CN113862085A - Process for producing methyl ester by using waste oil - Google Patents
Process for producing methyl ester by using waste oil Download PDFInfo
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- CN113862085A CN113862085A CN202111059697.6A CN202111059697A CN113862085A CN 113862085 A CN113862085 A CN 113862085A CN 202111059697 A CN202111059697 A CN 202111059697A CN 113862085 A CN113862085 A CN 113862085A
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- Prior art keywords
- methyl ester
- glycerol
- methanol
- waste oil
- reactor
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/06—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils with glycerol
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/10—Ester interchange
Abstract
The invention discloses a process for producing methyl ester by using waste grease, which comprises the following working steps: (1) collecting kitchen waste grease raw materials and recycling glycerol and putting the raw materials and the recycled glycerol into an esterification reactor; (2) preheating to control temperature and vacuum; (3) carrying out reverse esterification reaction on glycerol and free fatty acid; (4) reducing the acid value of the material to 2 mgKOH/g; (5) adding methanol and a catalyst in a certain proportion, mixing in a batching tank, and then putting into an ester exchange reactor; (6) discharging reaction products of glycerol and soap at the bottom settling part of the reactor to a glycerol treatment section after reaction; (7) putting the obtained crude methyl ester into a heat exchanger for heat exchange and heating; (8) heating the mixed methyl ester to enter a distillation tower, carrying out evaporation separation on the methyl ester in the distillation tower, wherein the heavy impurities removed from the bottom of the distillation tower are plant asphalt, and collecting the mixed methyl ester in an intermediate tank after the mixed methyl ester is condensed and refluxed by a condenser at the top of the distillation tower; the waste kitchen grease which cannot be directly used is utilized and the recovered glycerol is matched to refine the methyl ester, so that the resources are effectively utilized.
Description
Technical Field
The invention relates to the technical field of methyl ester production, in particular to a process for producing methyl ester by using waste grease.
Background
The methyl ester is also called fatty acid methyl ester, is a raw material of biodiesel with wide application, and can be used for producing two major surfactants from the fatty acid methyl ester; one is the production of fatty acid Methyl Ester Sulfonate (MES) by sulfonation neutralization and the other is the production of fatty alcohol by hydrogenation; the price is expensive; if the product is directly purchased, a large amount of cost is consumed, and the product is inconvenient for the long-term development of enterprises; at present, an acid-base two-step method is mainly adopted for producing methyl ester, acid catalysis is required to be carried out when the acid value is high in the production process, the produced waste acid is more, the pollution is larger, and the current concepts of green environmental protection and sustainable development cannot be met.
In view of the above, there is a need for an improved methyl ester production process that can accommodate the current needs for methyl ester production.
Disclosure of Invention
Because a two-step acid-base method is usually adopted during the production of methyl ester at present, high acid value must be catalyzed, more waste acid is generated, and the pollution is larger, a process for producing methyl ester by using waste gas oil is designed on the basis of the defects of the prior art, a strong acid catalysis pre-esterification process of the two-step acid-base method is not needed during the production of the oil by a high acid value waste method, the acid value is reduced by adopting a glycerin de-esterification process without a catalyst, after the acid value is reduced, the methanol ester exchange is directly catalyzed by alkali, the corrosion of equipment can be avoided without using strong acid, and the pollution of strong acid waste water to the environment is reduced importantly.
The technical scheme of the invention is that the process for producing methyl ester by using waste grease comprises the following working steps:
(1) collecting kitchen waste grease raw materials and recycling glycerol and putting the raw materials and the recycled glycerol into an esterification reactor;
(2) preheating to control temperature and vacuum;
(3) heating to a reaction temperature by using a heater, and carrying out an esterification reaction on the glycerol and the free fatty acid;
(4) reducing the acid value of the material to 2mgKOH/g, and controlling the temperature of the material by heat exchange;
(5) adding methanol and a catalyst in a certain proportion, mixing in a batching tank, then putting into an ester exchange reactor, and controlling a certain reaction temperature; (ii) a
(6) Discharging reaction products of glycerol and soap at a sedimentation part at the bottom of the reactor to a glycerol treatment section after reacting for a certain time, then putting the rest reactants into a second-stage ester exchange reactor and a third-stage ester exchange reactor, continuously supplementing methanol and a catalyst, and enabling the materials to flow into a sedimentation tank after the reaction is finished; separating the bottom crude glycerin and the upper crude methyl ester;
(7) putting the obtained crude methyl ester into a heat exchanger for heat exchange and heating;
(8) heating to a certain temperature, feeding the methyl ester into a distillation tower, carrying out evaporation separation on the methyl ester in the distillation tower, removing heavy impurities at the bottom of the distillation tower to be plant asphalt, condensing and refluxing the mixed methyl ester by a tower top condenser, and collecting the mixed methyl ester in an intermediate tank; wherein the distillation column is powered by a reboiler;
(9) the mixed methyl ester in the intermediate tank is controlled to a certain extent by a pump through a flowmeter; the flow enters a rectifying tower for fractionation, wherein light components, namely low-sulfur methyl ester, are removed by fractionation at the top of the tower, and a low-carbon methyl ester product is condensed and refluxed by a condenser at the top of the tower.
Further supplementing the technical scheme, the crude methyl ester obtained in the step (6) is heated and then enters a flash tank to remove methanol.
The technical scheme is further supplemented, quantitative acid is added after methanol removal is finished, the mixture is uniformly mixed, and the mixture enters a centrifugal machine after being heated so as to remove residual glycerin and soap, and the obtained crude methyl ester is subjected to methyl ester rectification.
And (3) further supplementing the technical scheme, after a small amount of high-carbon substances are removed by tower bottom cutting in the step (9), continuously putting the high-carbon substances into a distillation tower for distillation, and recovering heavy-component high-carbon methyl ester.
The technical proposal is further supplemented, the crude glycerol in the step (6) is processed, and the methanol is rectified and recovered.
The technical proposal is further supplemented, the reaction products of glycerin and soap at the bottom settling part of the reactor in the step (6) are treated, and the products of crude glycerin and acidified oil are collected.
The technical proposal is further supplemented, and the reaction products of the glycerol, the soap and the crude glycerol obtained in the step (6) are rectified and recycled by methanol.
The technical proposal is further supplemented, and the methanol obtained after the rectification and recovery of the methanol is recycled to the step (5). The substance which is mixed with the waste water is the waste water which is treated and discharged quantitatively.
The technical proposal is further supplemented, and a certain amount of acid is citric acid after the methanol removal is finished.
The method has the advantages that the kitchen waste grease which cannot be directly used is utilized and the recovered glycerin is matched to further refine the methyl ester, so that enterprises can conveniently use the methyl ester as the raw material of the diesel oil, resources can be effectively utilized, the waste materials are recycled, and the enterprise expenditure cost is reduced; the strong acid catalysis pre-esterification process of an acid-base two-step method is not needed during the production of the high-acid-value waste method grease, the acid value is reduced by adopting a glycerin de-esterification process without a catalyst, the methanol ester exchange is directly catalyzed by alkali after the acid value is reached, the corrosion of equipment can be avoided without using strong acid, and the pollution of the strong acid wastewater to the environment is reduced importantly.
Detailed Description
Because a two-step acid-base method is usually adopted during the production of methyl ester at present, high acid value must be catalyzed, more waste acid is generated, and the pollution is larger, a process for producing methyl ester by using waste gas oil is designed on the basis of the defects of the prior art, a strong acid catalysis pre-esterification process of the two-step acid-base method is not needed during the production of the oil by a high acid value waste method, the acid value is reduced by adopting a glycerin de-esterification process without a catalyst, after the acid value is reduced, the methanol ester exchange is directly catalyzed by alkali, the corrosion of equipment can be avoided without using strong acid, and the pollution of strong acid waste water to the environment is reduced importantly.
In order to make the technical solution more clear to those skilled in the art, the technical solution of the present invention will be explained in detail below:
firstly, introducing raw materials adopted by the technical scheme, namely, kitchen waste oil generally refers to various inferior oils in life, such as recovered edible oil, repeatedly used frying oil and the like, and the occurrence of the kitchen waste oil not only pollutes the environment, but also can cause serious potential safety hazards of diet caused by the kitchen waste oil reflowing to a dining table; secondly, the recovered glycerin is oil produced by refining swill reserved and discharged by hotels, restaurants and food processing enterprises, and the normal regulation is to forbid the processing of the waste grease into edible oil, so in order to effectively utilize resources, people try to convert the waste grease from kitchens and the recovered glycerin into safer and more useful products; in life, because the cost of methyl ester is high, the purchase cost is high, and the pressure for enterprises is high, the technical scheme is designed for the long-term development of enterprises and the recycling of resources for various reasons, and comprises the following steps:
a process for producing methyl ester by using waste oil comprises the following working steps:
(1) collecting kitchen waste grease raw materials and recycling glycerol and putting the raw materials and the recycled glycerol into an esterification reactor; (ii) a
(2) Preheating the kitchen waste grease raw material and recovering glycerin for transesterification reaction to control the temperature and vacuum, wherein before the kitchen waste grease raw material and the recovered glycerin are subjected to transesterification reaction, the kitchen waste grease raw material is placed in a heat exchanger for temperature control, and then free moisture is removed in a grease dehydration tank;
(3) heating the raw materials in the step (2) to a reaction temperature by using a heater so as to perform an esterification reaction on the glycerol and the free fatty acid;
(4) reducing the acid value of the material to 2mgKOH/g, and controlling the temperature of the material by heat exchange;
(5) adding methanol and a catalyst in a certain proportion, mixing in a batching tank, then putting into an ester exchange reactor, and controlling a certain reaction temperature;
(6) discharging reaction products of glycerol and soap at a sedimentation part at the bottom of the reactor to a glycerol treatment working section after reacting for a certain time, and specifically, treating the reaction products of the glycerol and the soap to obtain crude glycerol and acidified oil; then putting the rest reactants into a second-stage ester exchange reactor and a third-stage ester exchange reactor, continuously supplementing methanol and a catalyst, and enabling the materials to flow into a settling tank after the reaction is finished; processing the bottom crude glycerol by a separation method, subsequently processing the crude glycerol, and rectifying and recovering methanol;
separating the upper crude methyl ester, wherein the upper crude methyl ester may contain more methanol, a small amount of glycerol, soap and other substances, and therefore needs to be reprocessed, namely heating the obtained crude methyl ester and then feeding the crude methyl ester into a flash tank to remove methanol; adding a certain amount of acid after the methanol removal is finished, uniformly mixing, preferably using citric acid as the acid, heating, and then feeding into a centrifugal machine to remove residual glycerol and soap, and performing methyl ester rectification on the obtained crude methyl ester;
(7) putting the obtained crude methyl ester into a heat exchanger for heat exchange and heating;
(8) heating to a certain temperature, feeding the methyl ester into a distillation tower, carrying out evaporation separation on the methyl ester in the distillation tower, removing heavy impurities at the bottom of the distillation tower to be plant asphalt, condensing and refluxing the mixed methyl ester by a tower top condenser, and collecting the mixed methyl ester in an intermediate tank; wherein the distillation column is powered by a reboiler;
(9) the mixed methyl ester in the intermediate tank is controlled to a certain extent by a pump through a flowmeter; the flow enters a rectifying tower for fractionation, wherein light components, namely low-sulfur methyl ester, are removed by fractionation at the top of the tower, and a low-carbon methyl ester product is condensed and refluxed by a condenser at the top of the tower; after removing a small amount of high-carbon substances from the bottom of the tower in the step (9), continuously putting the high-carbon substances into a distillation tower for distillation, and recovering heavy-component high-carbon methyl ester; the four products are low-sulfur methyl ester product, low-carbon methyl ester, high-carbon methyl ester and plant asphalt respectively;
further, for better utilization of resources, the reaction products of glycerol and soap and crude glycerol obtained in the step (6) are subjected to methanol rectification recovery treatment, and the methanol obtained after methanol rectification recovery is recycled to the step (5); the substance which is mixed with the waste water is the waste water which is treated and discharged quantitatively.
The technical solutions described above only represent the preferred technical solutions of the present invention, and some possible modifications to some parts of the technical solutions by those skilled in the art all represent the principles of the present invention, and fall within the protection scope of the present invention.
Claims (9)
1. A process for producing methyl ester by using waste oil is characterized by comprising the following working steps:
(1) collecting kitchen waste grease raw materials and recycling glycerol and putting the raw materials and the recycled glycerol into an esterification reactor;
(2) preheating to control temperature and vacuum;
(3) heating to a reaction temperature by using a heater, and carrying out an esterification reaction on the glycerol and the free fatty acid;
(4) reducing the acid value of the material to 2mgKOH/g, and controlling the temperature of the material by heat exchange;
(5) adding methanol and a catalyst in a certain proportion, mixing in a batching tank, then putting into an ester exchange reactor, and controlling a certain reaction temperature; (ii) a
(6) Discharging reaction products of glycerol and soap at a sedimentation part at the bottom of the reactor to a glycerol treatment section after reacting for a certain time, then putting the rest reactants into a second-stage ester exchange reactor and a third-stage ester exchange reactor, continuously supplementing methanol and a catalyst, and enabling the materials to flow into a sedimentation tank after the reaction is finished; separating the bottom crude glycerin and the upper crude methyl ester;
(7) putting the obtained crude methyl ester into a heat exchanger for heat exchange and heating;
(8) heating to a certain temperature, feeding the methyl ester into a distillation tower, carrying out evaporation separation on the methyl ester in the distillation tower, removing heavy impurities at the bottom of the distillation tower to be plant asphalt, condensing and refluxing the mixed methyl ester by a tower top condenser, and collecting the mixed methyl ester in an intermediate tank; wherein the distillation column is powered by a reboiler;
(9) the mixed methyl ester in the intermediate tank is controlled to a certain extent by a pump through a flowmeter; the flow enters a rectifying tower for fractionation, wherein light components, namely low-sulfur methyl ester, are removed by fractionation at the top of the tower, and a low-carbon methyl ester product is condensed and refluxed by a condenser at the top of the tower.
2. The process for producing methyl ester by using waste oil and fat as claimed in claim 1, wherein the crude methyl ester obtained in the step (6) is heated and then enters a flash tank to remove methanol.
3. The process for producing methyl ester by using waste oil and fat as claimed in claim 2, wherein the methyl ester is rectified by adding a predetermined amount of acid after the methanol removal, mixing uniformly, heating, and feeding into a centrifuge to remove residual glycerin and soap.
4. The process for producing methyl ester by using waste oil and fat as claimed in claim 1, wherein after a small amount of high-carbon substances are removed from the bottom of the tower in the step (9), the high-carbon substances are continuously distilled in a distillation tower, and heavy high-carbon methyl ester is recovered.
5. The process for producing methyl ester by using waste oil and fat as claimed in claim 1, wherein the crude glycerol in the step (6) is treated and rectified and recycled by methanol.
6. The process for producing methyl ester by using waste oil and fat as claimed in claim 1, wherein the reaction product glycerol and soap settled at the bottom of the reactor in the step (6) are treated, and the crude glycerol and the acidified oil are collected.
7. The process for producing methyl ester by using waste oil and fat as claimed in claim 6, wherein the reaction product glycerol and soap obtained in step (6) and crude glycerol are subjected to methanol rectification recovery treatment.
8. The process for producing methyl ester by using waste oil and fat as claimed in claim 7, wherein the methanol obtained after rectification and recovery of methanol is recycled to the step (5). The substance which is mixed with the waste water is the waste water which is treated and discharged quantitatively.
9. The process for producing methyl ester by using waste oil and fat as claimed in claim 3, wherein the acid added in a certain amount after the methanol removal is completed is citric acid.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111059697.6A CN113862085A (en) | 2021-09-09 | 2021-09-09 | Process for producing methyl ester by using waste oil |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111059697.6A CN113862085A (en) | 2021-09-09 | 2021-09-09 | Process for producing methyl ester by using waste oil |
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| CN113862085A true CN113862085A (en) | 2021-12-31 |
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Citations (7)
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| US20100175312A1 (en) * | 2009-01-13 | 2010-07-15 | Allan Donald Roden | Method for producing biodiesel material |
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| CN103820224A (en) * | 2014-03-13 | 2014-05-28 | 安徽天意环保科技有限公司 | Biodiesel and preparation method thereof |
| CN106675789A (en) * | 2017-01-24 | 2017-05-17 | 江苏悦达卡特新能源有限公司 | Method for preparing biodiesel with low sulfur content from gutter oil |
| CN106929162A (en) * | 2017-03-30 | 2017-07-07 | 迈安德集团有限公司 | A kind of utilization waste grease produces the deacidification technique of glycerine |
| CN108277090A (en) * | 2018-01-30 | 2018-07-13 | 浙江工业大学 | A kind of preparation method of low-sulphur biodiesel |
| CN111019720A (en) * | 2019-12-31 | 2020-04-17 | 浙江卓尚环保能源有限公司 | Green production process of biodiesel |
-
2021
- 2021-09-09 CN CN202111059697.6A patent/CN113862085A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100175312A1 (en) * | 2009-01-13 | 2010-07-15 | Allan Donald Roden | Method for producing biodiesel material |
| CN103060097A (en) * | 2012-12-30 | 2013-04-24 | 上海油好同盟新能源科技有限公司 | Continuous production line for producing biodiesel under catalysis of solid catalyst |
| CN103820224A (en) * | 2014-03-13 | 2014-05-28 | 安徽天意环保科技有限公司 | Biodiesel and preparation method thereof |
| CN106675789A (en) * | 2017-01-24 | 2017-05-17 | 江苏悦达卡特新能源有限公司 | Method for preparing biodiesel with low sulfur content from gutter oil |
| CN106929162A (en) * | 2017-03-30 | 2017-07-07 | 迈安德集团有限公司 | A kind of utilization waste grease produces the deacidification technique of glycerine |
| CN108277090A (en) * | 2018-01-30 | 2018-07-13 | 浙江工业大学 | A kind of preparation method of low-sulphur biodiesel |
| CN111019720A (en) * | 2019-12-31 | 2020-04-17 | 浙江卓尚环保能源有限公司 | Green production process of biodiesel |
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