CN108579126B - Method for decoloring mineral insulating oil by using alkaline chitosan film - Google Patents
Method for decoloring mineral insulating oil by using alkaline chitosan film Download PDFInfo
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- CN108579126B CN108579126B CN201810450682.4A CN201810450682A CN108579126B CN 108579126 B CN108579126 B CN 108579126B CN 201810450682 A CN201810450682 A CN 201810450682A CN 108579126 B CN108579126 B CN 108579126B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
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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
- C10M1/00—Liquid compositions essentially based on mineral lubricating oils or fatty oils; Their use as lubricants
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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
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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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
Abstract
The invention discloses a method for decoloring mineral insulating oil by using an alkaline chitosan film, which comprises the following steps: 1) firstly, dispersing chitosan powder in a solvent system mixed by alkali and urea, and sequentially freezing, unfreezing and defoaming to obtain a chitosan alkaline solution; then adding epoxy chloropropane into the chitosan alkaline solution for crosslinking and defoaming to obtain a chitosan pre-gel solution; casting the chitosan pre-gel solution in a mold for membrane forming, and finally washing and drying the formed membrane to obtain an alkaline chitosan membrane; 2) pouring the mineral oil to be treated into a reactor, adding the alkaline chitosan film obtained in the step 1), mixing, heating to 60-80 ℃, reacting for 8-12h, cooling and filtering to obtain the decolored mineral oil. The prepared alkaline chitosan membrane has high adsorption performance, simple decolorization step, convenient operation, green and environmental protection, and is suitable for large-scale application.
Description
Technical Field
The invention relates to the application field of chitosan films, in particular to a method for decoloring mineral insulating oil by using an alkaline chitosan film.
Background
The mineral insulating oil used in transformer equipment is mainly composed of various mixed hydrocarbons with complex structures, and serves as an insulating and cooling medium in the transformer, and components such as an iron core, a coil and the like can be isolated from air and moisture, so that rusting of the components is avoided. The change of the color, the acid value and the gas content in the mineral insulating oil can reflect the internal information of oil products and equipment. In actual use, the color of the oil is an important indicator of the properties of the base oil. By comparing the color changes of the oils, the oxidation, deterioration and contamination can be roughly estimated.
The decolorization is an important process in oil refining and waste oil recycling, and aims to remove pigments and trace metals, soap grains, colloid, residual pesticides and other impurities in oil. There are three common waste oil treatment processes: extraction method, acid-base decolorization method and adsorption method. The Yao is characterized in that the decolorization, deslagging and deodorization treatment of diesel oil is carried out by selecting acid washing and combining with a methanol-ammonia water composite solvent extraction method in the process research of decolorization, deslagging and deodorization of inferior diesel oil, the color number of the extracted diesel oil can be reduced to No. 6-7, and the method is generally used for primary decolorization. The diesel oil is decolorized by acid and alkali, and the decolorization research shows that 98% concentrated sulfuric acid and methanol saturated alkali liquor have good effect on the decolorization of the diesel oil, but the use of strong acid causes certain pollution to the environment. The adsorption method is the most common decoloring method, and activated clay, activated carbon, inorganic flocculant and the like can be used for adsorption decoloring, wherein the activated clay is researched most and the decoloring effect of the activated clay is ideal; however, the decolorizing effect of the oil with high acid value, deep color and more impurities is not ideal.
Disclosure of Invention
The invention provides a method for decoloring mineral insulating oil by using an alkaline chitosan membrane, and the prepared alkaline chitosan membrane has the advantages of high adsorption performance, simple decoloring step, convenience in operation, greenness and environmental friendliness, and is suitable for large-scale application.
The invention is realized by adopting the technical scheme that: the method for decoloring mineral insulating oil by using the alkaline chitosan film is characterized by comprising the following steps of:
1) firstly, dispersing chitosan powder in a solvent system mixed by alkali and urea, and sequentially freezing, unfreezing and defoaming to obtain a chitosan alkaline solution; then adding epoxy chloropropane into the chitosan alkaline solution for crosslinking and defoaming to obtain a chitosan pre-gel solution; casting the chitosan pre-gel solution in a mold for membrane forming, and finally washing and drying the formed membrane to obtain an alkaline chitosan membrane;
2) decoloring the mineral insulating oil by using the alkaline chitosan film, pouring the mineral oil to be processed into a reactor, then adding the alkaline chitosan film obtained in the step 1), mixing, heating to 60-80 ℃, reacting for 8-12h, cooling and filtering to obtain the decolored mineral oil.
Further, in the step 1), the solvent system for mixing the alkali and the urea is an aqueous solution composed of 4% by mass of lithium hydroxide and 10% by mass of urea, or an aqueous solution composed of 6% by mass of potassium hydroxide and 10% by mass of urea.
Further, in the step 1), the mass fraction of chitosan in the chitosan alkaline solution is 2-8%.
Further, in the step 1), the mass fraction of chitosan in the chitosan alkaline solution is 3-5%.
Further, in the step 1), the temperature of the freezing treatment is below minus 30 ℃, the freezing time is above 6h, the environment is at room temperature during unfreezing, and vacuum defoaming is carried out for 10-30min at the temperature of 0 ℃ during defoaming.
Further, in the step 1), the epoxy chloropropane is added into the chitosan alkaline solution with the proportion of 200ml, 5-10m of L epoxy chloropropane is added, the crosslinking reaction temperature is below minus 20 ℃ and the time is 2-3h, and the vacuum deaeration is carried out for 20-40min at the temperature of 0 ℃ during the deaeration.
Further, in the step 1), vacuum drying and forming are carried out at 40-50 ℃ during forming; the washing is carried out repeatedly by adopting absolute ethyl alcohol and water, and then vacuum drying is carried out at 100 ℃.
Furthermore, the viscosity of the chitosan powder is more than 800m Pa.s, and the deacetylation degree is more than 80%.
Chitosan, a product of deacetylation of chitin, is also known as chitosan. The chitosan has the advantages of no toxicity, biodegradability, strong flocculation effect and the like, so that the chitosan becomes an ideal environment-friendly adsorbent, and can overcome the defects that the traditional adsorbent is difficult to perform innocent treatment and is easy to cause secondary pollution. Based on the situation, the alkaline chitosan membrane prepared by the invention can be used for preparing the chitosan membrane which has high strength, good adsorption effect, no toxicity, safety, greenness and environmental protection in batches, and has the characteristics of simple preparation process, high decolorization rate, lower oil absorption rate and greenness and environmental protection; can effectively remove the color in the mineral insulating oil and is suitable for large-scale industrial application.
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FIG. 1 is a color chart of a sample before and after treatment in example 3 of the present invention.
Detailed Description
The present invention will be described in more detail with reference to examples.
Example 1:
dispersing chitosan powder with a certain viscosity of 900 mPa.s and a deacetylation degree of 82% in an alkali/urea solvent system consisting of lithium hydroxide with the mass fraction of 4% and urea with the mass fraction of 10%, continuously stirring until the powder is uniformly dispersed, then freezing the powder at-30 ℃ for 6h, stirring and thawing at room temperature, and then defoaming in vacuum at 0 ℃ for 10min to obtain a chitosan alkaline solution with the mass fraction of 3%.
And adding 5m of L epoxy chloropropane into the obtained chitosan alkaline solution, stirring for 2h at the temperature of minus 20 ℃ for crosslinking, and then carrying out vacuum defoamation for 30min at the temperature of 0 ℃ to obtain a clear and transparent chitosan pre-gel solution.
The obtained chitosan pre-gel solution is cast in a mould, and then is dried in vacuum at 40 ℃ until a film is formed.
And (3) repeatedly washing the obtained membrane in absolute ethyl alcohol and water for 3 times in sequence, removing redundant epoxy chloropropane, alkali and urea, and then drying in vacuum at 100 ℃ until the water is completely removed to obtain the alkaline chitosan membrane with the alkali content of 30% by mass fraction.
Pouring mineral oil into a reactor, adding the alkaline chitosan film with the mass fraction of 3%, slowly stirring, heating to 65 ℃, reacting for 11h, cooling and filtering to obtain the decolored mineral oil.
Example 2:
dispersing chitosan powder with a certain viscosity of 1000m Pa.s and a deacetylation degree of 85% in an alkali/urea solvent system consisting of 6% by mass of potassium hydroxide and 10% by mass of urea, continuously stirring until the powder is uniformly dispersed, then freezing the powder at-30 ℃ for 7h, stirring and thawing at room temperature, and then defoaming in vacuum at 0 ℃ for 20min to obtain a chitosan alkaline solution with a mass fraction of 5%.
Adding 8m L epoxy chloropropane into the obtained chitosan alkaline solution, stirring for 2h at-20 ℃ for crosslinking, and then carrying out vacuum defoamation for 30min at 0 ℃ to obtain a clear and transparent chitosan pre-gel solution.
The obtained chitosan pre-gel solution is cast in a mould, and then is dried in vacuum at the temperature of 45 ℃ until a film is formed.
And (3) repeatedly washing the obtained membrane in absolute ethyl alcohol and water for 4 times in sequence, removing redundant epoxy chloropropane, alkali and urea, and then drying in vacuum at 100 ℃ until the water is completely removed to obtain the alkaline chitosan membrane with the alkali content of 40% by mass fraction.
Pouring mineral oil into a reactor, adding the alkaline chitosan film with the mass fraction of 3%, slowly stirring, heating to 70 ℃, reacting for 10h, cooling and filtering to obtain the decolored mineral oil.
Example 3:
dispersing chitosan powder with a certain viscosity of 1500 mPa.s and a deacetylation degree of 85% in an alkali/urea solvent system consisting of 6% by mass of potassium hydroxide and 10% by mass of urea, continuously stirring until the powder is uniformly dispersed, then freezing the powder at-30 ℃ for 7h, stirring and thawing at room temperature, and then defoaming in vacuum at 0 ℃ for 30min to obtain a chitosan alkaline solution with a mass fraction of 5%.
And adding 6m of L epoxy chloropropane into the obtained chitosan alkaline solution, stirring for 3h at the temperature of minus 20 ℃ for crosslinking, and then carrying out vacuum defoamation for 30min at the temperature of 0 ℃ to obtain a clear and transparent chitosan pre-gel solution.
The obtained chitosan pre-gel solution is cast in a mould, and then is dried in vacuum at the temperature of 45 ℃ until a film is formed.
And (3) repeatedly washing the obtained membrane in absolute ethyl alcohol and water for 4 times in sequence, removing redundant epoxy chloropropane, alkali and urea, and then drying in vacuum at 100 ℃ until the water is completely removed to obtain the alkaline chitosan membrane with the alkali content of 50% by mass fraction.
Pouring mineral oil into a reactor, adding the alkaline chitosan film with the mass fraction of 4%, slowly stirring, heating to 70 ℃, reacting for 10 hours, cooling and filtering to obtain the decolored mineral oil.
The color of the oil product is tested by referring to GB/T6540-.
As can be seen from FIG. 1, the color of the sample before and after treatment changed significantly, the sample before treatment had a certain color, while the sample after treatment was colorless and transparent, which indicates that the method of the present invention can effectively remove the color of mineral oil.
TABLE 1
| Test specimen | Oil before treatment | Treated oil |
| Color number | 1.3 | 0.5 |
The above-described embodiments are merely preferred embodiments of the present invention, and should not be construed as limiting the present invention, and the scope of the present invention is defined by the claims, and equivalents including technical features described in the claims. I.e., equivalent alterations and modifications within the scope hereof, are also intended to be within the scope of the invention.
Claims (6)
1. The method for decoloring the mineral insulating oil by using the alkaline chitosan film is characterized by comprising the following steps of:
1) the preparation method of the alkaline chitosan membrane comprises the steps of firstly dispersing chitosan powder in a solvent system mixed by alkali and urea, sequentially freezing, unfreezing and defoaming to obtain a chitosan alkaline solution, then adding epoxy chloropropane into the chitosan alkaline solution for crosslinking and defoaming, adding 5-10m L epoxy chloropropane into the chitosan alkaline solution with the proportion of 200m L, wherein the crosslinking reaction temperature is below minus 20 ℃ for 2-3h, and the chitosan alkaline solution is defoamed in vacuum for 20-40min at the temperature of 0 ℃ during defoaming to obtain a chitosan pre-gel solution;
2) decoloring the mineral insulating oil by using the alkaline chitosan film, pouring the mineral oil to be processed into a reactor, then adding the alkaline chitosan film obtained in the step 1), mixing, heating to 60-80 ℃, reacting for 8-12h, cooling and filtering to obtain the decolored mineral oil.
2. The method of claim 1, wherein: in the step 1), the solvent system mixed by the alkali and the urea is an aqueous solution composed of 4% by mass of lithium hydroxide and 10% by mass of urea, or an aqueous solution composed of 6% by mass of potassium hydroxide and 10% by mass of urea.
3. The method of claim 1, wherein: in the step 1), the mass fraction of chitosan in the chitosan alkaline solution is 2-8%.
4. The method of claim 1, wherein: in the step 1), the mass fraction of chitosan in the chitosan alkaline solution is 3-5%.
5. The method of claim 1, wherein: in the step 1), the temperature of the freezing treatment is below minus 30 ℃, the freezing time is more than 6h, the environment is at room temperature during thawing, and vacuum deaeration is carried out for 10-30min at the temperature of 0 ℃ during deaeration.
6. The method of claim 1, wherein: the viscosity of the chitosan powder is more than 800m Pa.s, and the deacetylation degree is more than 80%.
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| CN201810450682.4A CN108579126B (en) | 2018-05-11 | 2018-05-11 | Method for decoloring mineral insulating oil by using alkaline chitosan film |
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| CN201810450682.4A CN108579126B (en) | 2018-05-11 | 2018-05-11 | Method for decoloring mineral insulating oil by using alkaline chitosan film |
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| CN110449133A (en) * | 2019-07-16 | 2019-11-15 | 湖北工程学院 | Chitosan/silicon dioxide composite material |
| CN114425308A (en) * | 2021-12-31 | 2022-05-03 | 国网湖北省电力有限公司孝感供电公司 | Clay/chitosan-based deteriorated transformer oil regeneration adsorbent and preparation and regeneration methods thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467760A (en) * | 2013-09-09 | 2013-12-25 | 浙江大学 | Method for preparing high-strength chitosan/cellulose composite hydrogel film |
| CN107744799A (en) * | 2017-11-17 | 2018-03-02 | 湖北工程学院 | Chitosan microball, its preparation method and its application in mineral oil dielectric loss is reduced |
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| WO2011150417A2 (en) * | 2010-05-28 | 2011-12-01 | University Of South Florida | Use of cactus mucilage as a dispersant and absorbant for oil in oil-water mixtures |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103467760A (en) * | 2013-09-09 | 2013-12-25 | 浙江大学 | Method for preparing high-strength chitosan/cellulose composite hydrogel film |
| CN107744799A (en) * | 2017-11-17 | 2018-03-02 | 湖北工程学院 | Chitosan microball, its preparation method and its application in mineral oil dielectric loss is reduced |
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