CN113105949A - Equipment and process for producing high-purity octadecyl methyl ester by using waste animal and vegetable oil - Google Patents
Equipment and process for producing high-purity octadecyl methyl ester by using waste animal and vegetable oil Download PDFInfo
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- CN113105949A CN113105949A CN202110353895.7A CN202110353895A CN113105949A CN 113105949 A CN113105949 A CN 113105949A CN 202110353895 A CN202110353895 A CN 202110353895A CN 113105949 A CN113105949 A CN 113105949A
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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
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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
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
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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
- B01D3/16—Fractionating columns in which vapour bubbles through liquid
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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
- C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
- C11B7/0075—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of melting or solidifying points
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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
- C11C3/10—Ester interchange
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- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
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Abstract
The invention discloses equipment for producing high-purity octadecane methyl ester by using waste animal and vegetable oil, which comprises a heat exchanger, wherein one side of the heat exchanger is connected with three esterification towers at equal intervals through pipelines, and one side of one esterification tower is connected with a separation tank through a pipeline; the process of producing high purity methyl octadecanoate with waste animal and vegetable oil includes the following steps. The method has mild reaction conditions, can fully convert the waste animal and vegetable oil into the octadecane methyl ester, can obtain the octadecane methyl ester with the purity of 99 percent, the iodine value of more than 135 and the condensation point of less than or equal to minus 8 ℃, has high reaction speed of the rectification equipment, greatly improves the reaction time and the reaction quality compared with the conventional equipment, obtains a high-purity oil mixture, can ensure the full fusion of crude fatty acid methyl ester during rectification, and greatly ensures the output of the high-purity octadecane methyl ester through the improvement of the rectification equipment.
Description
Technical Field
The invention relates to the field of chemical production, in particular to equipment and a process for producing high-purity octadecane methyl ester by using waste animal and vegetable oil.
Background
The octadecane methyl ester has the characteristics of insolubility in water, flash point of more than 185 ℃, aromatic smell, no carcinogen, safe use and the like, is mainly applied to the aspects of cleaning of high-precision instruments and meters, raw materials for synthesizing nylon, novel ester cleaning agents and the like as a novel biological new material, and the application field of the octadecane methyl ester is continuously researched and developed, so that the market demand is increased.
The existing process technology for producing the octadecyl methyl ester by using the waste animal and vegetable oil has the defects of low raw material utilization rate, low octadecyl methyl ester purity and the like, has high process difficulty and high production cost, and is not beneficial to large-scale application of the process for converting the waste animal and vegetable oil into the octadecyl methyl ester in industrial production.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides equipment and a process for producing high-purity octadecane methyl ester by using waste animal and vegetable oil.
In order to achieve the purpose, the invention adopts the following technical scheme:
s1, esterification: animal and vegetable oil enters an esterification tower through a heat exchanger, and is subjected to esterification reaction with methanol in the esterification tower under the action of an organic acid catalyst to obtain an oil mixture;
s2, standing and separating: separating the grease mixture by a separation tank, removing impurities to obtain a grease solution, and feeding the grease solution into a storage tank through a pipeline;
s3, ester exchange: the grease solution in the storage tank enters an ester exchange tower to perform ester exchange reaction with methanol under the action of an alkaline catalyst to obtain a mixture of glycerol and crude fatty acid methyl ester;
s4, separation: introducing the mixture of the glycerol and the crude fatty acid methyl ester into a separator for separation to respectively obtain the glycerol and the crude fatty acid methyl ester;
s5, rectification: introducing the crude fatty acid methyl ester into a first rectifying tower, rectifying light components from the top of the first rectifying tower, rectifying mixed fatty acid methyl ester from the middle of the first rectifying tower, and obtaining heavy biodiesel from the bottom of the first rectifying tower;
s6, rectification: introducing the mixed fatty acid methyl ester into a second rectifying tower, and rectifying C from the tower top of the second rectifying tower14-C16And (4) distilling the methyl ester and the middle part to obtain the octadecyl methyl ester, namely the target product.
Preferably, in step S1, the organic acid catalyst is one of p-toluenesulfonic acid and methanesulfonic acid, the amount of methanol is more than 12% of the animal and vegetable fat, and the amount of the organic acid catalyst is 5% of the animal and vegetable fat.
Preferably, in the step S3, the grease solution in the storage tank enters the transesterification tower when the temperature is 50-80 ℃, and the alkaline catalyst is sodium hydroxide.
Preferably, the animal and vegetable oil and fat is one or more of acidified oil, illegal cooking oil, animal dirty oil, condensate oil of a range hood, clay refined desorption oil, oil sludge generated in an oil extraction process and beef and mutton tallow oil.
Preferably, the esterification reaction in the step S1 is a continuous esterification reaction.
Preferably, the pressure of the esterification reaction in the step S1 is normal pressure.
Preferably, the temperature of the esterification reaction in the step S1 is 50 to 120 ℃.
Utilize abandonment animal and vegetable fat production high purity methyl ester's equipment, including the heat exchanger, one side of heat exchanger has three esterifying tower through equidistant being connected with of pipeline, and there is the knockout drum one side of one of them esterifying tower through the pipe connection, the one end of knockout drum has the storage tank through the pipe connection, the one end of storage tank has the ester exchange tower through the pipe connection, the one end of ester exchange tower has the separator through the pipe connection, one side of separator has first rectifying column through the pipe connection, be equipped with two-way spray mechanism and liquid distribution mechanism in the first rectifying column, there is the second rectifying column one side middle part of first rectifying column through the pipe connection, lower extreme one side of first rectifying column and second rectifying column all is connected with the reboiler.
Preferably, the two-way mechanism that sprays is including the fixed pipe of fixed suit in first rectifying column one side, the one end of fixed pipe is connected with the connecting pipe, the both sides of connecting pipe all are connected with solid fixed ring, gu fixed ring's both ends are fixed on the relative lateral wall in first rectifying column through the clamp, gu fixed ring's upper end a week equidistant slope is fixed with a plurality of shower nozzles.
Preferably, liquid distribution mechanism is including setting up the liquid distributor in first rectifying column, and the top of liquid distributor setting in first rectifying column, install two packing layers in the first rectifying column, the upper end of packing layer is equipped with two dispersion boards, and fixes through a plurality of bracing pieces between two dispersion boards, and the lower extreme of one of them dispersion board is contradicted in the upper end of packing layer, a week equidistant of dispersion board is equipped with a plurality of distribution holes.
The method has mild reaction conditions, can fully convert the waste animal and vegetable oil into the octadecane methyl ester, the purity of the obtained octadecane methyl ester can reach 99 percent, the iodine value is more than 135, the condensation point is less than or equal to minus 8 ℃, the waste animal and vegetable oil can be converted into glycerol, C8-C12 methyl ester, heavy biodiesel and the like, the raw materials can be fully utilized, the waste is changed into valuable, the method is green and environment-friendly, meanwhile, the rectifying equipment has high reaction speed, the reaction time and the reaction quality are greatly improved compared with the conventional equipment, a high-purity oil mixture is obtained, meanwhile, the full fusion of crude fatty acid methyl ester during rectification can be ensured, and the output of the high-purity octadecane methyl ester is greatly ensured through the improvement of the rectifying equipment.
Drawings
FIG. 1 is a process flow diagram of the equipment for producing high-purity methyl octadecanoate by using waste animal and vegetable oil.
FIG. 2 is a schematic diagram of the internal structure of the first rectifying tower of the device for producing high-purity methyl octadecanoate from waste animal and vegetable oil.
FIG. 3 is a schematic structural diagram of a dispersing plate of an apparatus for producing high-purity methyl octadecanoate from waste animal and vegetable oils according to the present invention.
FIG. 4 is an enlarged view of the structure of the apparatus A for producing high-purity octadecyl methyl ester from waste animal and vegetable fats.
In the figure: 1 heat exchanger, 2 esterification towers, 3 knockout drum, 4 storage tanks, 5 ester exchange towers, 6 separators, 7 first rectifying column, 8 reboiler, 9 second rectifying column, 10 dispersion boards, 11 bracing pieces, 12 packing layers, 13 liquid distributors, 14 fixed rings, 15 connecting pipes, 16 fixed pipes, 17 clamps, 18 shower nozzles, 19 distribution holes.
Detailed Description
The technical solutions in the embodiments will be described clearly and completely with reference to the drawings in the embodiments, and it is obvious that the described embodiments are only a part of the embodiments, but not all embodiments.
Referring to fig. 2-4, the device comprises a heat exchanger 1, wherein three esterification towers 2 are connected to one side of the heat exchanger 1 at equal intervals through pipelines, one side of one esterification tower 2 is connected with a separation tank 3 through a pipeline, one end of the separation tank 3 is connected with a storage tank 4 through a pipeline, one end of the storage tank 4 is connected with an ester exchange tower 5 through a pipeline, one end of the ester exchange tower 5 is connected with a separator 6 through a pipeline, one side of the separator 6 is connected with a first rectifying tower 7 through a pipeline, the middle part of one side of the first rectifying tower 7 is connected with a second rectifying tower 9 through a pipeline, and the middle part of the second rectifying tower 9 is used for discharging octadecyl methyl ester with the purity of 99%.
In the invention, one side of the lower ends of the first rectifying tower 7 and the second rectifying tower 9 is connected with a reboiler 8, so that the waste animal and vegetable oil can be fully converted into the methyl octadecanoate, the purity of the obtained methyl octadecanoate can reach 99 percent, the iodine value is more than 135, the condensation point is less than or equal to minus 8 ℃, and the waste animal and vegetable oil can also be converted into glycerol and C14-C16Methyl ester, heavy biodiesel and the like, and the raw materials can be fully utilized, thereby changing waste into valuable and being environment-friendly.
In the invention, the bidirectional spraying mechanism comprises a fixed pipe 16 fixedly sleeved on one side of the first rectifying tower 7, one end of the fixed pipe 16 is connected with a connecting pipe 15, two sides of the connecting pipe 15 are both connected with fixed rings 14, two ends of each fixed ring 14 are fixed on opposite side walls in the first rectifying tower 7 through clamps 17, a plurality of spray heads 18 are obliquely fixed on the upper end of each fixed ring 14 at equal intervals in a circle, the spray heads 18 which are annularly arranged can uniformly spray, and are obliquely arranged at the same time, so that the scattering property of sprayed liquid is further improved, and the crude fatty acid methyl ester and the packing layer 12 can be fully fused.
In the invention, the liquid distribution mechanism comprises a liquid distributor 13 arranged in the first rectifying tower 7, the liquid distributor 13 is arranged at the top in the first rectifying tower 7, two packing layers 12 are arranged in the first rectifying tower 7, two dispersion plates 10 are arranged at the upper ends of the packing layers 12, the two dispersion plates 10 are fixed through a plurality of support rods 11, the lower end of one dispersion plate 10 abuts against the upper ends of the packing layers 12, a plurality of distribution holes 19 are arranged in the periphery of each dispersion plate 10 at equal intervals, the distribution holes 19 are arranged into a plurality of irregular holes, and the dispersion plates are rectangular, circular and the like, so that liquid drops can be fully intercepted, the liquid drops can be fully merged once again due to low drops, meanwhile, the dispersion plates 10 abut against the packing layers 12, and the packing layers 12 can be prevented from rising along with light components.
Referring to fig. 1, in the invention, the process of the equipment for producing high-purity methyl octadecanoate by using waste animal and vegetable oil comprises the following steps:
esterification: the method comprises the steps of enabling animal and vegetable oil to enter an esterification tower 2 through a heat exchanger 1, carrying out esterification reaction on the animal and vegetable oil and methanol in the esterification tower 2 under the action of an organic acid catalyst to obtain an oil mixture, wherein the organic acid catalyst is one of p-toluenesulfonic acid or methanesulfonic acid, the amount of the methanol is more than 12% of that of the animal and vegetable oil, the amount of the organic acid catalyst is 5 per mill of that of the animal and vegetable oil, the esterification reaction is a continuous esterification reaction, the pressure of the esterification reaction is normal pressure, and the temperature of the esterification reaction is 50-120 ℃.
Standing and separating: and after the oil mixture is separated by a separation tank 3, removing impurities to obtain an oil solution, wherein the oil solution enters a storage tank 4 through a pipeline, and the animal and vegetable oil comprises one or more of acidified oil, illegal cooking oil, animal visceral oil, condensate oil of a range hood, clay refined desorption oil, oil sludge generated in the oil pressing process and cow and sheep skin oil.
Ester exchange: the grease solution in the storage tank 4 enters the ester exchange tower 5 to perform ester exchange reaction with methanol under the action of an alkaline catalyst to obtain a mixture of glycerol and crude fatty acid methyl ester, the grease solution in the storage tank 4 enters the ester exchange tower 5 when the temperature is 50-80 ℃, and the alkaline catalyst is sodium hydroxide.
Separation: introducing the mixture of the glycerol and the crude fatty acid methyl ester into a separator 6 for separation to respectively obtain the glycerol and the crude fatty acid methyl ester;
and (3) rectification: introducing the crude fatty acid methyl ester into a first rectifying tower 7, rectifying light components from the top of the first rectifying tower 7, rectifying mixed fatty acid methyl ester from the middle of the first rectifying tower 7, and obtaining heavy biodiesel from the bottom of the first rectifying tower;
and (3) rectification: introducing the mixed fatty acid methyl ester into a second rectifying tower 9, and rectifying C from the top of the second rectifying tower 914-C16And (4) distilling the methyl ester and the middle part to obtain the octadecyl methyl ester, namely the target product.
In the invention, when the production of the octadecanoic methyl ester is needed, the acidified oil, the illegal cooking oil and the animal visceral oil are heated by a heat exchanger 1 in advance and then sent into an esterification tower 2, after the esterification reaction is carried out on the acidified oil, the illegal cooking oil and the animal visceral oil in the esterification tower 2 and a methyl alcohol and a p-toluenesulfonic acid organic acid catalyst, the amount of the methyl alcohol is more than 12 percent of that of the animal and vegetable oil, the amount of the p-toluenesulfonic acid organic acid catalyst is 5 per thousand of that of the animal and vegetable oil, the reaction temperature is 70 ℃, the reaction pressure is normal pressure, then the high-purity oil mixture is separated by a separation tank 3, impurities are removed to obtain a high-purity oil solution, the high-purity oil solution is conveyed into a storage tank 4 through a pipeline, then the high-purity oil solution in the storage tank 4 is conveyed into an ester exchange tower 5 to carry out the ester exchange reaction with an alkaline catalyst and the methyl alcohol to obtain a mixture of the glycerol and the crude fatty acid methyl ester, respectively obtaining glycerol and crude fatty acid methyl ester, then introducing the crude fatty acid methyl ester into a first rectifying tower 7, when rectifying in the first rectifying tower 7, the crude fatty acid methyl ester enters two fixed rings 14 through a fixed pipe 16 and a connecting pipe 15, and then the crude fatty acid methyl ester and the connecting pipe are all subjected to distillation through inclined spray heads 18Evenly spray to the both sides of two packing layers 12, liquid of lower extreme is after distribution hole 19 on dispersion plate 10, it is that the liquid drop is abundant low to fall on packing layer 12 of lower extreme, guarantee abundant integration, lighter component is through packing layer 12 and dispersion plate 10 of upper end with the liquid homodisperse once more in the lighter component, it is abundant integration to make it fall to hang down, the light component is rectified at first rectifying column 7 top to the part of lightest, mix fatty acid methyl ester in the middle part rectification, obtain heavy biodiesel in the bottom, at last with mixing in fatty acid methyl ester lets in second rectifying column 9, the top of the tower of second rectifying column 9 rectifies C14-C16Methyl ester and high-purity octadecyl methyl ester are rectified in the middle.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the scope of the present invention, and equivalents and modifications of the technical solutions and concepts thereof should be considered to be covered by the present invention.
Claims (8)
1. The process of the equipment for producing the high-purity octadecyl methyl ester by utilizing the waste animal and vegetable oil is characterized by comprising the following steps:
s1, esterification: animal and vegetable oil enters an esterification tower (2) through a heat exchanger (1), and is subjected to esterification reaction with methanol in the esterification tower (2) under the action of an organic acid catalyst to obtain an oil mixture;
s2, standing and separating: separating the grease mixture by a separation tank (3), removing impurities to obtain a grease solution, and feeding the grease solution into a storage tank (4) through a pipeline;
s3, ester exchange: the grease solution in the storage tank (4) enters an ester exchange tower (5) and is subjected to ester exchange reaction with methanol under the action of an alkaline catalyst to obtain a mixture of glycerol and crude fatty acid methyl ester;
s4, separation: introducing the mixture of the glycerol and the crude fatty acid methyl ester into a separator (6) for separation to respectively obtain the glycerol and the crude fatty acid methyl ester;
s5, rectification: introducing the crude fatty acid methyl ester into a first rectifying tower (7), rectifying light components at the top of the first rectifying tower (7), rectifying mixed fatty acid methyl ester in the middle, and obtaining heavy biodiesel at the bottom;
s6, rectification: introducing the mixed fatty acid methyl ester into a second rectifying tower (9), and rectifying C at the tower top of the second rectifying tower (9)14-C16And (4) distilling the methyl ester and the middle part to obtain the octadecyl methyl ester, namely the target product.
2. The process of the equipment for producing the high-purity octadecyl methyl ester by using the waste animal and vegetable oil and fat as the claim 1 is characterized in that: in the step S1, the organic acid catalyst is one of p-toluenesulfonic acid and methanesulfonic acid, the amount of methanol is more than 12% of the animal and vegetable fat, and the amount of the organic acid catalyst is 5% per mill of the animal and vegetable fat.
3. The process of the equipment for producing the high-purity octadecyl methyl ester by using the waste animal and vegetable oil and fat as claimed in claim 1, which is characterized in that: and in the step S3, when the temperature of the grease solution in the storage tank (4) is 50-80 ℃, the grease solution enters the ester exchange tower (5), and the alkaline catalyst is sodium hydroxide.
4. The process of the equipment for producing the high-purity octadecyl methyl ester by using the waste animal and vegetable oil and fat as claimed in claim 1, which is characterized in that: the animal and vegetable oil comprises one or more of acidified oil, illegal cooking oil, animal visceral oil, condensate oil of a range hood, clay refined desorption oil, oil sludge generated in the oil pressing process and cattle and sheep skin oil.
5. The process of the equipment for producing the high-purity octadecyl methyl ester by using the waste animal and vegetable oil and fat as claimed in claim 1, which is characterized in that: the esterification reaction in the step S1 is a continuous esterification reaction, the pressure of the esterification reaction in the step S1 is normal pressure, and the temperature of the esterification reaction in the step S1 is 50-120 ℃.
6. Utilize equipment of abandonment animal and vegetable oil production high-purity octadecyl methyl ester, including heat exchanger (1), its characterized in that: one side of heat exchanger (1) is connected with three esterification towers (2) through the pipeline equidistant, and there are knockout drum (3) one side of one of them esterification tower (2) through pipe connection, there are storage tank (4) one end of knockout drum (3) through pipe connection, there are ester exchange tower (5) one end of storage tank (4) through pipe connection, there are separator (6) one end of ester exchange tower (5) through pipe connection, there are first rectifying column (7) one side of separator (6) through pipe connection, be equipped with two-way spray mechanism and liquid distribution mechanism in first rectifying column (7), there are second rectifying column (9) in one side middle part of first rectifying column (7) through pipe connection, the lower extreme one side of first rectifying column (7) and second rectifying column (9) all is connected with reboiler (8).
7. The apparatus for producing high-purity octadecyl methyl ester by using waste animal and vegetable oil and fat according to claim 6, characterized in that: two-way spray mechanism is including fixed suit fixed pipe (16) in first rectifying column (7) one side, the one end of fixed pipe (16) is connected with connecting pipe (15), the both sides of connecting pipe (15) all are connected with solid fixed ring (14), the both ends of solid fixed ring (14) are passed through clamp (17) and are fixed on the relative lateral wall in first rectifying column (7), the upper end a week equidistant slope of solid fixed ring (14) is fixed with a plurality of shower nozzles (18).
8. The apparatus for producing high-purity octadecyl methyl ester by using waste animal and vegetable oil and fat according to claim 6, characterized in that: liquid distribution mechanism is including setting up liquid distributor (13) in first rectifying column (7), and liquid distributor (13) set up the top in first rectifying column (7), install two packing layers (12) in first rectifying column (7), the upper end of packing layer (12) is equipped with two dispersion boards (10), and fixes through a plurality of bracing pieces (11) between two dispersion boards (10), and the lower extreme of one of them dispersion board (10) is contradicted in the upper end of packing layer (12), a week equidistant of dispersion board (10) is equipped with a plurality of distribution holes (19).
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