CN108559574A - A method of utilizing gutter oil production environmental protection base oil - Google Patents
A method of utilizing gutter oil production environmental protection base oil Download PDFInfo
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- CN108559574A CN108559574A CN201810278580.9A CN201810278580A CN108559574A CN 108559574 A CN108559574 A CN 108559574A CN 201810278580 A CN201810278580 A CN 201810278580A CN 108559574 A CN108559574 A CN 108559574A
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- oil
- base oil
- gutter
- environmental protection
- protection base
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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
- C10M101/00—Lubricating compositions characterised by the base-material being a mineral or fatty oil
- C10M101/04—Fatty oil fractions
-
- 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
- C11B13/00—Recovery of fats, fatty oils or fatty acids from waste materials
-
- 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
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of methods producing environmental protection base oil as raw material using gutter oil, this method first cleans to gutter oil, degumming and decolorization, then with two step catalysis with acid esterifications, crude base oil is obtained, then crude base oil is washed, is decolourized, obtains environmental protection base oil.The present invention produces environmental protection base oil come alternative ore oil base oil using recycling gutter oil, realizes the high-end recycling of gutter oil, and the biological degradability of the base oil is good; it being capable of preferably environmental protection; its preparation process is simple, and reaction condition is mild, without special refinement treatment；In the present invention, primary esterification reaction and transesterification are successively carried out using two step acidification methods of improvement, the conversion rate of products and quality of gutter oil production environmental protection base oil can be significantly improved.
Description
Technical field
The present invention relates to a kind of preparation methods of base oil, and in particular to a kind of to utilize gutter oil production environmental protection base oil
Method.
Background technology
China generates millions of tons of gutter oils every year as edible oil big country, if the mismanagement meeting pair of these gutter oils
Environment and food security cause to seriously threaten.Currently, with the appearance of relevant laws and regulations, the purchase and processing of gutter oil have obtained
A degree of improvement, but to be mainly used to the production added values such as biodiesel and soap very low for recycling gutter oil at present
Industry, with the development of technology, by gutter oil efficiently use production high value added product be inexorable trend.
Lubricating oil is to ensure that machinery manufacturing industry and automobile develop rapidly essential product, China's lubricating oil in recent years
Consumption is gradually increasing, and has 6,800,000 tons to 2015 have reached more than 1,000 ten thousand tons from 2010.Wherein 80% or more be from
The non-renewable mineral based lubricating oil of Petroleum refining, main component are the poisonous and harmful petroleum hydrocarbon groups such as cycloalkane, aromatic hydrocarbon
Divide the base oil constituted and the additive containing certain heavy metal components, pollution is caused to water source, soil, air.Now due to
People increasingly pay attention to environment, and lubricating oil is also from mineral fundamental mode to environmentally friendly development.Produce millions of tons of ground per year in China
Ditch oil, if not only can ring can also be used the value maximization of gutter oil by its recycle to lubricating oil field
The lubricating oil alternative ore based lubricating oil of guarantor's type, environmental protection, also can protect resource to avoid wasting from many aspects, have significant
Economic benefit and social benefit.
Invention content
To solve the deficiencies in the prior art, the purpose of the present invention is to provide a kind of environmental protection base is produced using gutter oil
The method of oil, it is intended to which promoting to recycle gutter oil becomes the 5th class base oil, and the production for high-end lubricating oil provides raw material.
In order to realize that above-mentioned target, the present invention adopt the following technical scheme that：
A method of utilizing gutter oil production environmental protection base oil, which is characterized in that include the following steps：
S1, cleaned to gutter oil, degumming and decolorization obtain intermediate product I；
S2, intermediate product I is handled to obtain crude base oil using two steps acidification catalytic treatment method；
S3, upper oil phase, vacuum distillation is taken to obtain intermediate product II after carrying out washing standing to crude base oil；
S4, environmental protection base oil is obtained to the progress decolorization of intermediate product II.
Preferably, in abovementioned steps S1, the acid value of gutter oil is 50~180mgKOH/g, and the gutter oil of the high acid value is free
Aliphatic acid it is more, be adapted to prepare lube base oil, be cleaned to gutter oil using filtration method.
Preferably, degumming process is carried out at 60 DEG C using acidification-aquation combination method, specific embodiment is：First, to
The phosphoric acid that trench oil quality 0.2% is added in gutter oil handles 30min, then add trench oil volume 2% go from
Sub- water hydratable handles 20min, and standing takes upper oil phase to carry out next step decolorization.It can be removed by the decolorization step
Some can influence the oxidation stability substance of base oil, and the purity of base oil is made to increase.
Preferably, in abovementioned steps S1, joint decoloration is carried out to gutter oil using hydrogen peroxide and diatomite.
It is highly preferred that in abovementioned steps S2, specific embodiment is：(1), by sulfuric acid and hydrochloric acid according to volume ratio 1:2
Ratio mixes, then alcohols material is added thereto, and obtained mixed liquor is added in gutter oil, react 3 at 80~90 DEG C~
5h, after reaction vacuum distillation remove water and alcohols material；(2), hydrochloric acid and alcohols are added in the product obtained to step (1)
The mixture of substance reacts 4~6h at 80~90 DEG C, obtains crude base oil.It, cannot be direct since gutter oil acid value is higher
With base catalysis, sulfuric acid and hydrochloric acid are according to volume ratio 1 in the step:2 ratio mixing, sulfuric acid can be used as dehydrating agent, contribute to
The progress of reaction can make the conversion ratio of reaction reach 95% or more by two-step method catalysis.
It is highly preferred that in abovementioned steps (1), the volume ratio of alcohols material and gutter oil is 10%~25%.
More preferably, aforementioned alcohols material is one or more in ethyl alcohol, trimethylolpropane and pentaerythrite.
More preferably, the washings employed in above mentioned steps S3 are the saturated salt solution of alkalinity, and alkaline matter is hydrogen-oxygen
Change one or more in potassium, sodium hydroxide and sodium carbonate.
More preferably, in abovementioned steps S4, joint decoloration is carried out to intermediate product II using hydrogen peroxide and diatomite.
It is further preferred that the specific embodiment of aforementioned combinations decoloration is：At 70~90 DEG C of temperature, to pending object
It is middle that the hydrogen peroxide for accounting for pending amount of substance 1% is added, 30min is stirred, pending amount of substance 10% is then added thereto again
Diatomite simultaneously stirs 40min, and centrifugation takes upper oil phase to carry out next step reaction after standing 36h.
The invention has the beneficial effects that：The present invention produces environmental protection base oil come substitute mineral oil using recycling gutter oil
Base oil realizes the high-end recycling of gutter oil, and the biological degradability of the base oil is good, being capable of preferably protection ring
Border, preparation process is simple, and reaction condition is mild, without special refinement treatment；In the present invention, it is acidified using two steps of improvement
Facture successively carries out primary esterification reaction and transesterification, can significantly improve the production of gutter oil production environmental protection base oil
Product conversion ratio and quality.
Specific implementation mode
Specific introduce is made to the present invention below in conjunction with specific embodiment.
It is raw materials used such as without special theory the invention discloses the method for producing environmental protection base oil using recycling gutter oil
It is bright, it is purchased in market.
Embodiment 1
It is the gutter oil of the brownish black of 100mgKOH/g to take 200ml acid values, and heat filtering is carried out with the filter membrane of 1 μm (micron),
Then degumming process is carried out at 60 DEG C using acidification-aquation combination method：The phosphorus of trench oil quality 0.2% is added into gutter oil
Sour acidification 30min, then adds the deionized water hydration process 20min of trench oil volume 2%, and standing takes upper layer oily
Phase；Obtained upper oil phase is subjected to decolorization, obtains crocus gutter oil.
By sulfuric acid and hydrochloric acid according to volume ratio 1:2 ratio mixing, then ethyl alcohol is added thereto, obtained mixed liquor is added
Enter in gutter oil, the volume ratio of ethyl alcohol and gutter oil therein is 10%, and primary esterification is carried out at 80 DEG C and reacts 4h, reaction knot
Vacuum distillation removes water and ethyl alcohol after beam；Then the mixture of hydrochloric acid and ethyl alcohol, then into reactor is added, at 90 DEG C again
Catalytic esterification 4h is carried out, crude base oil is obtained.
Crude base oil is washed with alkaline saturated salt solution, alkaline matter is the mixing of sodium hydroxide and sodium carbonate
Object stands 12h after washing, carry out decolorization after vacuum distillation again, obtains environmental protection base oil.
All it is that joint decoloration, specific work are carried out using hydrogen peroxide and diatomite at noted earlier two " decolorization "
Skill process is：At 70~90 DEG C of temperature, the hydrogen peroxide for accounting for pending amount of substance 1%, stirring are added into pending object
Then 30min is added the diatomite of pending amount of substance 10% and stirs 40min thereto again, centrifugation takes after standing 36h
Layer oil phase carries out next step reaction.
The process of embodiment 2~4 is same as Example 1, and difference lies in the acid value for being gutter oil and each raw materials
Selection, it is specific as follows.
Embodiment 2
It is the gutter oil of the brownish black of 50mgKOH/g to take 200ml acid values, carries out heat filtering with the filter membrane of 1 μm (micron), so
Degumming process is carried out at 60 DEG C using acidification-aquation combination method afterwards：The phosphoric acid of trench oil quality 0.2% is added into gutter oil
Acidification 30min, then adds the deionized water hydration process 20min of trench oil volume 2%, and standing takes upper oil phase；
Obtained upper oil phase is subjected to decolorization, obtains crocus gutter oil.
By sulfuric acid and hydrochloric acid according to volume ratio 1:2 ratio mixing, then ethyl alcohol is added thereto, obtained mixed liquor is added
Enter in gutter oil, the volume ratio of ethyl alcohol and gutter oil therein is 25%, and primary esterification is carried out at 90 DEG C and reacts 3h, reaction knot
Vacuum distillation removes water and ethyl alcohol after beam；Then the mixture of hydrochloric acid and trimethylolpropane, then into reactor is added, in 80
Catalytic esterification 5h is carried out at DEG C again, obtains crude base oil.
Crude base oil is washed with alkaline saturated salt solution, alkaline matter is potassium hydroxide, is stood after washing
12h carries out decolorization again after vacuum distillation, obtain environmental protection base oil.
Embodiment 3
It is the gutter oil of the brownish black of 180mgKOH/g to take 200ml acid values, and heat filtering is carried out with the filter membrane of 1 μm (micron),
Then degumming process is carried out at 60 DEG C using acidification-aquation combination method：The phosphorus of trench oil quality 0.2% is added into gutter oil
Sour acidification 30min, then adds the deionized water hydration process 20min of trench oil volume 2%, and standing takes upper layer oily
Phase；Obtained upper oil phase is subjected to decolorization, obtains crocus gutter oil.
By sulfuric acid and hydrochloric acid according to volume ratio 1:2 ratio mixing, then pentaerythrite is added thereto, the mixing that will be obtained
Liquid is added in gutter oil, and the volume ratio of pentaerythrite and gutter oil therein is 15%, and primary esterification reaction is carried out at 90 DEG C
5h, after reaction vacuum distillation remove water；Then the mixture of hydrochloric acid and trimethylolpropane, then into reactor is added,
It carries out catalytic esterification 6h again at 90 DEG C, obtains crude base oil.
Crude base oil is washed with alkaline saturated salt solution, alkaline matter is sodium carbonate, and 12h is stood after washing,
Decolorization is carried out after vacuum distillation again, obtains environmental protection base oil.
Performance detection
The viscosity for the environmental protection base oil that 1~embodiment of the embodiment of the present invention 3 is prepared below, density, pour point, sudden strain of a muscle
Point, acid value, moisture etc. are detected, and detection method and testing result are referring to table 1.
Comparative example 1 is the performance data of commercially available lube base oil.
The performance test results of 1 Examples 1 to 3 of table and comparative example 1
By table 1 as it can be seen that the present invention produces environmental protection base oil come alternative ore oil base oil using recycling gutter oil, realize
The high-end recycling of gutter oil.Compared with comparative example 1, base oil biological degradability of the invention is good, can preferably protect
Retaining ring border, and preparation process is simple, reaction condition is mild, without special refinement treatment.Especially, using two steps of improvement acid
Change facture and successively carry out primary esterification reaction and transesterification, can reduce individually makes what reaction was carbonized to show with sulfuric acid
As that can also utilize the dehydration property of sulfuric acid, be conducive to react, the product of gutter oil production environmental protection base oil can be significantly improved
Conversion ratio and quality, conversion rate of products are up to 95% or more, and coloration, viscosity and density of product etc. can meet the high-end need of industry
It asks.
The basic principles, main features and advantages of the invention have been shown and described above.The technical staff of the industry should
Understand, the invention is not limited in any way above-described embodiment, all to be obtained by the way of equivalent substitution or equivalent transformation
Technical solution is all fallen in protection scope of the present invention.
Claims (10)
1. a kind of method producing environmental protection base oil using gutter oil, which is characterized in that include the following steps：
S1, cleaned to gutter oil, degumming and decolorization obtain intermediate product I；
S2, intermediate product I is handled to obtain crude base oil using two steps acidification catalytic treatment method；
S3, upper oil phase, vacuum distillation is taken to obtain intermediate product II after carrying out washing standing to crude base oil；
S4, environmental protection base oil is obtained to the progress decolorization of intermediate product II.
2. a kind of method producing environmental protection base oil using gutter oil according to claim 1, which is characterized in that described
In step S1, the acid value of gutter oil is 50 ~ 180mgKOH/g, is cleaned to gutter oil using filtration method.
3. a kind of method producing environmental protection base oil using gutter oil according to claim 1, which is characterized in that described
In step S1, degumming process is carried out at 60 DEG C using acidification-aquation combination method, specific embodiment is：First, to gutter oil
The middle phosphoric acid that trench oil quality 0.2% is added handles 30min, then adds the deionized water aquation of trench oil volume 2%
20min is handled, standing takes upper oil phase to carry out next step decolorization.
4. a kind of method producing environmental protection base oil using gutter oil according to claim 1, which is characterized in that described
In step S1, joint decoloration is carried out to gutter oil using hydrogen peroxide and diatomite.
5. a kind of method producing environmental protection base oil using gutter oil according to claim 1, which is characterized in that described
In step S2, specific embodiment is：（1）, by sulfuric acid and hydrochloric acid according to volume ratio 1:2 ratio mixing, then be added thereto
Obtained mixed liquor is added in gutter oil alcohols material, and 3 ~ 5h is reacted at 80 ~ 90 DEG C, and vacuum distillation after reaction removes
Remove water and alcohols material；（2）, to step（1）The mixture of hydrochloric acid and alcohols material is added in obtained product, in 80 ~ 90 DEG C
4 ~ 6h of lower reaction, obtains crude base oil.
6. a kind of method producing environmental protection base oil using gutter oil according to claim 5, which is characterized in that described
Step（1）In, the volume ratio of alcohols material and gutter oil is 10% ~ 25%.
7. a kind of method producing environmental protection base oil using gutter oil according to claim 6, which is characterized in that described
Alcohols material is one or more in ethyl alcohol, trimethylolpropane and pentaerythrite.
8. a kind of method producing environmental protection base oil using gutter oil according to claim 1, which is characterized in that described
Washings employed in step S3 are the saturated salt solution of alkalinity, and alkaline matter is potassium hydroxide, sodium hydroxide and sodium carbonate
In it is one or more.
9. a kind of method producing environmental protection base oil using gutter oil according to claim 1, which is characterized in that described
In step S4, joint decoloration is carried out to intermediate product II using hydrogen peroxide and diatomite.
10. a kind of method producing environmental protection base oil using gutter oil according to claim 4 or 9, which is characterized in that
Combining the specific embodiment decolourized is：At 70 ~ 90 DEG C of temperature, it is added into pending object and accounts for the double of pending amount of substance 1%
Oxygen water stirs 30min, the diatomite of pending amount of substance 10% is then added thereto again and stirs 40min, and centrifugation is stood
Upper oil phase is taken to carry out next step reaction after 36h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810278580.9A CN108559574B (en) | 2018-03-31 | 2018-03-31 | Method for producing environment-friendly base oil by using illegal cooking oil |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810278580.9A CN108559574B (en) | 2018-03-31 | 2018-03-31 | Method for producing environment-friendly base oil by using illegal cooking oil |
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| CN108559574B CN108559574B (en) | 2021-04-16 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108102765A (en) * | 2017-11-15 | 2018-06-01 | 孟庆桓 | It is a kind of to be acidified the method that gutter oil prepares antiwear additive |
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| CN103087809A (en) * | 2012-12-11 | 2013-05-08 | 福建达安能源实业有限责任公司 | Preparation method of biomass truck lubricating oil |
| CN104711126A (en) * | 2015-02-13 | 2015-06-17 | 新疆福克油品股份有限公司 | High-quality utilization method for waste oil |
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2018
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103087809A (en) * | 2012-12-11 | 2013-05-08 | 福建达安能源实业有限责任公司 | Preparation method of biomass truck lubricating oil |
| CN104711126A (en) * | 2015-02-13 | 2015-06-17 | 新疆福克油品股份有限公司 | High-quality utilization method for waste oil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108102765A (en) * | 2017-11-15 | 2018-06-01 | 孟庆桓 | It is a kind of to be acidified the method that gutter oil prepares antiwear additive |
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Effective date of registration: 20221207 Address after: 210012 Tie Xin Qiao Jie Dao Tie Xin Cun, Yuhuatai District, Nanjing City, Jiangsu Province Patentee after: Nanjing Tongchuang Machinery Lubricant Co.,Ltd. Address before: No.12 Huatai Road, Yuchun District, Nanjing, Jiangsu Province Patentee before: LUBAOTE (NANJING) ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. |