining oil sample.
The viscosity, acid value, pour point, dielectric loss, insulating property, electrical property and the like of the drainage oil-based insulating oil obtained in the embodiment were measured, and the test results are shown in table 1.
Comparative example 1:
a method for preparing a trench oil-based insulating oil, which comprises substantially the same steps as in example 1. Compared with example 1, the difference is that: in the step (3) of stripping deodorization, a method of gradually raising the temperature in three steps for stripping is not adopted, but the temperature of the illegal cooking oil is directly raised to 225 ℃, and steam is introduced into the bottom layer of a deodorization tower for stripping and recovery for 2 hours.
The specific stripping deodorization steps are as follows:
and (3) deodorizing the degummed illegal cooking oil obtained in the step (2), wherein the treatment method comprises the following steps: and (2) injecting the illegal cooking oil into a deodorization tower, circulating the oil in the deodorization tower, circularly heating to 225 ℃ in vacuum, introducing steam into the bottom layer of the deodorization tower, cooling the upper layer of the deodorization tower, flowing into a distillation tank of the deodorization tower, circularly stripping for 2 hours in the way, and cooling to normal temperature under the vacuum condition to obtain the deodorization illegal cooking oil.
The viscosity, acid value, pour point, dielectric loss, insulating property, electrical property and the like of the drainage oil-based insulating oil obtained in the comparative example were measured, and the test results are shown in table 1.
Comparative example 2:
a method for preparing a trench oil-based insulating oil, which comprises substantially the same steps as in example 1. Compared with example 1, the difference is that: in the decoloring step (4), the contents of activated carbon and activated clay are reduced. The specific decoloring steps are as follows:
and (4) carrying out decoloring treatment on the deodorized illegal cooking oil obtained in the step (3), wherein the treatment method comprises the following steps: adding 1% of activated carbon and 1% of activated clay by volume of the illegal cooking oil into the deodorized illegal cooking oil, stirring in vacuum for decolorization and adsorption for 2h, and then filtering out the activated carbon and the activated clay by a physical filtration method to obtain the decolorized illegal cooking oil.
The viscosity, acid value, pour point, dielectric loss, insulating property, electrical property and the like of the drainage oil-based insulating oil obtained in the comparative example were measured, and the test results are shown in table 1.
Table 1 results of performance test of the illegal cooking oil-based insulating oil of each example and comparative example
As can be seen from table 1, the acid value, viscosity and pour point of the drainage oil-based insulating oil obtained in example 1 and example 2 of the present invention are significantly lower than those of comparative example 1 and comparative example 2; the ignition and flash points are significantly higher than comparative examples 1 and 2; the performance parameters of breakdown voltage, volume resistivity and dielectric loss factor are obviously due to comparative examples 1 and 2. In addition, the method of stripping and deodorizing in three steps is adopted in the embodiment 1 of the invention, and compared with the one-step stripping method of the comparative example 1, the obtained illegal cooking oil-based insulating oil has obviously better performances.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The preparation method of the illegal cooking oil-based insulating oil is characterized by comprising the following steps:
step 1): mixing the illegal cooking oil with phosphoric acid, heating, stirring, reacting, standing, separating out a water phase, and removing water from an oil phase to obtain degummed illegal cooking oil;
step 2): heating the degummed illegal cooking oil to 108-115 ℃ under a vacuum condition, and introducing steam for steam stripping for 25-30 min; heating the degummed illegal cooking oil to 205-210 ℃, and introducing steam for steam stripping for 25-35 min; then heating the degummed illegal cooking oil to 220-230 ℃, and continuously introducing steam for steam stripping for 50-60 min; cooling the degummed illegal cooking oil under a vacuum condition to obtain deodorized illegal cooking oil;
step 3): mixing the deodorized illegal cooking oil with active carbon and activated clay, stirring and decoloring in vacuum, and then filtering to obtain decolored illegal cooking oil;
step 4): heating the decolored illegal cooking oil to 40-55 ℃, mixing the decolored illegal cooking oil with alkali liquor, stirring and reacting for 2-3 hours, then heating to 70-90 ℃, standing for 8-10 hours, separating out a water phase, and taking an oil phase to obtain an alkali refined oil sample;
step 5): and sequentially carrying out water washing, vacuum dehydration and heat filtration on the alkali refined oil sample to obtain the illegal cooking oil base insulating oil.
2. The method for preparing the illegal cooking oil-based insulating oil according to claim 1, wherein the step of introducing steam for stripping in the step 2) comprises the steps of: heating the degummed illegal cooking oil to 110 ℃ under the vacuum condition, and introducing steam for steam stripping for 30 min; heating the degummed illegal cooking oil to 210 ℃, and introducing steam for steam stripping for 30 min; and then heating the degummed illegal cooking oil to 225 ℃, and continuously introducing steam for steam stripping for 60 min.
3. The method for preparing the illegal cooking oil-based insulating oil according to claim 1, wherein the steam stripping operation in the step 2) is: and injecting the degummed illegal cooking oil into a deodorization tower, and introducing steam from the bottom of the deodorization tower to strip the degummed illegal cooking oil.
4. The preparation method of the illegal cooking oil-based insulating oil according to claim 1, wherein in the step 3), the dosage of the activated carbon is 1.8-2% of the volume of the deodorized illegal cooking oil, the dosage of the activated clay is 3.5-4% of the volume of the deodorized illegal cooking oil, and the time for vacuum stirring and decoloring is 1.8-2 h.
5. The method for preparing the illegal cooking oil-based insulating oil according to claim 1, wherein in the step 4), the amount of alkali substances in the lye is 5-10 times of the theoretical alkali amount required for neutralizing acidic substances in the decolored illegal cooking oil, and the amount of the lye is 20-25% of the volume of the decolored illegal cooking oil.
6. The method for preparing the illegal cooking oil-based insulating oil according to claim 1, wherein the water washing in the step 5) specifically comprises the steps of:
heating the alkali refined oil sample to 60-80 ℃, adding water with the same temperature as the alkali refined oil sample under the stirring condition, stirring for 2-2.2 h, standing for 4-6 h for layering, removing a water phase, taking an oil phase, and obtaining a primary water washing oil sample; wherein the using amount of the water is 20-25% of the volume of the alkali refined oil sample;
and repeating the water washing steps for one time on the primary water-washed oil sample to obtain a secondary water-washed oil sample.
7. The method of preparing a illegal cooking oil-based insulating oil according to any one of claims 1 to 6, wherein the vacuum degree of the vacuum dehydration in step 5) is 20 to 50mmHg, and the dehydration temperature is 60 to 80 ℃.
8. The method for preparing the illegal cooking oil-based insulating oil according to any one of claims 1 to 6, wherein the phosphoric acid in the step 1) is a phosphoric acid solution with a mass fraction of 70-80%, and the amount of the phosphoric acid solution is 2-3% by volume of the illegal cooking oil.
9. The method for preparing the illegal cooking oil-based insulating oil according to any one of claims 1 to 6, wherein the step of standing after the heating and stirring reaction in the step 1) comprises the steps of:
stirring the mixed solution of the illegal cooking oil and the phosphoric acid at 60-70 ℃ for reacting for 28-32 min, standing at 70-80 ℃ for 1.5-2 h after the reaction is finished for layering, separating out a water phase, taking out an oil phase, and removing water from the oil phase to obtain the degumming illegal cooking oil.
10. A illegal cooking oil-based insulating oil prepared by the preparation method according to any one of claims 1 to 9.
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