CN113337337A - Regeneration treatment method of waste oil - Google Patents
Regeneration treatment method of waste oil Download PDFInfo
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- CN113337337A CN113337337A CN202110345394.4A CN202110345394A CN113337337A CN 113337337 A CN113337337 A CN 113337337A CN 202110345394 A CN202110345394 A CN 202110345394A CN 113337337 A CN113337337 A CN 113337337A
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- 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
- 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
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
-
- 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
- C11B3/02—Refining fats or fatty oils by chemical reaction
- C11B3/04—Refining fats or fatty oils by chemical reaction with acids
-
- 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
- C11B3/02—Refining fats or fatty oils by chemical reaction
- C11B3/06—Refining fats or fatty oils by chemical reaction with bases
-
- 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
- C11B3/10—Refining fats or fatty oils by adsorption
-
- 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)
- Microbiology (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to a regeneration treatment method of waste oil, which comprises the following specific steps: 1) filtering the waste grease to remove impurities, and dehydrating to remove water to obtain clear waste grease; 2) mixing the filtered waste oil and fat with concentrated sulfuric acid for reaction, standing for layering, and separating to obtain primary purified oil on the upper layer and acidic waste residue on the lower layer; 3) mixing and stirring the primary purified oil and the alkaline solid powder for reaction, and filtering to obtain secondary purified oil and solid residues; 4) mixing the solid residue with the acidic waste residue for reaction, and calcining to remove organic matters after the reaction is completed to obtain an inorganic salt product; 5) and treating the secondary purified oil with an adsorbent to obtain purified oil. The regeneration treatment method of the waste oil can recycle the high-grade fatty acid and the glycerol, and also recycle the residue, does not generate waste, has simple process, low cost, is green and environment-friendly, and is suitable for industrial application.
Description
Technical Field
The invention belongs to the technical field of refining of fat or fatty oil, and relates to a regeneration treatment method of waste oil.
Background
The consumption of grease in the food field is extremely large, the total amount of the waste grease generated by the method, such as old oil with too many frying times, waste oil collected by a range hood, grease extracted from waste meat in a slaughterhouse, waste grease in a kitchen, and the like, is remarkable, and the recycling of the substances can reduce pollution, save resources and bring certain economic benefits.
The main method for treating the waste oil at the present stage is to decompose the waste oil into higher fatty acid and glycerin by adopting a noble metal catalyst catalytic decomposition mode. The higher fatty acid and the glycerol obtained by the method can be used as raw materials of products such as washing powder, biodiesel, glycerol and the like, but the treatment method has the advantages of higher catalyst cost, low recovery rate and no industrial production prospect.
In order to solve the problem, the applicant researches a new method for treating waste grease to obtain high-quality oil which can be used as raw materials of products such as soap, washing powder, biodiesel and glycerol.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a regeneration treatment method of waste oil and fat aiming at the defects in the prior art, the method can obtain fatty acid, glycerin and inorganic salt products with higher quality, the comprehensive utilization rate is high, the economic benefit is good, and the process is pollution-free.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the regeneration treatment method of the waste oil comprises the following specific steps:
1) filtering the waste grease to remove impurities, and dehydrating to remove water to obtain clear waste grease;
2) mixing the filtered waste oil and fat with concentrated sulfuric acid for reaction, standing for layering, and separating to obtain primary purified oil on the upper layer and acidic waste residue on the lower layer;
3) mixing the primary purified oil obtained in the step 2) with alkaline solid powder, stirring, reacting, and filtering to obtain secondary purified oil and solid residues;
4) mixing the solid residue obtained in the step 3) with the acidic waste residue obtained in the step 2) for reaction, and calcining to remove organic matters after the reaction is completed to obtain an inorganic salt product;
5) treating the secondary purified oil obtained in the step 3) with an adsorbent to obtain purified oil.
According to the scheme, the waste oil in the step 1) comprises old oil with too many frying times, waste oil collected by a smoke exhaust ventilator, oil extracted from waste meat in a slaughterhouse and kitchen waste oil.
According to the scheme, the dehydration method in the step 1) adopts a vacuum dehydrator for dehydration.
According to the scheme, the mass ratio of the filtered waste oil in the step 2) to the concentrated sulfuric acid is 3-30: 1, the mass concentration of the concentrated sulfuric acid is more than 90%.
According to the scheme, the mixing reaction temperature of the waste oil and the concentrated sulfuric acid in the step 2) is 0-80 ℃, and the reaction time is 1-12 hours.
According to the scheme, the alkaline solid powder in the step 3) is MgO, Mg (OH)2，MgCO3，CaO， CaCO3，ZnO，ZnCO3，Fe2O3，Al2O3，Al(OH)3One or more of them.
According to the scheme, the mass ratio of the primary purified oil in the step 3) to the alkaline solid powder is 10-80: 1.
according to the scheme, the stirring reaction temperature in the step 3) is 0-80 ℃, and the reaction time is 0.5-5 h.
According to the scheme, the mass ratio of the solid residues to the acidic waste residues in the step 4) is 0.3-1.5: 1.
according to the scheme, the mixing reaction temperature in the step 4) is room temperature (15-35 ℃), and the reaction time is 30 min-3 h.
According to the scheme, the calcining temperature in the step 4) is 400-1000 ℃, and the calcining time is 1-5 h.
According to the scheme, the adsorbent in the step 5) is one of mesoporous silicon, mesoporous carbon and active zeolite.
According to the scheme, the mass ratio of the secondary purified oil in the step 5) to the adsorbent is 30-80: 1.
the method comprises the steps of firstly filtering and dehydrating the waste oil and fat, removing solid impurities and water in the waste oil and fat, then carrying out acid pickling on the filtered and dehydrated waste oil and fat, carrying out oxidation dissolution and condensation on harmful substances such as heavy metals, mechanical impurities and putrefactive oil and fat in the waste oil and fat by utilizing the strong oxidizing property of concentrated sulfuric acid to obtain primary purified oil and acidic waste residue (the acidic waste residue is mainly a viscous solid-liquid mixture), neutralizing and adsorbing residual trace acid and rancid oil in the primary purified oil by adopting alkaline solid powder, carrying out neutralization reaction on the alkaline solid powder and residual trace acid in the primary purified oil, leading the alkaline solid powder to have certain adsorption property and bring a slight decoloration effect, filtering to obtain secondary purified oil and solid residue, removing the water in the oil by utilizing an adsorbent, further optimizing the quality of the oil, leading the component of the purified oil to be mainly high-grade fatty acid glyceride, the purity of the acid waste residue is about 90-98%, the generated acid waste residue and the solid residue are mixed, the residual sulfuric acid in the acid waste residue and the alkaline powder in the solid residue are subjected to neutralization reaction to generate sulfate, and a sulfate product with the purity of more than 80% can be obtained after roasting.
The invention has the beneficial effects that: 1. the regeneration treatment method of the waste oil can recycle the high-grade fatty acid and the glycerol, and also recycle the residue, so that no waste is generated, the process is simple, the cost is low, and the regeneration treatment method is green and environment-friendly and is suitable for industrial application; 2. the high-quality purified oil obtained by the invention has the main component of higher fatty glyceride, can be used as the raw material of products such as soap, washing powder, biodiesel, glycerin and the like, and has good economic value.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention is further described in detail with reference to the following examples.
The waste grease raw material used in the embodiment of the invention is old oil in a certain restaurant in Wuhan.
Example 1
A regeneration treatment method of waste oil comprises the following specific steps:
1) filtering 50Kg of waste grease by a box filter to remove impurities, and dehydrating by a vacuum dehydrator to obtain clear waste grease;
2) mixing the filtered waste oil and 98 wt% of concentrated sulfuric acid according to a mass ratio of 20: 1, mixing, heating to 35 ℃, reacting for 3 hours, standing for layering, filtering and separating to obtain primary purified oil on the upper layer and acidic waste residue on the lower layer;
3) mixing the primary purified oil obtained in the step 2) with MgO powder according to the mass ratio of 20: 1, mixing, heating to 30 ℃, stirring for reaction for 3 hours, and filtering to obtain secondary purified oil and alkaline residue;
4) mixing the alkaline residue obtained in the step 3) and the acidic waste residue obtained in the step 2) according to a mass ratio of 1: 1 mixing and reacting for 40min, calcining at 600 ℃ for 4h after complete reaction to remove organic matters to obtain an inorganic salt product, and measuring that the main component of the inorganic salt product is MgSO4The mass percentage content is more than 80 percent;
5) adding a mesoporous silicon adsorbent into the secondary purified oil obtained in the step 3), wherein the mass ratio of the secondary purified oil to the adsorbent is 50: 1, stirring, standing, filtering and vacuum dehydrating to obtain about 43.1Kg of purified oil, which was found to contain higher fatty acid glycerides as a main component and to have a purity of about 95% by weight.
Example 2
A regeneration treatment method of waste oil comprises the following specific steps:
1) filtering 50Kg of waste grease by a box filter to remove impurities, and dehydrating by a vacuum dehydrator to obtain clear waste grease;
2) mixing the filtered waste oil and 98 wt% of concentrated sulfuric acid according to a mass ratio of 15: 1, mixing, heating to 30 ℃, reacting for 3 hours, standing for layering, filtering and separating to obtain primary purified oil on the upper layer and acidic waste residue on the lower layer;
3) mixing the primary purified oil obtained in the step 2) with MgCO3The powder comprises the following components in percentage by mass 15: 1, mixing, heating to 30 ℃, stirring for reaction for 3 hours, and filtering to obtain secondary purified oil and alkaline residue;
4) mixing the alkaline residue obtained in the step 3) and the acidic waste residue obtained in the step 2) according to a mass ratio of 1: 1 mixing and reacting for 40min, calcining at 600 ℃ for 3h after complete reaction to remove organic matters to obtain an inorganic salt product, wherein the main component of the inorganic salt product is MgSO4The content is more than 80 wt%;
5) adding an active mesoporous carbon adsorbent into the secondary purified oil obtained in the step 3), wherein the mass ratio of the secondary purified oil to the adsorbent is 40: 1, stirring, standing, filtering and vacuum dehydrating to obtain about 43.6Kg of purified oil, the main component of which is higher fatty glyceride and the purity is about 96 wt%.
Example 3
A regeneration treatment method of waste oil comprises the following specific steps:
1) filtering 50Kg of waste grease by a box filter to remove impurities, and dehydrating by a vacuum dehydrator to obtain clear waste grease;
2) mixing the filtered waste oil and 93 wt% concentrated sulfuric acid according to the mass ratio of 10: 1, mixing, stirring and reacting for 3 hours at room temperature (about 20 ℃), standing and layering, and filtering and separating to obtain primary purified oil on the upper layer and acidic waste residue on the lower layer;
3) mixing the primary purified oil obtained in the step 2) with CaCO3The powder comprises the following components in percentage by mass 15: 1, mixing, heating to 30 ℃, stirring for reaction for 3 hours, and filtering to obtain secondary purified oil and alkaline residue;
4) mixing the alkaline residue obtained in the step 3) and the acidic waste residue obtained in the step 2) according to a mass ratio of 1: 1 mixing and reacting for 40min, calcining at 650 ℃ for 3h after complete reaction to remove organic matters to obtain an inorganic salt product, wherein the main component of the inorganic salt product is CaSO4The content is more than 80 wt%;
5) adding a mesoporous silicon adsorbent into the secondary purified oil obtained in the step 3), wherein the mass ratio of the secondary purified oil to the adsorbent is 30: 1, stirring, standing, filtering and vacuum dehydrating to obtain about 44.0Kg purified oil, the main component of which is higher fatty glyceride with the purity of about 98 wt%.
The waste oil raw materials used in the embodiment of the invention and the purified oil samples obtained in the embodiments 1 to 3 are subjected to performance tests, the test standards refer to the relevant national food safety standards, part of the standards refer to the national food safety standard vegetable oil GB 2716-2018, and the test results are shown in Table 1. The results of calculation of the waste oil/fat recovery rate are shown in Table 2. The inorganic salt product obtained by calcination was subjected to the test, and the results are shown in Table 3.
In the examples of the present invention, the method for measuring higher fatty acid glycerides in purified oil regenerated according to the present invention was a hydrolysis-extraction method described in "measurement of fatty acids in food products" of GB 5009.168-2016. The measured total fat content is 90-98g/100g, the purity of the higher fatty glyceride obtained by conversion is about 90-98%, and the higher fatty glyceride can be processed to obtain higher fatty acid, glycerol and the like, and can be used for manufacturing products such as soap, washing powder, biodiesel, glycerol and the like, so that waste is changed into valuable.
TABLE 1
Table 2 examples 1-3 waste oil recovery
| Examples | Example 1 | Example 2 | Example 3 |
| Percent recovery rate% | 86.2 | 87.2 | 88.0 |
Table 3 examples 1-3 test results of contents of main components of inorganic salts
Note: the content of other trace metal sulfates is very small and is not shown in the table.
Table 1 shows that part of the physicochemical properties of the purified oil obtained by the regeneration treatment method of the invention are close to the performance requirements of national standard GB 2716-2018 national food safety standard vegetable oil, and the purified oil obtained by the embodiment of the invention has better oil quality.
Table 2 shows that the recovery rate of the purified oil by the regeneration treatment method of the invention is as high as 90-91%, and the recovery rate is higher.
Table 3 shows that not only can better grease be obtained by the regeneration treatment method of the invention, but also a sulfate product with higher purity can be obtained.
The invention is not limited to the specific details of the above three embodiments. Within the requirements of the invention, many simple variants of the solution are possible, all falling within the scope of protection of the invention.
Claims (10)
1. The regeneration treatment method of the waste oil is characterized by comprising the following specific steps:
1) filtering the waste grease to remove impurities, and dehydrating to remove water to obtain clear waste grease;
2) mixing the filtered waste oil and fat with concentrated sulfuric acid for reaction, standing for layering, and separating to obtain primary purified oil on the upper layer and acidic waste residue on the lower layer;
3) mixing the primary purified oil obtained in the step 2) with alkaline solid powder, stirring, reacting, and filtering to obtain secondary purified oil and solid residues;
4) mixing the solid residue obtained in the step 3) with the acidic waste residue obtained in the step 2) for reaction, and calcining to remove organic matters after the reaction is completed to obtain an inorganic salt product;
5) treating the secondary purified oil obtained in the step 3) with an adsorbent to obtain purified oil.
2. The regeneration treatment method of waste oil and fat according to claim 1, wherein the waste oil and fat in step 1) comprises old oil with excessive frying times, waste oil collected by a range hood, oil extracted from meat waste in a slaughterhouse and kitchen waste oil and fat.
3. The regeneration treatment method of waste oil and fat according to claim 1, wherein the mass ratio of the filtered waste oil and fat to concentrated sulfuric acid in the step 2) is 3-30: 1, the mass concentration of the concentrated sulfuric acid is more than 90%; and 2) mixing the waste oil and concentrated sulfuric acid for reaction at the temperature of 0-80 ℃ for 1-12 h.
4. The method for recycling waste oils and fats according to claim 1, wherein said alkaline solid powder of step 3) is MgO, Mg (OH)2，MgCO3，CaO，CaCO3，ZnO，ZnCO3，Fe2O3，Al2O3，Al(OH)3One or more of the above, the mass ratio of the primary purified oil in the step 3) to the alkaline solid powder is 10-80: 1.
5. the regeneration treatment method of waste oil and fat according to claim 1, wherein the stirring reaction temperature in the step 3) is 0-80 ℃, and the reaction time is 0.5-5 h.
6. The regeneration treatment method of waste oil and fat according to claim 1, wherein the mass ratio of the solid residue to the acid waste residue in the step 4) is 0.3-1.5: 1.
7. the regeneration treatment method of waste oil and fat according to claim 1, wherein the mixing reaction temperature in the step 4) is room temperature, and the reaction time is 30 min-3 h.
8. The regeneration treatment method of waste oil and fat according to claim 1, wherein the calcination temperature in the step 4) is 400-1000 ℃, and the calcination time is 1-5 hours.
9. The method for recycling waste oils and fats according to claim 1, wherein the adsorbent in step 5) is one of a silicon, aluminum, carbon-based adsorbent having a microporous or mesoporous structure, or an activated zeolite.
10. The regeneration treatment method of waste oil and fat according to claim 1, wherein the mass ratio of the secondary purified oil in step 5) to the adsorbent is 30-80: 1.
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Citations (6)
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| CN106520381A (en) * | 2016-11-11 | 2017-03-22 | 云南磷化集团有限公司 | Decoloration and deodorization method for drainage oil fatty acid |
| CN109126813A (en) * | 2018-09-17 | 2019-01-04 | 龙岩卓越新能源股份有限公司 | Utilize the method for waste animal and plant fat production atoleine |
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2021
- 2021-03-31 CN CN202110345394.4A patent/CN113337337B/en active Active
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| CN101074389A (en) * | 2007-06-01 | 2007-11-21 | 甘肃顺成化工有限责任公司 | Production of biological diesel oil |
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| WO2010136079A1 (en) * | 2008-06-17 | 2010-12-02 | Linde Aktiengesellschaft | Process for producing tall oil and use of brine deactivation in the production of tall oil |
| CN106318593A (en) * | 2016-08-25 | 2017-01-11 | 刘雁 | Recycled lubricating oil regeneration technology |
| CN106520381A (en) * | 2016-11-11 | 2017-03-22 | 云南磷化集团有限公司 | Decoloration and deodorization method for drainage oil fatty acid |
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Non-Patent Citations (1)
| Title |
|---|
| 李凌等: "《生物化学与分子生物学实验指导》", 31 August 2015 * |
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