Glycerol esterified oil thorough transesterification equipment

Abstract

The invention discloses glycerol esterified oil thorough ester exchange equipment which comprises a raw material storage unit, a reaction unit and a product storage unit, and the raw material storage unit comprises a glycerol esterified oil storage tank, an alcohol-containing crude glycerol storage tank and a methanol alkali solution storage tank; the reaction unit comprises at least three reaction towers which are connected in sequence; the glycerol esterified oil storage tank and the alcohol-containing crude glycerol storage tank are connected with a feed port of the first reaction tower, and the methanol alkali solution storage tank is connected with feed ports of all the reaction towers; the product storage unit comprises a crude methyl ester storage tank and a crude glycerol storage tank, the heavy phase outlet of the first reaction tower is connected with the crude glycerol storage tank, and the light phase outlet of the last reaction tower is connected with the crude methyl ester storage tank. Compared with the prior art, the complete ester exchange equipment provided by the invention has the advantages that potassium hydroxide in alcohol-containing crude glycerine is utilized to perform alkali refining and deacidification on glyceryl esterified oil, the purpose of partial ester exchange is achieved, and the content and the yield of fatty acid methyl ester in biodiesel are greatly improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of ester exchange, in particular to a glyceride oil esterification complete ester exchange equipment. BACKGROUND

[0002] Due to the increasing depletion of petrochemical fuel resources and the urgent need for environmental protection, the development of clean energy has attracted more and more attention. Energy researchers around the world are actively exploring the development of alternative fuels and renewable energy. Among them, biodiesel is one of the core research directions.

[0003] At present, the key factor restricting the development of biodiesel is the price of raw materials, and finding a cheap raw material and converting it is the key research direction. Waste oil meets the needs of biodiesel production due to its low cost and wide source. Preparing biodiesel from waste oil not only solves the impact of waste oil on food safety and environmental protection, but also solves the problem of high cost of biodiesel raw materials. However, the traditional waste oil biodiesel ester exchange has the problems of large amount of catalyst and alcohol, large oil loss, and incomplete ester exchange reaction.

[0004] Therefore, it is urgent to provide a new biodiesel production method to solve the above problems. SUMMARY

[0005] The purpose of the present application is to overcome the above technical deficiencies, and to provide a glyceride oil esterification complete ester exchange equipment to solve the technical problem of incomplete ester exchange of traditional waste oil biodiesel in the prior art.

[0006] To achieve the above technical purpose, the following technical scheme is adopted in the present application: The present application provides a glyceride oil esterification complete ester exchange equipment, which comprises a raw material storage unit, a reaction unit and a product storage unit, The raw material storage unit comprises a glyceride oil storage tank, an alcohol-containing crude glycerol storage tank and a methanol alkali solution storage tank; The reaction unit comprises at least three reaction towers connected in series, each reaction tower has a heavy phase outlet, a feed inlet and a light phase outlet arranged from bottom to top, and in adjacent two reaction towers, the light phase outlet of the former reaction tower is connected to the feed inlet of the latter reaction tower, and the heavy phase outlet of the latter reaction tower is connected to the feed inlet of the former reaction tower; the glyceride oil storage tank and the alcohol-containing crude glycerol storage tank are connected to the feed inlet of the first reaction tower, and the methanol alkali solution storage tank is connected to the feed inlet of each reaction tower; The product storage unit comprises a crude methyl ester storage tank and a crude glycerol storage tank, the heavy phase outlet of the first reaction tower is connected to the crude glycerol storage tank, and the light phase outlet of the last reaction tower is connected to the crude methyl ester storage tank.

[0007] In some embodiments, the reaction column comprises a column body having the heavy phase outlet, the feed inlet and the light phase outlet, a grid plate and a first circulation device, the first circulation device comprises a first distributor, the grid plate and the first distributor are both arranged in the column body, and the column body is divided into a heavy phase settling separation zone, a loop reaction zone and a light phase settling separation zone arranged in sequence from bottom to top, the heavy phase outlet communicates with the heavy phase settling separation zone, the feed inlet communicates with the loop reaction zone, and the light phase outlet communicates with the light phase settling separation zone.

[0008] In some embodiments, the first circulation device further comprises a first circulation pipe and a first circulation pump, the upper end of the first circulation pipe is located below the light phase outlet and communicates with the light phase settling separation zone, the lower end of the first circulation pipe is connected to the first distributor, the first circulation pump is arranged on the first circulation pipe to drive the material to flow from the upper end of the first circulation pipe to the first distributor, and the first distributor is arranged downward.

[0009] In some embodiments, the reaction column further comprises a second circulation device, the second circulation device comprises a second circulation pipe, a second circulation pump and a second distributor, the upper end of the second circulation pipe communicates with the loop reaction zone, the lower end of the second circulation pipe extends from the feed inlet to the loop reaction zone and is connected to the second distributor, the second distributor is arranged in the loop reaction zone and the outlet end of the second distributor is arranged upward, and the second circulation pump is arranged on the second circulation pipe to drive the material to flow from the upper end of the second circulation pipe to the second distributor.

[0010] In some embodiments, the reaction column further comprises a heating device, the heating device comprises a heater, a temperature sensor and a controller, the heater is arranged in the loop reaction zone and located between the upper end of the second circulation pipe and the second distributor, the temperature sensor is arranged in the light phase settling separation zone, and the temperature sensor is connected to the heater through the controller.

[0011] In some embodiments, the first reaction column has a first feed inlet and a second feed inlet, the first feed inlet communicates with the heavy phase settling separation zone, and the second feed inlet communicates with the loop reaction zone; the glyceride oil storage tank and the crude glycerol storage tank containing alcohol are connected to the first feed inlet, and the methanol alkali solution storage tank and the heavy phase outlet of the subsequent reaction column are connected to the second feed inlet.

[0012] In some embodiments, the raw material storage unit further comprises a methanol storage tank, the methanol storage tank is connected to the feed inlet of the remaining reaction columns except the first and last reaction columns.

[0013] In some embodiments, the raw material storage unit further comprises a constant temperature heat exchanger arranged on a pipeline connecting the glyceride oil storage tank and the alcohol-containing crude glycerol storage tank with the reaction tower.

[0014] In some embodiments, a tail gas treatment unit is further included, which is in communication with the top of the alcohol-containing crude glycerol storage tank, the methanol alkali solution storage tank, each of the reaction towers, the crude methyl ester storage tank and the crude glycerol storage tank, respectively.

[0015] In some embodiments, the tail gas treatment unit comprises a main pipe, a plurality of branch pipes and a condensing device, the main pipe is connected with the alcohol-containing crude glycerol storage tank, the methanol alkali solution storage tank, each of the reaction towers, the crude methyl ester storage tank and the crude glycerol storage tank via each of the branch pipes, and the condensing device is arranged on the main pipe.

[0016] Compared with the prior art, the glyceride oil complete transesterification equipment provided by the present application uses potassium hydroxide in alcohol-containing crude glycerol to perform alkali refining deacidification on glyceride oil and achieve the purpose of partial transesterification, which reduces the amount of alkali catalyst used in the subsequent transesterification reaction process and also reduces the solubilization and dispersion of glycerol in the system, thereby realizing effective separation of glycerol and fatty acid methyl ester and greatly improving the content and yield of fatty acid methyl ester in biodiesel. BRIEF DESCRIPTION OF DRAWINGS

[0017] Figure 1 is a structural schematic diagram of the glyceride oil complete transesterification equipment provided by the embodiment of the present application; Figure 2 is a structural schematic diagram of the reaction tower in Figure 1 Figure 3 is a structural schematic diagram of the first reaction tower in Figure 1 DETAILED DESCRIPTION

[0018] In order to make the purpose, technical solutions and advantages of the present application clearer, the present application is further described in detail below in combination with the drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present application and do not limit the present application.

[0019] In order to solve the technical problem of incomplete transesterification of traditional waste oil biodiesel, the present application provides a glyceride oil complete transesterification equipment, which can realize complete transesterification and greatly improve the content and yield of fatty acid methyl ester in biodiesel.

[0020] Please refer to Figure 1 , Figure 1 ​​Figure 1 is a structural schematic diagram of a complete transesterification device for glyceride oil in an embodiment of the present application. The complete transesterification device for glyceride oil comprises a raw material storage unit 1, a reaction unit 2, and a product storage unit 3. Figure 1 The arrows indicate the flow direction of the liquid or gas.

[0021] The raw material storage unit 1 comprises a glyceride oil storage tank 11, an alcohol-containing crude glycerol storage tank 12, and a methanol alkali solution storage tank 13. The glyceride oil storage tank 11 stores glyceride oil produced using waste oil and fat. The alcohol-containing crude glycerol storage tank 12 stores crude glycerol containing methanol and alkali, typically potassium hydroxide and other impurities. The methanol alkali solution storage tank 13 stores a potassium hydroxide solution of methanol, which is used as a catalyst and a methanol supplement.

[0022] The reaction unit comprises at least three reaction towers 2 connected in sequence, as shown in Figure 2. Figure 2 Each reaction tower 2 has a heavy phase outlet 201, a feed inlet 202, and a light phase outlet 203 arranged in sequence from bottom to top. In adjacent two reaction towers 2, the light phase outlet 203 of the former reaction tower 2 is connected to the feed inlet 202 of the latter reaction tower 2, and the heavy phase outlet 201 of the latter reaction tower 2 is connected to the feed inlet 202 of the former reaction tower 2.

[0023] In this embodiment, there are three reaction towers 2, which are arranged in sequence as a first reaction tower 2A, a second reaction tower 2B, and a third reaction tower 2C for ease of description. The first reaction tower 2A is the first reaction tower, the third reaction tower 2C is the last reaction tower, and the second reaction tower 2B is the middle reaction tower. Therefore, the connection relationship between them is that the light phase outlet 203 of the first reaction tower 2A is connected to the feed inlet 202 of the second reaction tower 2B, the heavy phase outlet 201 of the second reaction tower 2B is connected to the feed inlet 202 of the first reaction tower 2A; the light phase outlet 203 of the second reaction tower 2B is connected to the feed inlet 202 of the third reaction tower 2C, and the heavy phase outlet 201 of the third reaction tower 2C is connected to the feed inlet 202 of the second reaction tower 2B.

[0024] It is easy to understand that in other embodiments, more than three reaction towers 2 can also be provided, such as four, five, or six, etc. The arrangement is a first reaction tower 2A, a plurality of second reaction towers 2B, and a third reaction tower 2C connected in sequence, and the connection mode is the same as described above, which will not be described again.

[0025] The glyceride oil storage tank 11 and the alcohol-containing crude glycerol storage tank 12 are connected to the feed inlet 202 of the first reaction tower, i.e., the first reaction tower 2A, and the methanol alkali solution storage tank 13 is connected to the feed inlet 202 of each reaction tower 2. Methanol can play a role in demulsification, promoting the separation of oil and fat and alcohol-containing glycerol soap.

[0026] The product storage unit 3 comprises a crude methyl ester storage tank 31 and a crude glycerol storage tank 32, the crude glycerol storage tank 32 is connected to the heavy phase outlet 201 of the first reaction column, i.e. the first reaction column 2A, and the crude methyl ester storage tank 31 is connected to the light phase outlet 203 of the last reaction column, i.e. the third reaction column 2C.

[0027] In some embodiments, the raw material storage unit 1 further comprises a methanol storage tank 14, which stores high-purity methanol for supplementing the reaction. The methanol storage tank 14 is connected to each of the reaction columns 2 except the first and last reaction columns 2, i.e. the feed inlet 202 of each second reaction column 2B.

[0028] In some embodiments, the raw material storage unit 1 further comprises a constant-temperature heat exchanger 15, which is arranged on the pipeline connecting the glycerol esterification oil storage tank 11 and the crude glycerol containing alcohol storage tank 12 to the first reaction column 2A. The constant-temperature heat exchanger 15 is used to heat the glycerol esterification oil and the crude glycerol containing alcohol to a preset temperature.

[0029] Please refer again to Figure 2 , Figure 2 is Figure 1 the structural diagram of the reaction column 2. In some embodiments, the first reaction column 2A, the second reaction column 2B and the third reaction column 2C are all in the form of the reaction column 2.

[0030] The reaction column 2 comprises a column body 21, a grid plate 22 and a first circulating device 23. The column body 21 has a heavy phase outlet 201, a feed inlet 202 and a light phase outlet 203. The first circulating device 23 comprises a first distributor 231. The grid plate 22 and the first distributor 231 are both arranged in the column body 21, and divide the column body 21 into a heavy phase sedimentation separation zone 204, a loop reaction zone 205 and a light phase sedimentation separation zone 206 arranged in sequence from bottom to top. The heavy phase outlet 201 is connected to the heavy phase sedimentation separation zone 204, the feed inlet 202 is connected to the loop reaction zone 205, and the light phase outlet 203 is connected to the light phase sedimentation separation zone 206. The grid plate 22 is a porous structure, and the material can pass through the grid plate 22, but the grid plate 22 can slow down the speed of the material passing through.

[0031] Further, the first circulating device 23 further comprises a first circulating pipe 232 and a first circulating pump 233. The upper end of the first circulating pipe 232 is located below the light phase outlet 203 and is connected to the light phase sedimentation separation zone 206, and the lower end of the first circulating pipe 232 is connected to the first distributor 231. The first circulating pump 233 is arranged on the first circulating pipe 232 to drive the material to flow from the upper end of the first circulating pipe 232 to the first distributor 231. The first distributor 231 is arranged downwardly to send the material into the loop reaction zone 205.

[0032] In the preferred embodiment, the reaction column 2 further comprises a second circulating device 24, which is similar to the first circulating device 23 and comprises a second distributor 241, a second circulating pipe 242 and a second circulating pump 243. The upper end of the second circulating pipe 242 is connected to the loop reaction zone 205, and the lower end of the second circulating pipe 242 extends from the feed inlet 202 to the loop reaction zone 205 and is connected to the second distributor 241. The second distributor 241 is arranged in the loop reaction zone 205 and has its discharge end upwardly arranged. The second circulating pump 243 is arranged on the second circulating pipe 242 to drive the material to flow from the upper end of the second circulating pipe 242 to the second distributor 241, and the second distributor 241 sends the material into the loop reaction zone 205.

[0033] The material enters the loop reaction zone 205 through the feed inlet 202, and in some embodiments, the material can also be fed through the second circulating device 24. The material in the loop reaction zone 205 performs the ester exchange reaction, and the light phase product moves upwardly, a part of which is transported again to the bottom of the loop reaction zone 205 by the second circulating device 24 to perform the reaction again, thereby improving the conversion rate of the material. Another part of the light phase product enters the light phase settling separation zone 206 to perform the settling separation, and the light phase product continues to move upwardly, a part of which is transported again to the loop reaction zone 205 by the first circulating device 23 to perform the reaction, and another part is discharged through the overflow of the light phase outlet 203. The heavy phase product generated by the ester exchange reaction in the loop reaction zone 205 moves downwardly and falls into the heavy phase settling separation zone 204 after passing through the grid plate 22, and after the settling separation in the heavy phase settling separation zone 204, the heavy phase product is discharged through the heavy phase outlet 201. The light material in the upper layer of the heavy phase settling separation zone 204 can also be transported back to the loop reaction zone 205 again by the second circulating device 24.

[0034] In some embodiments, the reaction column 2 further comprises a heating device 25, which comprises a heater 251, a temperature sensor 252 and a controller 253. The heater 251 is arranged in the loop reaction zone 205 and located between the upper end of the second circulating pipe 242 and the second distributor 241. The temperature sensor 252 is arranged in the light phase settling separation zone 206, and the temperature sensor 252 is connected to the heater 251 through the controller 253. The heater 251 can adopt the forms of electric heating, steam heating, etc. to maintain the reaction temperature in the loop reaction zone 205. The temperature sensor 252 indirectly infers the temperature in the loop reaction zone 205 by detecting the temperature in the light phase settling separation zone 206, so as to feedback adjust the heating power of the heater 251 through the controller 253, so that the reaction temperature is maintained in the appropriate range.

[0035] Please refer to Figure 3In some embodiments, the first reaction tower 2A is different from the other reaction towers 2 in structure, and the difference is that the first reaction tower 2A has two feed inlets, i.e. a first feed inlet 202a and a second feed inlet 202b. The first feed inlet 202a is connected to the heavy phase settling separation zone 204, and the second feed inlet 202b is connected to the loop reaction zone 205. The glyceride oil storage tank 11 and the crude glycerol storage tank 12 containing alcohol are connected to the first feed inlet 202a, and the methanol alkali solution storage tank 13 and the heavy phase outlet 201 of the subsequent reaction tower 2, i.e. the second reaction tower 2B, are connected to the second feed inlet 202b.

[0036] In other words, in this embodiment, the raw materials provided by the glyceride oil storage tank 11 and the crude glycerol storage tank 12 containing alcohol are first fed into the heavy phase settling separation zone 204 of the first reaction tower 2A, and after the transesterification reaction and settling separation in the heavy phase settling separation zone 204, the heavy phase is fed from the heavy phase outlet into the crude glycerol storage tank 32, and the light phase is fed into the loop reaction zone 205 through the second circulating device. The subsequent material flow is the same as that of the other reaction towers 2, and thus will not be described again.

[0037] In some embodiments, since various materials have volatility, the complete glyceride oil transesterification equipment also includes a tail gas treatment unit 4 connected to the top of the crude glycerol storage tank 12 containing alcohol, the methanol alkali solution storage tank 13, the methanol storage tank 14, each reaction tower 2, the crude methyl ester storage tank 31, and the crude glycerol storage tank 32, respectively, for treating the volatile gases generated by them.

[0038] In a preferred embodiment, the tail gas treatment unit 4 includes a main pipe 41, a plurality of branch pipes 42, and a condensing device 43. The main pipe 41 is connected to the crude glycerol storage tank 12 containing alcohol, the methanol alkali solution storage tank 13, the methanol storage tank 14, each reaction tower 2, the crude methyl ester storage tank 31, and the crude glycerol storage tank 32 through the branch pipes 42, respectively. The condensing device 43 is arranged on the main pipe 41, and is used to condense various volatile gases back to liquids, which are collected and then fed back into the equipment for reaction.

[0039] It is easy to understand that one or more valves can be arranged on various pipelines of the equipment according to actual needs, so as to control the flow of liquids or gases.

[0040] For better understanding of the present application, the technical solutions of the present application are described in detail: the glyceride oil in the glyceride oil storage tank 11 and the alcohol-containing crude glycerol in the alcohol-containing crude glycerol storage tank 12 are mixed and then transported into the first reaction tower 2A, and the methanol alkali solution in the methanol alkali solution storage tank 13 is added as a catalyst. Then, the reaction and sedimentation separation are carried out in the first reaction tower 2A, to obtain the first oil and the first alcohol-containing glycerol soap, and the first oil is transported into the second reaction tower 2B, and after adding the methanol alkali solution and the methanol in the methanol storage tank 14, the transesterification reaction is carried out again. The first alcohol-containing glycerol soap is transported into the crude glycerol storage tank 32 for storage. The second oil and the second alcohol-containing glycerol soap are generated in the second reaction tower 2B, the second oil is transported into the third reaction tower 2C, and after adding the methanol alkali solution and the methanol in the methanol storage tank 14, the transesterification reaction is carried out again. The second alcohol-containing glycerol soap is transported into the first reaction tower 2A. The third oil and the third alcohol-containing glycerol soap are generated in the third reaction tower 2C, the third oil is transported into the crude methyl ester storage tank 31 for storage, and the third alcohol-containing glycerol soap is transported into the second reaction tower 2B.

[0041] The specific embodiments of the present application described above do not constitute a limitation on the protection scope of the present application. Any various other corresponding changes and modifications made according to the technical concept of the present application shall be included in the protection scope of the claims of the present application.

Claims

1. A device for complete transesterification of glycerol esterified oil, characterized in that, include: The raw material storage unit includes a glycerol esterified oil storage tank, an alcohol-containing crude glycerol storage tank, and a methanol alkaline solution storage tank. The reaction unit includes at least three reaction towers connected in sequence. Each reaction tower has a heavy phase outlet, a feed inlet, and a light phase outlet arranged from bottom to top. In two adjacent reaction towers, the light phase outlet of the preceding reaction tower is connected to the feed inlet of the following reaction tower, and the heavy phase outlet of the following reaction tower is connected to the feed inlet of the preceding reaction tower. The glycerol esterification oil storage tank and the alcohol-containing crude glycerol storage tank are connected to the feed inlet of the first reaction tower, and the methanol alkaline solution storage tank is connected to the feed inlets of each reaction tower. The product storage unit includes a crude methyl ester storage tank and a crude glycerol storage tank. The heavy phase outlet of the first reaction tower is connected to the crude glycerol storage tank, and the light phase outlet of the last reaction tower is connected to the crude methyl ester storage tank.

2. The glycerol esterification oil complete transesterification device according to claim 1, characterized in that, The reaction tower includes a tower body, a grid plate, and a first circulation device. The tower body has a heavy phase outlet, a feed inlet, and a light phase outlet. The first circulation device includes a first distributor. The grid plate and the first distributor are both disposed in the tower body. The tower body is divided into a heavy phase sedimentation separation zone, a loop reaction zone, and a light phase sedimentation separation zone arranged sequentially from bottom to top. The heavy phase outlet is connected to the heavy phase sedimentation separation zone, the feed inlet is connected to the loop reaction zone, and the light phase outlet is connected to the light phase sedimentation separation zone.

3. The glycerol esterification oil complete transesterification device according to claim 2, characterized in that, The first circulation device further includes a first circulation pipe and a first circulation pump. The upper end of the first circulation pipe is located below the light phase outlet and communicates with the light phase sedimentation separation zone. Its lower end is connected to the first distributor. The first circulation pump is disposed on the first circulation pipe to drive the material to flow from the upper end of the first circulation pipe to the first distributor. The first distributor is arranged downwards.

4. The glycerol esterification oil complete transesterification device according to claim 2, characterized in that, The reaction tower also includes a second circulation device, which includes a second circulation pipe, a second circulation pump, and a second distributor. The upper end of the second circulation pipe is connected to the loop reaction zone, and its lower end extends from the feed inlet into the loop reaction zone and is connected to the second distributor. The second distributor is disposed in the loop reaction zone with its discharge end facing upward. The second circulation pump is disposed on the second circulation pipe to drive the material to flow from the upper end of the second circulation pipe to the second distributor.

5. The glycerol esterification oil complete transesterification device according to claim 2, characterized in that, The reaction tower also includes a heating device, which includes a heater, a temperature sensor, and a controller. The heater is located in the loop reaction zone and between the upper end of the second circulation pipe and the second distributor. The temperature sensor is located in the light phase sedimentation separation zone and is connected to the heater through the controller.

6. The glycerol esterification oil complete transesterification device according to claim 2, characterized in that, The first reaction tower has a first inlet and a second inlet, the first inlet being connected to the heavy phase sedimentation separation zone, and the second inlet being connected to the loop reaction zone; the glycerol esterification oil storage tank and the alcohol-containing crude glycerol storage tank are connected to the first inlet, and the methanol alkaline solution storage tank and the heavy phase outlet of the subsequent reaction tower are connected to the second inlet.

7. The glycerol esterification oil complete transesterification device according to claim 1, characterized in that, The raw material storage unit also includes a methanol storage tank, which is connected to the feed inlets of the remaining reaction towers excluding the first and last reaction towers.

8. The glycerol esterification oil complete transesterification device according to claim 1, characterized in that, The raw material storage unit also includes a constant temperature heat exchanger, which is arranged on the pipeline connecting the glycerol esterified oil storage tank and the alcohol-containing crude glycerol storage tank to the reaction tower.

9. The glycerol esterification oil complete transesterification device according to claim 1, characterized in that, It also includes an exhaust gas treatment unit, which is connected to the top of the alcohol-containing crude glycerol storage tank, the methanol alkaline solution storage tank, each of the reaction towers, the crude methyl ester storage tank, and the crude glycerol storage tank.

10. The glycerol esterification oil complete transesterification device according to claim 9, characterized in that, The exhaust gas treatment unit includes a main pipe, multiple branch pipes, and a condenser. The main pipe is connected to the alcohol-containing crude glycerol storage tank, the methanol alkaline solution storage tank, each of the reaction towers, the crude methyl ester storage tank, and the crude glycerol storage tank via the branch pipes. The condenser is installed on the main pipe.

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