CN214571789U - Device for continuously preparing biodiesel - Google Patents
Device for continuously preparing biodiesel Download PDFInfo
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- CN214571789U CN214571789U CN202023004879.7U CN202023004879U CN214571789U CN 214571789 U CN214571789 U CN 214571789U CN 202023004879 U CN202023004879 U CN 202023004879U CN 214571789 U CN214571789 U CN 214571789U
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Abstract
The application discloses serialization preparation biodiesel's device, including two stirred tank reactors, two jar and a tubular reactor of stewing, the back is preheated to methyl alcohol solution and the reaction liquid that contain the catalyst, get into first stirred tank reactor reaction, then the separation of stewing is upper grease layer and lower floor's glycerine, upper grease layer gets into second stirred tank reactor reaction back, the jar separation that stews of reentrant second, the mixture that the jar bottom of second stewing depositd reenters first stirred tank reactor, the oil reservoir result that the upper exit of jar was stood to the second and another part contain the methyl alcohol solution of catalyst and get into tubular reactor in the lump, reach reaction balance after, the cooling gets into the product jar. When the device is used for preparing the biodiesel, the methanol in the raw materials can be recycled, the cost required by the reaction is reduced, the ester exchange conversion rate is improved, and the biodiesel is continuously produced.
Description
Technical Field
The application relates to a device for continuously preparing biodiesel.
Background
With the continuous development of the industry in China, the demand of petrochemical resources is continuously increased, and certain energy crisis is brought while the economic level is improved. The exploitation and utilization of non-renewable energy sources cause serious pollution to the ecological environment. Nowadays, the construction of ecological civilization is continuously strengthened in China, the industrial production is pushed to move to the direction of environmental protection and sustainability, and meanwhile, the industrial production faces the problems of price rise and industrial production cost improvement caused by shortage of petroleum resources. Under the double pressure of resource shortage and too high production cost, biodiesel, a nontoxic, biodegradable and renewable product, is selected as an alternative fuel. At present, the yield of the biodiesel in the world is continuously increased, but the production method is various, and the production method is generally adopted, is also an intermittent production mode, and is also continuously produced. Chinese patent CN203513652U discloses an intermittent biodiesel preparation device, which has a simple structure, does not need a stirring device, and can perform stirring function while feeding by itself. Chinese patent CN202912930U discloses that adding a co-solvent increases the content of methanol in the oil phase and the content of oil in the supercritical methanol phase simultaneously, which increases the reaction rate, but introducing a co-solvent will cause inconvenience in subsequent treatment and increase the cost of raw materials. CN106800976A discloses a method for continuously preparing biodiesel by glycerol circulation, wherein heated crude oil and glycerol are simultaneously introduced into a reactor, and esterification reaction is directly carried out by controlling temperature, vacuum degree and raw material flow. After the reaction, the mixture and the methanol dissolved with the potassium hydroxide are simultaneously introduced into a continuous ester exchange reactor for circular reaction. However, the transesterification reaction is reversible and requires a higher alcohol/oil molar ratio to increase the conversion. The method for continuously preparing the biodiesel can recycle the methanol in the raw materials, reduce the cost required by the reaction and improve the conversion rate of the grease.
Disclosure of Invention
To the above-mentioned technical problem that prior art exists, the aim at of this application provides a device of serialization preparation biodiesel, and the problem of biodiesel's serialization production can be solved to this application, can practice thrift the human cost, reduces the methyl alcohol quantity.
The device for continuously preparing the biodiesel is characterized by comprising a preheater, two stirring reactors, two standing tanks, a reactant delivery pump and a tubular reactor, wherein a reaction liquid of raw oil, methanol and a catalyst is preheated by the preheater and then introduced into a first stirring reactor for reaction, and an outlet at the bottom of the first stirring reactor is connected with a feed inlet in the middle of the first standing tank through a pipeline; the first standing tank plays a role in layering, an outlet at the bottom of the first standing tank is connected with the glycerin tank through a first glycerin pump by a pipeline, and an outlet at the upper layer of the first standing tank is connected with an inlet of the second stirring reactor through a pipeline;
an outlet at the bottom of the second stirring reactor is connected with a feed inlet in the middle of a second standing tank through a pipeline, the second standing tank plays a role in layering, and a mixture of glycerol and unreacted methanol discharged from the outlet at the bottom of the second standing tank can be reused in the first stirring reactor;
the inlet of the reactant delivery pump is divided into two paths, one path is filled with a methanol solution containing a catalyst, and the other path is filled with a product flowing out from an upper outlet of the second standing tank; the outlet of the reactant delivery pump is connected with the inlet of the tubular reactor through a pipeline, and the outlet of the tubular reactor is connected with the product tank through a cooler and a pipeline.
The device for continuously preparing the biodiesel is characterized by further comprising a methanol tank, a grease storage tank, a methanol delivery pump, a grease delivery pump and a second glycerin pump, wherein a methanol solution containing a catalyst is contained in the methanol tank; the outlet at the bottom of the methanol tank is connected with the inlet of a methanol delivery pump through a pipeline, the outlet of the methanol delivery pump is divided into two paths, one path is connected with the inlet of a preheater through the pipeline, and the other path is connected with the inlet of one path of a reactant delivery pump through the pipeline so as to input a methanol solution containing a catalyst into the reactant delivery pump; an outlet at the bottom of the grease storage tank is connected with an inlet of the preheater through a grease delivery pump by a pipeline, and an outlet at the bottom of the second standing tank is connected with an inlet of the preheater through a second glycerin pump by a pipeline; flow meters and regulating valves are arranged on the corresponding pipelines.
The method for continuously preparing the biodiesel by adopting the device is characterized by comprising the following steps of:
1) dissolving a catalyst in methanol to form a methanol solution, and dividing the prepared methanol solution into two parts for feeding; mixing a first part of methanol solution with raw oil to form a reaction liquid, preheating the reaction liquid by a preheater, introducing the reaction liquid into a first stirring reactor for stirring reaction, introducing a first-stage reaction product flowing out of an outlet at the bottom of the first stirring reactor into a first standing tank, layering the reaction product into an upper oil layer and a lower glycerin layer, collecting the lower glycerin layer in a glycerin tank, and introducing the upper oil layer into a second stirring reactor for stirring reaction;
2) and introducing a second-stage reaction product flowing out from an outlet at the bottom of the second stirring reactor into a second standing tank for standing and layering, returning a mixture of glycerol and methanol which is not completely reacted and precipitated at the bottom of the second standing tank into the first stirring reactor, mixing a product on the upper layer of the second standing tank with a second part of methanol solution, then flowing into the tubular reactor for continuous reaction, cooling the final product by a cooler, and collecting the final product in a product tank to obtain the biodiesel product.
Further, the catalyst is at least one of NaOH, KOH, sodium methoxide and potassium methoxide, and the total mass of the catalyst dissolved in the methanol solution of the two parts is 0.2-3% of the mass of the raw oil; the raw oil is vegetable oil.
Further, in the step 1), the residence time of the reaction liquid in the first stirring reactor is 0.2-2 hours, preferably 0.4-1 hour; the reaction temperature in the first stirring reactor is 50-100 ℃, and preferably 64-65 ℃; the stirring speed during the reaction is 50-200 rpm.
Further, in the step 2), the reaction residence time in the second stirring reactor is 0.2-2 hours, preferably 0.4-1 hour; the reaction temperature in the second stirring reactor is 50-100 ℃, and preferably 64-65 ℃; the stirring speed during the reaction is 50-200 rpm.
Further, in the step 1), the mass flow ratio of the first part of methanol solution to the raw oil is 0.3-0.8: 1; the mass flow ratio of the second part of methanol solution in the step 2) to the raw oil in the step 1) is 0.1-0.5: 1.
Furthermore, the reaction residence time in the tubular reactor is 2-40 min, and the reaction temperature in the tubular reactor is 50-100 ℃, preferably 64-65 ℃.
The beneficial effects obtained by the invention are as follows:
1. the production device comprises two stirring reactors, two standing tanks and a tubular reactor, wherein reaction liquid of raw oil, methanol and a catalyst enters the first stirring reactor for reaction after being preheated, then is subjected to standing separation to form an upper grease layer and lower glycerin layer, and the upper grease layer enters the second stirring reactor and then enters the second standing tank for separation of glycerin. And the mixture of the glycerin precipitated at the bottom of the second standing tank and the methanol which is not completely reacted enters the first stirring reactor again, and the methanol dissolved in the glycerin is fully utilized. And mixing the incompletely reacted oil layer flowing out of the upper outlet of the second standing tank with the other part of the methanol solution containing the catalyst, allowing the mixture to enter a tubular reactor, and cooling the mixture to enter a product tank after reaction balance is achieved. The invention can fully recycle the methanol in the glycerol, improve the ester exchange conversion rate and realize the continuous production of the biodiesel; the method for continuously preparing the biodiesel can recycle the methanol in the raw materials, reduce the cost required by the reaction and improve the conversion rate of the grease.
2. The device has simple structure, scientific and reasonable design, high ester exchange efficiency and capability of reducing manual operation and continuously carrying out ester exchange reaction.
3. In the whole process, the incompletely reacted glycerin and the methanol dissolved in the glycerin realize the function of recycling, the cost of raw materials is reduced, and the conversion efficiency of the biodiesel is improved.
Drawings
FIG. 1 is a schematic structural diagram of a continuous biodiesel production apparatus according to the present invention;
in fig. 1: the method comprises the following steps of 1-a methanol tank, 2-a grease storage tank, 3-a methanol delivery pump, 4-a grease delivery pump, 5-a regulating valve, 6-a flow meter, 9-a preheater, 10-a first stirring reactor, 11-a first standing tank, 12-a first glycerine pump, 13-a second stirring reactor, 14-a second standing tank, 15-a second glycerine pump, 16-a tubular reactor, 17-a cooler, 18-a product tank, 19-a glycerine tank and 20-a reactant delivery pump.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example (b): compare FIG. 1
A device for continuously preparing biodiesel comprises a preheater 9, two stirring reactors, two standing tanks, a reactant delivery pump 20 and a tubular reactor, wherein a reaction liquid of raw oil, methanol and a catalyst is preheated by the preheater 9 and then introduced into a first stirring reactor 10 for reaction, and an outlet at the bottom of the first stirring reactor 10 is connected with a feed inlet in the middle of a first standing tank 11 through a pipeline; the first standing tank 11 plays a role in layering, the bottom outlet of the first standing tank 11 is connected with the glycerin tank 19 through a first glycerin pump 12 by a pipeline, and the upper outlet of the first standing tank 11 is connected with the inlet of the second stirring reactor 13 through a pipeline. An outlet at the bottom of the second stirring reactor 13 is connected with a feed inlet in the middle of the second standing tank 14 through a pipeline, the second standing tank 14 plays a role in layering, and a mixture of glycerol and unreacted methanol discharged from an outlet at the bottom of the second standing tank 14 can be reused in the first stirring reactor 10; the inlet of the reactant delivery pump 20 is divided into two paths, one path is introduced into the methanol solution containing the catalyst, and the other path is introduced into the product flowing out from the upper outlet of the second standing tank 14; the outlet of the reactant transfer pump 20 is connected to the inlet of the pipe reactor 16 via a pipe, and the outlet of the pipe reactor 16 is connected to the product tank 18 via a cooler 17 via a pipe.
Referring to fig. 1, the device of the present application further includes a methanol tank 1, a grease storage tank 2, a methanol delivery pump 3, a grease delivery pump 4, and a second glycerin pump 15, wherein the methanol tank 1 contains a methanol solution containing a catalyst. An outlet at the bottom of the methanol tank 1 is connected with an inlet of a methanol delivery pump 3 through a pipeline, an outlet of the methanol delivery pump 3 is divided into two paths, one path is connected with an inlet of a preheater 9 through a pipeline, and the other path is connected with an inlet of one path of a reactant delivery pump 20 through a pipeline so as to input a methanol solution containing a catalyst into the reactant delivery pump 20; an outlet at the bottom of the grease storage tank 2 is connected with an inlet of the preheater 9 through a grease delivery pump 4 by a pipeline, and an outlet at the bottom of the second standing tank 14 is connected with the preheater 9 through a second glycerin pump 15 by a pipeline; and a flowmeter 6 and a regulating valve 5 are arranged on the corresponding pipelines.
Example 1:
a method for continuously preparing biodiesel (the production device adopts the structure shown in figure 1) comprises the following processes:
1) the KOH catalyst is dissolved in methanol to form a methanol solution, and the prepared methanol solution is divided into two parts to be fed.
The first part of the methanol solution was fed to the preheater at a flow rate of 5kg/h, while the soybean oil was fed to the preheater at a flow rate of 10 kg/h; the reaction materials are heated to 65 ℃ by the preheater and then flow into the first stirring reactor to be stirred and reacted at 65 ℃ (the stirring speed is 70 rpm), and the residence time of the reaction liquid in the first stirring reactor is 1 h; the first-stage reaction product flows into a first standing tank and is layered into an upper grease layer and a lower layer of glycerin, the lower layer of glycerin is collected in a glycerin tank, the upper grease layer enters a second stirring reactor again to be stirred and reacted, the stirring reaction is carried out at 65 ℃ (the stirring speed is 70 rpm), and the residence time of the reaction liquid in the second stirring reactor is 1 h;
2) and introducing a second-stage reaction product flowing out from an outlet at the bottom of the second stirring reactor into a second standing tank for standing and layering, and returning a mixture of the glycerol and the incompletely reacted methanol precipitated at the bottom of the second standing tank into the first stirring reactor for continuous cyclic reaction. And (3) an upper layer outlet of the second standing tank flows out of an oil layer product which is not completely reacted, and the yield of the biodiesel product is about 92 percent by detecting the oil layer product.
3) And (3) allowing an oil layer product which is not completely reacted to flow out of an upper layer outlet of the second standing tank to flow into the tubular reactor, allowing a second part of methanol solution to flow into the tubular reactor at a flow rate of 3kg/h for continuous reaction, allowing the reaction temperature in the tubular reactor to be 65 ℃, allowing the reaction solution to stay in the tubular reactor for 20min, allowing the reaction solution to flow into a cooler for cooling to room temperature, and collecting a biodiesel product in a product tank to obtain the biodiesel with the yield of 98.6%.
Wherein the total mass of KOH dissolved in the two methanol solutions is 1% of the mass of soybean oil.
Example 2:
a method for continuously preparing biodiesel (the production device adopts the structure shown in figure 1) comprises the following processes:
1) the KOH catalyst is dissolved in methanol to form a methanol solution, and the prepared methanol solution is divided into two parts to be fed.
The first part of the methanol solution was fed to the preheater at a flow rate of 8kg/h, while the soybean oil was fed to the preheater at a flow rate of 10 kg/h; the reaction materials are heated to 65 ℃ by the preheater and then flow into the first stirring reactor to be stirred and reacted at 65 ℃ (the stirring speed is 70 rpm), and the residence time of the reaction liquid in the first stirring reactor is 0.4 h; the first-stage reaction product flows into a first standing tank and is layered into an upper grease layer and a lower layer of glycerin, the lower layer of glycerin is collected in a glycerin tank, the upper grease layer enters a second stirring reactor again to be stirred and reacted, the stirring reaction is carried out at 65 ℃ (the stirring speed is 70 rpm), and the residence time of the reaction liquid in the second stirring reactor is 0.6 h;
2) and introducing a second-stage reaction product flowing out from an outlet at the bottom of the second stirring reactor into a second standing tank for standing and layering, and returning a mixture of the glycerol and the incompletely reacted methanol precipitated at the bottom of the second standing tank into the first stirring reactor for continuous cyclic reaction. And (3) an upper layer outlet of the second standing tank flows out of an oil layer product which is not completely reacted, and the yield of the biodiesel product is about 93.5 percent by detecting the oil layer product.
3) And (3) allowing an oil layer product which is not completely reacted to flow out of an upper layer outlet of the second standing tank to flow into the tubular reactor, allowing a second part of methanol solution to flow into the tubular reactor at a flow rate of 1kg/h for continuous reaction, allowing the reaction temperature in the tubular reactor to be 65 ℃, allowing the reaction solution to stay in the tubular reactor for 15min, allowing the reaction solution to flow into a cooler for cooling to room temperature, and collecting the final biodiesel product in a product tank, wherein the yield of the obtained biodiesel is 98.2%.
Wherein the total mass of KOH dissolved in the two methanol solutions was 1.5% of the mass of soybean oil.
Example 3:
a method for continuously preparing biodiesel (the production device adopts the structure shown in figure 1) comprises the following processes:
1) the KOH catalyst is dissolved in methanol to form a methanol solution, and the prepared methanol solution is divided into two parts to be fed.
The first part of the methanol solution was fed to the preheater at a flow rate of 4kg/h, while the soybean oil was fed to the preheater at a flow rate of 10 kg/h; the reaction materials are heated to 65 ℃ by the preheater and then flow into the first stirring reactor to be stirred and reacted at 65 ℃ (the stirring speed is 70 rpm), and the residence time of the reaction liquid in the first stirring reactor is 0.5 h; the first-stage reaction product flows into a first standing tank and is layered into an upper grease layer and a lower layer of glycerin, the lower layer of glycerin is collected in a glycerin tank, the upper grease layer enters a second stirring reactor again to be stirred and reacted, the stirring reaction is carried out at 65 ℃ (the stirring speed is 70 rpm), and the residence time of the reaction liquid in the second stirring reactor is 0.5 h;
2) and introducing a second-stage reaction product flowing out from an outlet at the bottom of the second stirring reactor into a second standing tank for standing and layering, and returning a mixture of the glycerol and the incompletely reacted methanol precipitated at the bottom of the second standing tank into the first stirring reactor for continuous cyclic reaction. And (3) an upper layer outlet of the second standing tank flows out of an oil layer product which is not completely reacted, and the yield of the biodiesel product is about 90 percent by detecting the oil layer product.
3) And (3) allowing an oil layer product which is not completely reacted to flow out of an upper layer outlet of the second standing tank to flow into the tubular reactor, allowing a second part of methanol solution to flow into the tubular reactor at a flow rate of 4kg/h for continuous reaction, allowing the reaction temperature in the tubular reactor to be 65 ℃, allowing the reaction solution to stay in the tubular reactor for 15min, allowing the reaction solution to flow into a cooler for cooling to room temperature, and collecting the final biodiesel product in a product tank, wherein the yield of the obtained biodiesel is 97.2%.
Wherein the total mass of KOH dissolved in the two methanol solutions was 0.8% of the mass of soybean oil.
Example 4:
5g of KOH catalyst is dissolved in 400g of methanol to form methanol solution, then the methanol solution reacts with 500g of soybean oil in a reactor at 65 ℃ for 2h (the reaction stirring speed is 100 rpm), detection and analysis are carried out after the reaction is finished, and the yield of the biodiesel in the product is 97.3%.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.
Claims (2)
1. A device for continuously preparing biodiesel is characterized by comprising a preheater (9), a methanol tank (1), a methanol delivery pump (3), two stirring reactors, two standing tanks, a reactant delivery pump (20) and a tubular reactor, wherein reaction liquid is preheated by the preheater (9) and then introduced into a first stirring reactor (10) for reaction, and an outlet at the bottom of the first stirring reactor (10) is connected with a feed inlet in the middle of the first standing tank (11) through a pipeline; the first standing tank (11) plays a role in layering, an outlet at the bottom of the first standing tank (11) is connected with the glycerin tank (19) through a first glycerin pump (12) by a pipeline, and an outlet at the upper layer of the first standing tank (11) is connected with an inlet of the second stirring reactor (13) by a pipeline;
an outlet at the bottom of the second stirring reactor (13) is connected with a feed inlet in the middle of the second standing tank (14) through a pipeline, the second standing tank (14) plays a layering role, and a mixture discharged from the outlet at the bottom of the second standing tank (14) can be reused in the first stirring reactor (10);
an outlet at the bottom of the methanol tank (1) is connected with an inlet of a methanol delivery pump (3) through a pipeline, an outlet of the methanol delivery pump (3) is divided into two paths, one path is connected with an inlet of a preheater (9) through a pipeline, the other path is connected with one path of inlet of a reactant delivery pump (20) through a pipeline, and the other path of inlet of the reactant delivery pump (20) is connected with an upper layer outlet of a second standing tank (14); the outlet of the reactant delivery pump (20) is connected with the inlet of the tubular reactor (16) through a pipeline, and the outlet of the tubular reactor (16) is connected with the product tank (18) through a cooler (17) through a pipeline.
2. The apparatus for continuously preparing biodiesel according to claim 1, further comprising a grease storage tank (2), a grease transfer pump (4) and a second glycerin pump (15); an outlet at the bottom of the grease storage tank (2) is connected with an inlet of the preheater (9) through a grease delivery pump (4) by a pipeline, and an outlet at the bottom of the second standing tank (14) is connected with an inlet of the preheater (9) through a second glycerin pump (15) by a pipeline; flow meters (6) and regulating valves (5) are arranged on the corresponding pipelines.
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