CN112587948A - Fatty acid methyl ester rectification method - Google Patents
Fatty acid methyl ester rectification method Download PDFInfo
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- CN112587948A CN112587948A CN202011375122.0A CN202011375122A CN112587948A CN 112587948 A CN112587948 A CN 112587948A CN 202011375122 A CN202011375122 A CN 202011375122A CN 112587948 A CN112587948 A CN 112587948A
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- fatty acid
- methyl ester
- acid methyl
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
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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
- C11B3/12—Refining fats or fatty oils by distillation
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- Fats And Perfumes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a fatty acid methyl ester rectification method and fatty acid methyl ester rectification equipment. Specifically, the fatty acid methyl ester rectification method comprises the following steps: heating the crude fatty acid methyl ester by a tube heater before the crude fatty acid methyl ester enters the rectifying tower. The fatty acid methyl ester rectification equipment comprises a fatty acid methyl ester rectification tower, a tubular heater and a kettle liquid discharge pump; according to the method provided by the invention, only part of the kettle liquid pumped out needs to be heated by adding the tube nest heater, so that the fatty acid methyl ester residue can meet the discharge condition, the mode of completely heating the kettle liquid in the traditional distillation process is changed, the distillation efficiency is improved, and the distillation energy consumption is reduced.
Description
Technical Field
The application belongs to the technical field of biodiesel purification, and particularly relates to a fatty acid methyl ester rectification method.
Background
The biodiesel is an environment-friendly biomass energy source, is developed for more than 10 years in China as a fuel oil and petrochemical fuel in a mixed way, and is a very good environment-friendly biochemical raw material, namely fatty acid methyl ester.
Biodiesel, i.e., fatty acid methyl ester, with chemical formula RCOOCH3(wherein R is C12～17) The diesel oil is mainly prepared from vegetable oil (rice bran oil, cottonseed oil, crambe, peanut oil, rapeseed oil, soybean oil, sunflower seed oil and the like) or animal fat serving as a raw material, is a diesel oil substitute which is obtained from renewable biomass resources and has the property similar to that of diesel oil, and is a biomass renewable energy source. The main component is esters such as methyl ester or ethyl ester formed by long-chain fatty acid. The biodiesel uses alcohols such as methanol or ethanol and Triglyceride (Triglyceride) which is a main component in natural vegetable oil or animal fat to perform Transesterification reaction (Transesterification), replaces glyceryl on long-chain fatty acid with methoxyl, and breaks the Triglyceride into a plurality of long-chain fatty acid methyl esters, thereby reducing the length of a carbon chain, reducing the viscosity of the oil material, improving the fluidity and the vaporization performance of the oil material, and meeting the requirements of using the oil material as fuel.
The current methods for preparing biodiesel mainly comprise: 1) an esterification method in which an esterification reaction is carried out between fats and oils and methanol in the presence of an acidic catalyst; 2) an ester exchange method in which an ester exchange reaction is carried out between fats and oils and methanol in the presence of an alkaline catalyst; 3) for waste oil with more impurities such as waste oil, especially waste oil with higher content of free fat and acid, the ester exchange reaction can not be directly carried out by adopting alkaline catalysis, and generally esterification is carried out first and then base-catalyzed ester exchange is carried out.
After the raw oil is treated by an acid-base two-step method, a fatty acid methyl ester product can be obtained by reduced pressure rectification. At present, domestic enterprises generally adopt a packing vacuum tower to carry out vacuum distillation purification on fatty acid methyl ester, and the method ensures the purity of the fatty acid methyl ester by controlling the temperature of the top of the packing tower in the rectification process; the volatilization (residual amount) of the fatty acid methyl ester in the kettle liquid is ensured by controlling the kettle temperature. To simultaneously achieve the production of high-purity fatty acid methyl ester product and the low residue of the still liquid, the reflux ratio and the evaporation amount need to be increased simultaneously.
Relatively speaking, the purity index of distillate (main product) is realized by improving the reflux ratio, and the residue of the kettle liquid is ensured by increasing the evaporation capacity, which has great test on the separation effect of the rectifying tower; energy consumption also presents a major challenge for product quality. The thermal stability of the fatty acid methyl ester is not high, and the polymerization reaction of the kettle liquid can be caused after the evaporation amount (kettle temperature) is increased, thereby influencing the product yield and increasing the production cost. Rectification at high temperature can greatly damage the smell and color of the fatty acid methyl ester product, and influence the quality of the final product; meanwhile, the storage amount of the kettle liquid is large, so that the retention time of materials is too long, and the rectification yield is influenced by the reverse reaction.
For example, in order to achieve a fatty acid methyl ester purity of 95% and an acid value of less than 0.5, the reflux ratio should be increased to 1: 1-1.2: 1, and when the reflux ratio is increased, the temperature of the kettle should reach 245 ℃ in order to reduce the residual amount of the product in the kettle, however, the polymerization reaction of the fatty acid methyl ester in the kettle is aggravated at such a high temperature.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the fatty acid methyl ester rectification optimization method which is simple, efficient, low in energy consumption, stable in product quality and more suitable for industrial production.
The technical scheme adopted by the invention for solving the technical problems is as follows: provided is a fatty acid methyl ester rectification method, comprising: heating the crude fatty acid methyl ester by a tube heater before the crude fatty acid methyl ester enters the rectifying tower.
Further preferably, the fatty acid methyl ester rectification method comprises: and (3) connecting the rectifying tower kettle liquid with a bottom feed inlet of a tubular heater from a bottom discharge port of the rectifying tower kettle through a connecting pipe, allowing the kettle liquid to enter the tubular heater for evaporation, allowing residual fatty acid methyl ester in the kettle liquid entering the tubular heater to be vaporized, allowing the residue to enter the rectifying tower through an upper riser of the tubular heater, and discharging the concentrated kettle liquid from a kettle liquid discharge pump.
In the above method, the residual amount of fatty acid methyl ester in the discharged partial still is preferably controlled by controlling the flow rate of the discharge pump and the evaporation temperature of the tubular heater. Wherein, preferably, the discharge temperature of the tube nest heater is 200-250 ℃, and the temperature of the liquid in the rectifying tower is 200-220 ℃.
Further, after the kettle liquid is evaporated by a tube still heater, the gas-phase fatty acid methyl ester enters a rectifying tower from a steam outlet of the evaporator, and the concentrated kettle liquid is directly discharged by a kettle liquid discharging pump.
In another preferred embodiment of the present invention, there is provided a fatty acid methyl ester rectification method comprising the steps of:
s1: opening a heat-conducting oil inlet and outlet valve of the tube array heater to preheat the tube array heater;
s2: opening a fatty acid methyl ester tower kettle valve and a bottom feeding valve of a tubular heater to enable kettle liquid to flow from the bottom of the heater to the bottom of the distillation tower;
s3: opening an inlet valve of a discharging pump when the temperature of an air rising pipe of the tube array heater and the temperature of a discharge port of the tube array heater rise to 200-;
s4: slowly opening a discharge valve of a discharge pump, adjusting the discharge flow, and controlling the flow to be in a specified range;
s5: after the system is stable, sampling and analyzing the residual amount of fatty acid methyl ester in the concentrated solution, and adjusting the opening amount of the discharge valve to enable the concentrated solution to reach the preset required concentration.
The second aspect of the invention also provides fatty acid methyl ester rectification equipment, which comprises a fatty acid methyl ester rectification tower, a tube array heater and a kettle liquid discharge pump;
wherein, a discharge port at the bottom of the rectifying tower is connected with a feed inlet at the bottom of the tube array heater through a communicating pipe, the upper part of the tube array heater is connected with the rectifying tower through a riser, and residual fatty acid methyl ester in the kettle liquid entering the tube array heater is vaporized and then enters the rectifying tower through the riser at the upper part of the tube array heater;
the tube nest heater is used for evaporating the entering kettle liquid, and the kettle liquid discharging pump is used for discharging the concentrated kettle liquid.
Specifically, when the fatty acid methyl ester rectification equipment is used: and (3) automatically flowing the bottom liquid of the rectifying tower into the tubular heater through the communicating pipe for heating and evaporation, vaporizing residual fatty acid methyl ester in the bottom liquid in the tubular heater, and then feeding the vaporized residual fatty acid methyl ester into the rectifying tower, and directly discharging the low-volatility bottom liquid from the bottom liquid discharge pump. Further preferably, the flow rate of the still liquid discharging pump and the evaporation temperature of the tube still heater are controlled to control the discharge of part of the still liquid residue. Further, the discharge temperature of the tubular heater is controlled to be 200-250 ℃, and the temperature of the liquid in the kettle of the rectifying tower is controlled to be 200-220 ℃.
According to the method provided by the invention, only part of the kettle liquid pumped out needs to be heated by adding the tube nest heater, so that the fatty acid methyl ester residue can meet the discharge condition, the mode of completely heating the kettle liquid in the traditional distillation process is changed, the distillation efficiency is improved, and the distillation energy consumption is reduced. The method provided by the invention does not need to reduce the volatilization of the whole tower bottom liquid by maintaining the temperature of the whole tower bottom liquid, and the heat energy consumption of the heat conducting oil can be reduced by 20 percent. The invention can control the holding amount of the kettle liquid to be at an extremely low level by adding the tube nest heater, the liquid level of the conventional distillation kettle is generally controlled to be within the liquid level height range of 1.5-1.8 m, the liquid level of the kettle liquid can be reduced to be within the range of 0.8-1 m by the invention, the retention time of materials is reduced to 1.5h from 3h, the reverse reaction generation in the rectification process is reduced, and the distillation yield can be improved by 2-3 points; compared with the conventional rectification process, the method can effectively reduce the temperature of the kettle liquid, reduce the odor and color quality of the product, and reduce the color from No. 70 to No. 50 as shown in figure 2.
Drawings
The technical solution of the present application is further explained below with reference to the drawings and the embodiments.
FIG. 1 is a schematic diagram of the structure of the apparatus used in the fatty acid methyl ester rectification method and the rectification flow;
wherein reference numeral 1: draft tube, 2: communication pipe, 3: conduction oil inlet valve, 4: conduction oil outlet valve, 5: tubular heater feed valve, 6: column bottom valve, 7: draft tube thermometer, 8: tube heater material thermometer.
FIG. 2 is a comparison of the color numbers of fatty acid methyl esters obtained by the rectification method of the present invention and the prior art method;
wherein, the left side is marked with 'modified' which means that the fatty acid methyl ester real object color chart prepared by the rectification method provided by the invention is basically colorless and transparent, and the color is No. 50;
the right side is marked with a physical picture of fatty acid methyl ester obtained by rectifying the fatty acid methyl ester by adopting the conventional equipment without adding a tubular heater, and the physical picture is yellow and transparent and has a color of No. 70.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
Example 1:
as shown in fig. 1, a fatty acid methyl ester rectification apparatus comprises a fatty acid methyl ester rectification tower, a tubular heater and a still liquid discharge pump;
wherein, a discharge port at the bottom of the rectifying tower is connected with a feed inlet at the bottom of a tube array heater through a communicating pipe 2, the upper part of the tube array heater is connected with the rectifying tower through a gas riser 1, and residual fatty acid methyl ester in the kettle liquid entering the tube array heater is vaporized and then enters the rectifying tower through the gas riser 1 at the upper part of the tube array heater;
the tube nest heater is used for evaporating the entering kettle liquid, and the kettle liquid discharging pump is used for discharging the concentrated kettle liquid.
When the device is used, the bottom liquid of the rectifying tower automatically flows into the tube array heater through the communicating tube to be heated and evaporated, residual fatty acid methyl ester in the bottom liquid in the heater enters the rectifying tower after being vaporized, and the low-volatilization bottom liquid is directly discharged by the bottom liquid discharge pump. And controlling the flow of the kettle liquid discharging pump and the evaporation temperature of the tube still heater to control the residual of the discharged kettle liquid. In this embodiment, the discharge temperature of the tubular heater is controlled to be 200-250 ℃, and the temperature of the liquid in the distillation tower is controlled to be 200-220 ℃.
Wherein the fatty acid methyl ester rectifying tower is a conventional distillation tower, in the embodiment, the design productivity is 50 tons/day, tower kettle reboilers adopt externally-hung falling film evaporators, the heat exchange areas of the two reboilers are respectively 100 square meters, and two 60m reboilers are equipped3A/h circulating pump.
As shown in figure 2, compared with the product obtained by the conventional rectifying tower without a tubular heater, the product obtained by the method of the invention can reduce the color from No. 70 to No. 50, and the color of the product is obviously improved.
Example 2
A fatty acid methyl ester distillation process comprising the steps of:
as shown in fig. 1, the heat conducting oil inlet and outlet valves 3 and 4 of the tubular heater are opened first to preheat the heater.
Then, a fatty acid methyl ester column bottom valve 6 and a tubular heater bottom feed valve 5 are opened, so that the kettle liquid flows in from the bottom of the tubular heater from the bottom of the distillation column. Observing the temperature 7 of the riser of the tube array heater and the temperature 8 of the discharge port of the tube array heater, opening an inlet valve of the discharge pump when the temperature rises to 200-250 ℃, and starting the kettle liquid discharge pump.
And slowly opening a discharge valve of the discharge pump, adjusting the discharge flow, and controlling the flow to be in a specified range.
And after the system is stabilized for 5 minutes, sampling and analyzing the residual amount of fatty acid methyl ester in the concentrated solution, and adjusting the opening amount of a discharge valve to enable the concentrated solution to reach the preset required concentration.
According to the invention, by adding the tube nest heater, only a small amount of kettle liquid needs to be heated for the second time, so that the mode of completely heating the kettle liquid in the traditional distillation process is changed, the distillation efficiency is improved, and the distillation energy consumption is reduced. Furthermore, the fatty acid methyl ester rectifying tower used in the embodiment of the invention is a conventional distillation tower, the designed capacity is 50 tons/day, tower kettle reboilers adopt externally-hung falling film evaporators, the heat exchange areas of the two reboilers are respectively 100 square meters, and two 60m rectifying towers are equipped3A/h circulating pump. The cost of conventional distillation energy consumption is about: 135 yuan/ton (wherein the hot oil is 110); the invention increases the tubular heater to evaporate the kettle liquid through technical transformation, and the hot oil distillation cost is reduced by 18.5 yuan/ton. In addition, after the tube still heater is changed in form, the residue of the fatty acid methyl ester in the kettle liquid is reduced from 15 percent to 2 percent, and the comprehensive yield is improved by 1.95 percent according to the accounting of 15 percent of the kettle liquid.
In light of the foregoing description of the preferred embodiments according to the present application, it is to be understood that various changes and modifications may be made without departing from the spirit and scope of the invention. The technical scope of the present application is not limited to the contents of the specification, and must be determined according to the scope of the claims.
Claims (7)
1. A fatty acid methyl ester rectification method is characterized by comprising the following steps: heating the crude fatty acid methyl ester by a tube heater before the crude fatty acid methyl ester enters the rectifying tower.
2. The fatty acid methyl ester rectification method according to claim 1, comprising: and (3) connecting the rectifying tower kettle liquid with a bottom feed inlet of a tubular heater from a bottom discharge port of the rectifying tower kettle through a connecting pipe, allowing the kettle liquid to enter the tubular heater for evaporation, allowing residual fatty acid methyl ester in the kettle liquid entering the tubular heater to be vaporized, allowing the residue to enter the rectifying tower through an upper riser of the tubular heater, and discharging the concentrated kettle liquid from a kettle liquid discharge pump.
3. The method for rectifying fatty acid methyl ester according to claim 1, wherein the residual amount of fatty acid methyl ester in the discharged partial still is controlled by controlling the flow rate of a discharge pump and the evaporation temperature of a tube heater.
4. The method for rectifying fatty acid methyl ester according to claim 1, wherein the discharge temperature of the tubular heater is controlled to be 200 to 250 ℃ and the temperature of the liquid in the rectifying tower is controlled to be 200 to 220 ℃.
5. The fatty acid methyl ester rectification method according to claim 1, characterized in that after the still liquid is evaporated by the tube still heater, the gas phase fatty acid methyl ester enters the rectification tower from the steam outlet of the evaporator, and the concentrated still liquid is directly discharged by the still liquid discharge pump.
6. The fatty acid methyl ester rectification method according to claim 1, characterized by comprising the steps of:
s1: opening a heat-conducting oil inlet and outlet valve of the tube array heater to preheat the tube array heater;
s2: opening a fatty acid methyl ester tower kettle valve and a bottom feeding valve of a tubular heater to enable kettle liquid to flow from the bottom of the heater to the bottom of the distillation tower;
s3: opening an inlet valve of a discharging pump when the temperature of an air rising pipe of the tube array heater and the temperature of a discharge port of the tube array heater rise to 200-;
s4: slowly opening a discharge valve of a discharge pump, adjusting the discharge flow, and controlling the flow to be in a specified range;
s5: after the system is stable, sampling and analyzing the residual amount of fatty acid methyl ester in the concentrated solution, and adjusting the opening amount of the discharge valve to enable the concentrated solution to reach the preset required concentration.
7. A fatty acid methyl ester rectification device is characterized by comprising a fatty acid methyl ester rectification tower, a tube array heater and a kettle liquid discharge pump;
wherein, a discharge port at the bottom of the rectifying tower is connected with a feed inlet at the bottom of the tube array heater through a communicating pipe, the upper part of the tube array heater is connected with the rectifying tower through a riser, and residual fatty acid methyl ester in the kettle liquid entering the tube array heater is vaporized and then enters the rectifying tower through the riser at the upper part of the tube array heater;
the tube nest heater is used for evaporating the entering kettle liquid, and the kettle liquid discharging pump is used for discharging the concentrated kettle liquid.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4595461A (en) * | 1983-06-23 | 1986-06-17 | Henkel Kommanditgesellschaft Auf Aktien | Process for the non-degenerative distillation of fatty acids |
| DE19531806C1 (en) * | 1995-08-30 | 1997-04-10 | Henkel Kgaa | Fine distillation of 6-24C fatty acids from plant or animal fats etc. |
| CN102628006A (en) * | 2012-04-13 | 2012-08-08 | 东南大学 | Catalytic distillation production method for biodiesel |
| CN203728804U (en) * | 2014-02-28 | 2014-07-23 | 上海中器环保科技有限公司 | Electrical heating biodiesel distillation tower |
| CN103977592A (en) * | 2014-05-30 | 2014-08-13 | 烟台国邦化工机械科技有限公司 | Rectification device comprising two reboilers and method for removing light solvent by using device |
| CN204607959U (en) * | 2015-04-28 | 2015-09-02 | 广东河山环保有限公司 | A kind of biofuel column |
| CN105695104A (en) * | 2016-03-29 | 2016-06-22 | 天津大学 | Intra-tower pump suction type high vacuum distillation method and device for precise separation of C16-C22 fatty acids |
| CN107312625A (en) * | 2017-06-14 | 2017-11-03 | 常州工程职业技术学院 | The technique of fatty acid methyl ester in a kind of multitower continuous rectification separation biodiesel |
-
2020
- 2020-11-30 CN CN202011375122.0A patent/CN112587948A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4595461A (en) * | 1983-06-23 | 1986-06-17 | Henkel Kommanditgesellschaft Auf Aktien | Process for the non-degenerative distillation of fatty acids |
| DE19531806C1 (en) * | 1995-08-30 | 1997-04-10 | Henkel Kgaa | Fine distillation of 6-24C fatty acids from plant or animal fats etc. |
| CN102628006A (en) * | 2012-04-13 | 2012-08-08 | 东南大学 | Catalytic distillation production method for biodiesel |
| CN203728804U (en) * | 2014-02-28 | 2014-07-23 | 上海中器环保科技有限公司 | Electrical heating biodiesel distillation tower |
| CN103977592A (en) * | 2014-05-30 | 2014-08-13 | 烟台国邦化工机械科技有限公司 | Rectification device comprising two reboilers and method for removing light solvent by using device |
| CN204607959U (en) * | 2015-04-28 | 2015-09-02 | 广东河山环保有限公司 | A kind of biofuel column |
| CN105695104A (en) * | 2016-03-29 | 2016-06-22 | 天津大学 | Intra-tower pump suction type high vacuum distillation method and device for precise separation of C16-C22 fatty acids |
| CN107312625A (en) * | 2017-06-14 | 2017-11-03 | 常州工程职业技术学院 | The technique of fatty acid methyl ester in a kind of multitower continuous rectification separation biodiesel |
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