CN212954953U - Device for producing fatty acid methyl ester by using low-concentration fatty acid and methanol - Google Patents
Device for producing fatty acid methyl ester by using low-concentration fatty acid and methanol Download PDFInfo
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Abstract
The utility model discloses a device for producing fatty acid methyl ester by using low-concentration fatty acid and methanol, which comprises a preheater, a fixed bed reactor, a catalytic distillation tower and a refining tower which are connected in sequence; reacting low-concentration fatty acid with methanol in a fixed bed reactor; the primary product enters a catalytic distillation tower to continue catalytic distillation reaction and is directly separated, and the esterification product at the bottom of the tower enters a product receiving device; the product at the top of the catalytic distillation tower is directly sent into a refining tower for separation without conventional tower top reflux; the recovered methanol is obtained at the top of the refining tower. The utility model discloses regard as the raw materials with the waste material that produces in the oleic acid production process, changing waste into valuables, fatty acid concentration not less than 10% can, the conversion rate of the product fatty acid that obtains is greater than or equal to 99.0%.
Description
Technical Field
The utility model relates to a device of production fatty acid methyl ester, concretely relates to utilize low concentration fatty acid and methyl alcohol to produce device of fatty acid methyl ester, further relate to an utilize device of low concentration fatty acid high conversion rate production fatty acid methyl ester.
Background
C12～C18The fatty acid methyl ester is one of the important raw materials for preparing the surfactant, and can be further processed into the epoxy fatty acid methyl ester, and the application of the epoxy fatty acid methyl ester in the field of the plasticizer is effectively promoted, so that the epoxy fatty acid methyl ester becomes an environment-friendly plasticizer which can replace phthalate plasticizers to a certain extent. When the carbon chain of the fatty acid is 12-18, the methyl ester is the basic component of the biodiesel. However, the production of domestic fatty acid ester uses a large amount of sulfuric acid catalytic process, which has the disadvantages of equipment corrosion and environmental pollution.
Chinese patent CN 208717200U discloses a method for producing fatty acid methyl ester by using fatty acid and methanol as raw materials, the production process adopts a new technology of a fixed bed and a catalytic distillation tower, because the catalytic distillation tower is provided with a material reflux device at the top of the tower, the water in the esterification reaction product of the fatty acid and the methanol flows back, the conversion rate of the fatty acid is not high, the waste of the fatty acid raw material exists, the impurity content of the fatty acid methyl ester product discharged from the bottom of the tower is high, and the economic benefit of the device investment is reduced.
China has a large amount of renewable resources, such as grease, which can generate a large amount of byproducts in the production process, wherein the byproducts comprise fatty glyceride in the form of esters and free fatty acid. A plurality of novel fatty acid esterification catalysts have been developed domestically based on environmental protection pressure, but the development of the fatty acid esterification process is less, the utility model provides a novel continuous esterification production process.
Disclosure of Invention
The utility model aims to solve the technical problem that the device for producing fatty acid methyl ester by using low-concentration fatty acid and methanol is provided aiming at the defects existing in the prior art. The device takes methanol and low-concentration fatty acid as raw materials, wherein the content of the fatty acid in the low-concentration fatty acid is more than 10 percent, and particularly relates to a fatty acid-containing waste material generated in the production process of the grease industry, which is a technology for producing fatty acid methyl ester by using the low-concentration fatty acid and the methanol.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
the utility model provides an utilize device of low concentration fatty acid methyl ester with methyl alcohol production fatty acid methyl ester, includes preheater, fixed bed reactor, catalytic distillation tower, the refining tower that connects gradually, its characterized in that:
the preheater be equipped with import and export, wherein: the inlet is divided into two paths, one path is connected with a device capable of providing fatty acid, and the other path is connected with a device capable of providing methanol;
fixed bed reactor, the top is equipped with feed inlet I, the bottom is equipped with discharge gate I, wherein: the feed inlet I is connected with the outlet of the preheater;
catalytic distillation tower, the top is equipped with gas vent I, the bottom is equipped with discharge gate II, the well upper portion of tower wall one side is equipped with feed inlet II, well lower part is equipped with feed inlet III, wherein: the feed inlet II is connected with a discharge outlet I of the fixed bed reactor; the feed port III is connected with a device capable of providing methanol, and excessive methanol is supplemented into the tower; an exhaust port I of the catalytic distillation tower is directly connected with a methanol recovery device, and a discharge port II is connected with a product receiving device;
methanol recovery unit be the refining tower, the refining tower top is equipped with gas vent II, the bottom is equipped with discharge gate III, the middle part of tower wall one side is equipped with feed inlet IV, the upper portion of tower wall opposite side is equipped with the backward flow mouth, wherein: the feed inlet IV is connected with an exhaust port I of the catalytic distillation tower; the exhaust port II is connected with a condenser and a reflux tank, and the outlet of the reflux tank is divided into two paths, wherein one path is connected with a reflux port, and the other path is connected with a device capable of providing methanol; the discharge port III is connected with a waste water receiving device.
In the technical scheme, the fixed bed reactor is internally filled with a catalyst A; the catalyst A is a solid acid catalyst, preferably a macroporous sulfonic acid cation resin catalyst.
In the technical scheme, the catalytic section of the catalytic distillation tower is filled with a catalyst B; the catalyst B is a solid acid catalyst, preferably a macroporous sulfonic acid cation resin catalyst.
In the technical scheme, the preheater, the fixed bed reactor, the catalytic distillation tower and the refining tower are all equipment in the prior art or commercially available equipment.
The utility model provides a method for producing fatty acid methyl ester by using low-concentration fatty acid and methanol, which comprises the following steps:
(1) esterification reaction: heating a low-concentration fatty acid raw material and methanol by a preheater, introducing the heated low-concentration fatty acid raw material and methanol into a fixed bed reactor through a feed inlet I, and carrying out esterification reaction on the methanol and the fatty acid under the catalytic action of a catalyst A in the fixed bed reactor to obtain a primary reaction product; the primary reaction product sequentially flows through a discharge port I and a feed port II and enters a catalytic distillation tower;
(2) catalytic distillation reaction: the primary reaction product formed in the fixed bed reactor enters a catalytic distillation tower, and is subjected to catalytic distillation reaction under the catalytic action of a catalyst B in the catalytic distillation tower and separated; separating to obtain light components at the top of the tower, wherein the light components are water and methanol, and are discharged from an exhaust port I and then connected with a refining tower; separating to obtain a final reaction product at the bottom of the tower, wherein the final reaction product is a mixture of fatty acid methyl ester, partial impurities in the low-concentration fatty acid raw material, trace fatty acid and trace methanol, and flows through a discharge hole II to be connected with a product receiving device; in the process of carrying out the catalytic distillation reaction, fresh and excessive methanol is introduced from the feed inlet III, so that the reaction is favorably carried out towards the direction of generating fatty acid methyl ester;
(3) refining: the material at the top of the catalytic distillation tower enters a refining tower and is separated in the refining tower, a light component is obtained at the top of the tower, the light component is gaseous methanol, the gaseous methanol is discharged from an exhaust port II and is condensed into liquid by a condenser and enters a reflux tank, one part of the material in the reflux tank returns to the refining tower through a reflux port for cyclic utilization, and the other part of the material is connected with a device capable of providing methanol; the heavy material discharged from the discharge port III at the bottom of the tower is connected with a waste water receiving device.
In the above technical scheme, in the step (1), the low-concentration fatty acid raw material is a waste material containing fatty acid generated in an industrial production process of oleic acid, wherein the concentration of the fatty acid is not lower than 10%.
In the above technical solution, in the step (1), the molar ratio of the fatty acid to the methanol in the low-concentration fatty acid raw material is 1: 3.
in the technical scheme, in the step (1), the low-concentration fatty acid raw material and methanol are heated to 70-80 ℃ by a preheater and then are introduced into a fixed bed reactor, and the space velocity is 0.6h-1。
In the above technical scheme, in the step (1), the esterification reaction conditions are as follows: the temperature is 70-80 ℃, and the pressure is 0.2-0.5 Mpa; the temperature is preferably 75 ℃ and the pressure is preferably 0.4 MPa.
In the above technical scheme, in the step (1), the catalyst a is a solid acid catalyst, preferably a macroporous sulfonic acid cationic resin catalyst.
In the technical scheme, in the step (2), the space velocity of the primary reaction product formed in the fixed bed reactor entering the catalytic distillation tower is 0.5-3h-1。
In the above technical scheme, in the step (2), the catalyst B is a solid acid catalyst, preferably a macroporous sulfonic acid cationic resin catalyst.
In the above technical scheme, in the step (2), the catalytic distillation reaction is performed under the following reaction conditions: the reaction temperature is 100-120 ℃, and the reaction pressure is 0.10-0.20 Mpa.
In the above technical solution, in the step (2), the catalytic distillation column has the following operating conditions: the temperature at the top of the tower is 80-120 ℃, and the pressure is 0.10-0.15 Mpa; the temperature of the tower bottom is 160-170 ℃, and the pressure is 0.15-0.35 Mpa.
In the technical scheme, in the step (2), the molar ratio of fresh and excessive methanol introduced into the catalytic distillation tower to methanol introduced into the preheater in the step (1) is 1-5: 1, preferably 3.5: 1.
in the above technical solution, in the step (3), the refining tower has the following operating conditions: the temperature at the top of the tower is 90-100 ℃, the pressure is 0.03-0.10 Mpa, the temperature at the bottom of the tower is 130-140 ℃, and the pressure is 0.10-0.25 Mpa.
In the technical scheme, in the step (3), the reflux is carried out at a reflux ratio of 10-12.
The utility model discloses technical scheme's advantage lies in:
(1) the utility model discloses a raw materials fatty acid can be for the waste material that produces in the oleic acid production process, and this waste material is useless for the danger, and this kind of waste material can not produce the benefit, needs to go out to take even and please other company to handle, causes the waste of fatty acid, brings economic benefits decline and environmental protection pressure, so the utility model discloses obvious economic benefits and environmental protection advantage have.
(2) The utility model discloses a raw materials fatty acid does not have high expectations to fatty acid's concentration, and fatty acid concentration is not less than 10% can.
(3) The utility model discloses a product conversion is high: the conversion rate of the fatty acid is more than or equal to 99.0 percent.
Drawings
FIG. 1: the utility model discloses the overall structure schematic diagram of the device;
wherein: 1 is a preheater, 2 is a fixed bed reactor, 3 is a catalytic distillation tower, and 4 is a refining tower.
Detailed Description
The following detailed description of the embodiments of the present invention, but the present invention is not limited to the following description:
the utility model provides an utilize device of low concentration fatty acid and methyl alcohol production fatty acid methyl ester, including preheater 1, fixed bed reactor 2, catalytic distillation tower 3, refining tower 4 that connect gradually, as shown in figure 1:
the preheater be equipped with import and export, wherein: the inlet is divided into two paths, one path is connected with a device capable of providing fatty acid, and the other path is connected with a device capable of providing methanol;
fixed bed reactor, the top is equipped with feed inlet I, the bottom is equipped with discharge gate I, wherein: the feed inlet I is connected with the outlet of the preheater;
catalytic distillation tower, the top is equipped with gas vent I, the bottom is equipped with discharge gate II, the well upper portion of tower wall one side is equipped with feed inlet II, well lower part is equipped with feed inlet III, wherein: the feed inlet II is connected with a discharge outlet I of the fixed bed reactor; the feed port III is connected with a device capable of providing methanol, and excessive methanol is supplemented into the tower; an exhaust port I of the catalytic distillation tower is directly connected with a methanol recovery device, and a discharge port II is connected with a product receiving device;
methanol recovery unit be the refining tower, the refining tower top is equipped with gas vent II, the bottom is equipped with discharge gate III, the middle part of tower wall one side is equipped with feed inlet IV, the upper portion of tower wall opposite side is equipped with backward flow mouth I, wherein: the feed inlet IV is connected with an exhaust port I of the catalytic distillation tower; the exhaust port II is connected with a condenser I and a reflux tank I, the outlet of the reflux tank I is divided into two paths, one path is connected with the reflux port I, and the other path is connected with a device capable of providing methanol; the discharge port III is connected with a waste water receiving device.
The fixed bed reactor is internally filled with a catalyst A; the catalyst A is a solid acid catalyst, preferably a macroporous sulfonic acid cation resin catalyst;
the catalytic section of the catalytic distillation tower is filled with a catalyst B; the catalyst B is a solid acid catalyst, preferably a macroporous sulfonic acid cation resin catalyst.
The utility model discloses in, pre-heater, fixed bed reactor, catalytic distillation tower, the refining tower is the equipment or the equipment of selling that prior art exists.
The utility model provides a method for producing fatty acid methyl ester by using low-concentration fatty acid and methanol, which comprises the following steps:
(1) esterification reaction: heating a low-concentration fatty acid raw material and methanol by a preheater, introducing the heated low-concentration fatty acid raw material and methanol into a fixed bed reactor through a feed inlet I, and carrying out esterification reaction on the methanol and the fatty acid under the catalytic action of a catalyst A in the fixed bed reactor to obtain a primary reaction product; the primary reaction product sequentially flows through a discharge port I and a feed port II and enters a catalytic distillation tower;
(2) catalytic distillation reaction: the primary reaction product formed in the fixed bed reactor enters a catalytic distillation tower, and is subjected to catalytic distillation reaction under the catalytic action of a catalyst B in the catalytic distillation tower and separated; after separation, light components are obtained at the tower top, wherein the light components are water and methanol, and are discharged from an exhaust port I and then connected with a refining tower, so that the esterification product of fatty acid and methanol, namely fatty acid methyl ester, is quickly separated from water; separating to obtain a final reaction product at the bottom of the tower, wherein the final reaction product is a mixture of fatty acid methyl ester, partial impurities in the low-concentration fatty acid raw material, trace fatty acid and trace methanol, and flows through a discharge hole II to be connected with a product receiving device; in the process of carrying out the catalytic distillation reaction, fresh and excessive methanol is introduced from the feed inlet III, so that the reaction is favorably carried out towards the direction of generating fatty acid methyl ester;
(3) refining: the material at the top of the catalytic distillation tower enters a refining tower and is separated in the refining tower, a light component is obtained at the top of the tower, the light component is gaseous methanol, the gaseous methanol is discharged from an exhaust port II and is condensed into liquid by a condenser and enters a reflux tank, one part of the material in the reflux tank returns to the refining tower through a reflux port for cyclic utilization, and the other part of the material is connected with a device capable of providing methanol; the heavy material discharged from the discharge port III at the bottom of the tower is connected with a waste water receiving device.
The invention is elucidated below in connection with specific embodiments:
example 1:
a method for producing fatty acid methyl ester by using low-concentration fatty acid and methanol specifically comprises the following steps:
(1) esterification reaction: methanol and fatty acid (molar ratio is 3: 1) are heated by a preheater to 65-70 ℃, and then are introduced into the fixed bed reactor from a feed inlet I, and the space velocity is 0.6h-1The methanol and the fatty acid are catalyzed by a catalyst A in a fixed bed reactor at 65-70 DEGPerforming esterification reaction at 0.4Mpa at deg.C to obtain primary reaction product; the primary reaction product sequentially flows through a discharge port I and a feed port II and enters a catalytic distillation tower;
the fatty acid raw material is waste generated in the production process of oleic acid, wherein the concentration of fatty acid is 50%, the concentration of heavy substances which do not participate in the reaction is 45%, and the balance is water;
the catalyst A is a macroporous sulfonic acid cation resin catalyst and adopts a KC105D type fatty acid esterification catalyst of Kery environmental protection science and technology Limited.
(2) Catalytic distillation reaction: the primary reaction product formed in the fixed bed reactor (space velocity of 2 h)-1) Entering a catalytic distillation tower, carrying out catalytic distillation reaction on a reaction section under the operation conditions of 100-110 ℃ and 0.10-0.15 Mpa under the catalytic action of a catalyst B in the catalytic distillation tower, and separating; after separation, light components are obtained at the top of the tower, wherein the light components comprise water (20% by mass) and methanol (80% by mass), and are discharged from an exhaust port I and enter a refining tower; separating to obtain a final reaction product at the bottom of the tower, wherein the final reaction product is a mixture of fatty acid methyl ester, partial impurities in raw material fatty acid, about 30 percent of methanol and a small amount of fatty acid, and flows through a discharge hole II to be connected with a product receiving device; during the catalytic distillation reaction, fresh, excess methanol was introduced at feed port III in a molar ratio of 3.5: 1.
the catalyst B is a macroporous sulfonic acid cation resin catalyst and adopts a KC105D type fatty acid esterification catalyst of Kery environmental protection science and technology Limited company;
the top operation conditions of the catalytic distillation tower are as follows: the temperature is 85-90 ℃, the pressure is 0.10-0.15 Mpa, and the tower bottom operation conditions are as follows: the temperature is 165-170 ℃, and the pressure is 0.25-0.30 Mpa;
(3) refining: the material at the top of the catalytic distillation tower enters a refining tower and is separated in the refining tower, a light component is obtained at the top of the tower, the light component is gaseous methanol, the gaseous methanol is discharged from an exhaust port II and is condensed into liquid through a condenser I to enter a reflux tank I, one part of the material in the reflux tank I returns to the refining tower through a reflux port I for cyclic utilization, and the other part of the material is connected with a device capable of providing methanol; the heavy material discharged from the discharge port III at the bottom of the tower is connected with a waste water receiving device.
The tower top operating conditions of the refining tower are as follows: the temperature is 90-100 ℃, the pressure is 0.03-0.1 Mpa, and the tower bottom operation conditions are as follows: the temperature of the tower bottom is 130-140 ℃, and the pressure is 0.10-0.25 Mpa;
the reflux ratio of the refining tower is 10.
In the product of this example, the conversion of fatty acid was 99.1%.
Example 2:
a method for producing fatty acid methyl ester by using low-concentration fatty acid and methanol specifically comprises the following steps:
(1) esterification reaction: methanol and fatty acid (molar ratio is 4: 1) are heated by a preheater to 70-80 ℃, and then are introduced into the fixed bed reactor from a feed inlet I, and the space velocity is 0.6h-1Carrying out esterification reaction on methanol and fatty acid under the catalytic action of a catalyst A in a fixed bed reactor at 70-80 ℃ and 0.4Mpa to obtain a primary reaction product; the primary reaction product sequentially flows through a discharge port I and a feed port II and enters a catalytic distillation tower;
the fatty acid raw material is waste generated in the production process of oleic acid, wherein the concentration of fatty acid is 12%, the concentration of heavy substances which do not participate in the reaction is 87%, and the balance is water;
the catalyst A is a macroporous sulfonic acid cation resin catalyst and adopts a KC105D type fatty acid esterification catalyst of Kery environmental protection science and technology Limited.
(2) Catalytic distillation reaction: the primary reaction product formed in the fixed bed reactor (space velocity of 2 h)-1) Entering a catalytic distillation tower, carrying out catalytic distillation reaction in a reaction section under the operation conditions of 110-120 ℃ and 0.10-0.15 Mpa under the catalytic action of a catalyst B in the catalytic distillation tower, and separating; separating to obtain light components at the top of the tower, wherein the light components comprise water (10% by mass) and methanol (90% by mass), and discharging the light components from an exhaust port I to enter a refining tower; separating to obtain final-stage reaction product at the bottom of the towerIs a mixture of fatty acid methyl ester, partial impurities in raw material fatty acid, about 30 percent of methanol and a small amount of fatty acid, and flows through a discharge port II to be connected with a product receiving device; during the catalytic distillation reaction, fresh, excess methanol was introduced at feed port III in a molar ratio of 5: 1.
the catalyst B is a macroporous sulfonic acid cation resin catalyst and adopts a KC105D type fatty acid esterification catalyst of Kery environmental protection science and technology Limited company;
the top operation conditions of the catalytic distillation tower are as follows: the temperature is 90-95 ℃, the pressure is 0.10-0.15 Mpa, and the tower bottom operation conditions are as follows: the temperature is 165-170 ℃, and the pressure is 0.25-0.30 Mpa;
(3) refining: the material at the top of the catalytic distillation tower enters a refining tower and is separated in the refining tower, a light component is obtained at the top of the tower, the light component is gaseous methanol, the gaseous methanol is discharged from an exhaust port II and is condensed into liquid through a condenser I to enter a reflux tank I, one part of the material in the reflux tank I returns to the refining tower through a reflux port I for cyclic utilization, and the other part of the material is connected with a device capable of providing methanol; the heavy material discharged from the discharge port III at the bottom of the tower is connected with a waste water receiving device.
The tower top operating conditions of the refining tower are as follows: the temperature is 90-100 ℃, the pressure is 0.03-0.1 Mpa, and the tower bottom operation conditions are as follows: the temperature of the tower bottom is 130-140 ℃, and the pressure is 0.10-0.25 Mpa;
the reflux ratio of the refining tower is 10.
In the product of this example, the conversion of fatty acid was 99.5%.
The above examples are merely illustrative of the technical concept and technical features of the present invention, and thus the scope of the present invention is not limited thereto. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (7)
1. The utility model provides an utilize device of low concentration fatty acid methyl ester with methyl alcohol production fatty acid methyl ester, includes preheater (1), fixed bed reactor (2), catalytic distillation tower (3), refining tower (4) its characterized in that connect gradually:
the preheater (1) is provided with an inlet and an outlet, wherein: the inlet is divided into two paths, one path is connected with a device capable of providing fatty acid, and the other path is connected with a device capable of providing methanol;
fixed bed reactor (2), the top is equipped with feed inlet I, the bottom is equipped with discharge gate I, wherein: the feed inlet I is connected with the outlet of the preheater;
catalytic distillation tower (3), the top is equipped with gas vent I, the bottom is equipped with discharge gate II, the well upper portion of tower wall one side is equipped with feed inlet II, well lower part is equipped with feed inlet III, wherein: the feed inlet II is connected with a discharge outlet I of the fixed bed reactor; the feed port III is connected with a device capable of providing methanol, and excessive methanol is supplemented into the tower; an exhaust port I of the catalytic distillation tower is directly connected with a methanol recovery device, and a discharge port II is connected with a product receiving device;
methanol recovery unit be refining tower (4), the refining tower top be equipped with gas vent II, the bottom is equipped with discharge gate III, the middle part of tower wall one side is equipped with feed inlet IV, the upper portion of tower wall opposite side is equipped with backward flow mouth I, wherein: the feed inlet IV is connected with an exhaust port I of the catalytic distillation tower; the exhaust port II is connected with a condenser I and a reflux tank I, the outlet of the reflux tank I is divided into two paths, one path is connected with the reflux port I, and the other path is connected with a device capable of providing methanol; the discharge port III is connected with a waste water receiving device.
2. The device for producing fatty acid methyl esters of claim 1, wherein: the fixed bed reactor is internally filled with a catalyst A.
3. The device for producing fatty acid methyl esters of claim 2, wherein: the catalyst A is a solid acid catalyst.
4. The device for producing fatty acid methyl esters of claim 3, wherein: the catalyst A is a macroporous sulfonic acid cation resin catalyst.
5. The device for producing fatty acid methyl esters of claim 1, wherein: the catalytic distillation tower is filled with a catalyst B in a catalytic section.
6. The device for producing fatty acid methyl esters of claim 5, wherein: the catalyst B is a solid acid catalyst.
7. The device for producing fatty acid methyl esters of claim 6, wherein: the catalyst B is a macroporous sulfonic acid cation resin catalyst.
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