A glyceride oil production system and a production method
Patent Information
- Application Number
- CN202610858337.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-06-15
- Publication Date
- 2026-09-29
AI Technical Summary
但微通道反应器极易堵塞,同时清理也非常困难
1、本发明提供的甘油二酯油生产系统能够充分提高甘油二酯油产品中的甘油二酯含量,可以根据甘油二酯含量生产多规格产品;而且各工段的副产物均可外售,无废水、废渣排放,更加经济、环保,适宜工业化生产。第九输出泵设置有三个出料口,可根据产品中甘油二酯的含量选择不同的处理路径,从而提高甘油二酯油的产量,生产多规格产品。
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Figure CN122828649A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to a diglyceride oil production system and method, belonging to the field of new resource food processing technology. Background Technology
[0002] Diglyceride oil is a new resource food in China, and it is defined as having a diglyceride content of over 40%. The production process of diglyceride oil uses soybean oil, rapeseed oil, peanut oil, corn oil, etc., as raw materials, and lipase preparations, water, glycerol, etc., as main auxiliary materials. It is produced through processes such as lipase catalysis and distillation separation.
[0003] Researchers have used soybean oil and glycerol as raw materials and liquid lipase as a catalyst to prepare diglyceride oil using a microchannel reactor. However, microchannel reactors are extremely prone to clogging, and cleaning them is also very difficult. Currently, the clogging problem of microreactors has become the biggest obstacle to their replacement of batch reactors.
[0004] In the production process of diglyceride oil, some people choose molecular sieves for the dehydration operation in the reaction process. However, molecular sieves have fatal drawbacks in this process: First, as the dehydration process proceeds, the adsorption capacity of the molecular sieve will gradually decrease, and high-temperature regeneration is required after a period of adsorption; Second, the crushing strength of molecular sieves is generally low, which greatly limits their application in this process.
[0005] Chinese patent document CN115975767A discloses a high-efficiency continuous production system and method for diglyceride oil. It utilizes a microchannel reactor to first emulsify edible oil and lipase to form an emulsion oil. Two micro-mixing operations are then performed to improve the mass transfer efficiency between the two phases of the reactants, promoting the transesterification reactions of triglycerides with glycerol, monoglycerides, and triglycerides, thereby increasing the yield of diglycerides (DAG). However, this structure suffers from the problem of easy clogging of the microchannel reactor, and cleaning is difficult.
[0006] Chinese patent document CN117736867A discloses a production system and method for structural oils based on liquid lipase catalysis. It achieves efficient production of structural oils by using a Venturi injector combined with a loop reaction system. However, this production system cannot handle the by-products generated in each process.
[0007] Moreover, the diglyceride oil production system in the above technology cannot be adjusted according to the content of diglyceride oil in the product, resulting in low production efficiency of diglyceride oil.
[0008] Therefore, there is an urgent need for a diglyceride oil production system and method that can both increase the yield of diglyceride oil and process the by-products of each stage of the process. Summary of the Invention
[0009] To address the aforementioned problems, this invention provides a diglyceride oil production system and method that can significantly increase the diglyceride content in the diglyceride oil product. It can also produce products of various specifications based on the diglyceride content. Furthermore, byproducts from each stage of the production process can be sold externally, with no wastewater or waste residue discharged.
[0010] To achieve the above objectives, the technical solution adopted by the present invention is as follows: In a first aspect, the present invention provides a diglyceride oil production system, comprising: First reaction unit; The dehydration unit is connected to the first reaction unit; The second reaction unit is connected to the dehydration unit and can also be connected to the first reaction unit; The first separation unit is connected to the second reaction unit; The adsorption unit is connected to the first separation unit via a crude product tank; The deodorization unit is connected to the adsorption unit via a crude product tank, and the deodorization unit is connected to a finished product tank on the side opposite to the adsorption unit. When the diglyceride content in the produced product is low, the material after the reaction in the second reaction unit directly enters the first separation unit. When the diglyceride content in the produced product is moderate, the material after the reaction in the second reaction unit enters the dehydration unit and the second reaction unit again for reaction, and the material enters the first separation unit after the second reaction. When the product has a high content of diglycerides, the material after being reacted in the second reaction unit re-enters the first reaction unit, the dehydration unit, and the second reaction unit. After being reacted again, the material enters the first separation unit.
[0011] In one embodiment of the present invention, the first reaction unit includes a first delivery pump, a first heat exchanger, a first stirring tank, a second delivery pump, a first enzyme reactor, and a transfer tank connected in sequence. A first feeding tank is connected to one side of the first stirring tank, and the outlet of the transfer tank is connected to the dehydration unit.
[0012] In one embodiment of the present invention, the dehydration unit includes a fourth delivery pump, a second heat exchanger, a first thin-film evaporator, a first receiving tank, a fifth delivery pump, a third heat exchanger, a second stirring tank, and a seventh delivery pump connected in sequence. The seventh delivery pump is connected to the second reaction unit, and the fourth delivery pump is connected to the transfer tank. The dehydration unit further includes a first condenser, a second receiving tank, a sixth delivery pump, and a first vacuum unit. The vacuum interface of the first thin-film evaporator is connected to the upper vacuum interface of the first condenser; the lower vacuum interface of the first condenser is connected to the first vacuum unit; the first condenser is connected to the second receiving tank; and the second receiving tank is connected to the sixth delivery pump.
[0013] In one embodiment of the present invention, the second reaction unit includes a second enzyme reactor, a third stirring tank and a ninth delivery pump connected in sequence. The second enzyme reactor is connected to the seventh delivery pump. The ninth delivery pump includes a first outlet, a second outlet and a third outlet. The first outlet is connected to the inlet of the transfer tank, the second outlet is connected to the inlet of the first enzyme reactor, and the third outlet is connected to the first separation unit. It also includes an eighth delivery pump, the two ends of which are connected to the second enzyme reactor and the transfer tank, respectively.
[0014] In one embodiment of the present invention, the first separation unit includes a semi-finished product tank, a tenth transfer pump, a second thin-film evaporator, a third receiving tank, an eleventh transfer pump, a first distillation apparatus, a fifth receiving tank, a thirteenth transfer pump, a second distillation apparatus, a seventh receiving tank, and a fifteenth transfer pump connected in sequence. The inlet of the semi-finished product tank is connected to the third outlet, and the fifteenth transfer pump is connected to the by-product tank. The second thin film evaporator is connected in sequence to a second condenser and a second vacuum unit on one side, and its outlet is connected in sequence to a fourth receiving tank and a twelfth delivery pump. The outlet of the first distillation unit is connected to a sixth receiving tank and a fourteenth delivery pump, and the outlet of the second distillation unit is connected to an eighth receiving tank and a sixteenth delivery pump, wherein the sixteenth delivery pump is connected to the crude product tank.
[0015] In one embodiment of the present invention, the adsorption unit includes a 22nd delivery pump, a 4th heat exchanger, a 4th stirring tank, a 23rd delivery pump, a filter, a 24th delivery pump, and a 5th heat exchanger connected in sequence. A 2nd feeding tank is connected to one side of the 4th stirring tank. The 22nd delivery pump is connected to the 1st crude product tank of the crude product tank. The outlet of the 5th heat exchanger is connected to the crude finished product tank.
[0016] In one embodiment of the present invention, the deodorization unit includes a 25th delivery pump, a 6th heat exchanger, a 7th heat exchanger, a deodorization tower, a 26th delivery pump, an 8th heat exchanger, a 9th heat exchanger, a collector, a vacuum pump, and a collection tank. The inlet of the 25th delivery pump is connected to the outlet of the 2nd crude product tank; the inlet of the 25th delivery pump is connected to the first inlet of the 6th heat exchanger; the fourth outlet of the 6th heat exchanger is connected to the inlet of the 7th heat exchanger; the 7th heat exchanger is connected to the deodorization tower; and the outlet of the deodorization tower is connected to the... The feed inlet of the 26th delivery pump is connected to the feed outlet of the 26th delivery pump; the discharge outlet of the 26th delivery pump is connected to the second feed inlet of the 6th heat exchanger; the fifth discharge outlet of the 6th heat exchanger is connected to the feed inlet of the 8th heat exchanger; the discharge outlet of the 8th heat exchanger is connected to the feed inlet of the 9th heat exchanger; the discharge outlet of the 9th heat exchanger is connected to the feed inlet of the 3rd finished product tank; the vacuum interface of the deodorization tower is connected to the upper vacuum interface of the trap; the top vacuum interface of the trap is connected to the vacuum pump; the discharge outlet of the trap is connected to the feed inlet of the collection tank.
[0017] In one embodiment of the present invention, a second separation unit is further included. The second separation unit includes a seventeenth delivery pump, a third distillation apparatus, a ninth receiving tank, an eighteenth delivery pump, a fourth distillation apparatus, an eleventh receiving tank, and a twentieth delivery pump connected in sequence. The seventeenth delivery pump is connected to the first crude product tank of the crude product tank, and the twentieth delivery pump is connected to the fourth crude product tank of the crude product tank. The tenth receiving tank, the nineteenth transfer pump, and the second crude product tank are sequentially connected to one side of the third distillation unit. The fourth distillation apparatus is connected in sequence to the twelfth receiving tank, the twenty-first transfer pump, and the third crude product tank.
[0018] Secondly, the present invention provides a method for producing diglyceride oil, using the aforementioned diglyceride oil production system, the method comprising the following steps: S1. The material enters the first reaction unit and reacts through the first heat exchanger, the first stirred tank and the first enzyme reactor before entering the transfer tank. S2. The material enters the dehydration unit from the transfer tank, and flows into the second reaction unit after being heated by the second heat exchanger, evaporated by the first thin film evaporator, cooled by the third heat exchanger, and stirred by the second stirring tank. S3. After being dehydrated by the dehydration unit, the material enters the second reaction unit, and after being reacted and stirred in the second enzyme reactor and the third stirring tank, it enters the ninth delivery pump. When the diglyceride content in the produced product is low, the material after the reaction in the second reaction unit directly enters the first separation unit. When the diglyceride content in the produced product is moderate, the material after the reaction in the second reaction unit enters the dehydration unit and the second reaction unit again for reaction, and the material enters the first separation unit after the second reaction. When the product has a high content of diglycerides, the material after being reacted in the second reaction unit enters the first reaction unit, the dehydration unit and the second reaction unit again, and after being reacted again, it enters the first separation unit. S4. The material is fed into the semi-finished product tank through the ninth conveying pump, and after evaporation by the second thin film evaporator and distillation by the first and second distillers, it enters the by-product tank and the first crude product tank. When the diglyceride content in the crude product produced by the first separation unit cannot meet the production requirements, the second separation unit needs to be added to further purify the crude product in the first separation unit, thereby increasing the diglyceride oil content in the final product.
[0019] S5. The material in the first crude product tank enters the adsorption unit for adsorption treatment, and after adsorption treatment, it enters the first crude finished product tank. S6. The material in the first crude finished product tank enters the deodorization unit for deodorization treatment, and after deodorization treatment, it enters the first finished product tank to complete the production of diglyceride oil.
[0020] In one embodiment of the present invention, the first heat exchanger is heated to 50-70°C; the evaporation surface temperature of the first thin-film evaporator is 90-110°C; the second heat exchanger is heated to 80-90°C; the third heat exchanger is cooled to 50-70°C; the evaporation surface temperature of the second thin-film evaporator is 120-170°C; the evaporation surface temperature of the first distillation apparatus is 200-250°C; and the evaporation surface temperature of the second distillation apparatus is 290-295°C.
[0021] The beneficial effects of this invention are: The present invention provides a diglyceride oil production system and method, which have the following advantages: 1. The diglyceride oil production system provided by this invention can significantly increase the diglyceride content in the diglyceride oil product, and can produce products of various specifications according to the diglyceride content; moreover, the by-products of each process can be sold externally, with no wastewater or waste residue discharge, making it more economical and environmentally friendly, and suitable for industrial production. The ninth output pump is equipped with three discharge ports, which can select different processing paths according to the diglyceride content in the product, thereby increasing the yield of diglyceride oil and producing products of various specifications.
[0022] 2. The adsorption unit of this diglyceride oil production system utilizes a filter to perform the filtration operation; after heat exchange in the fourth heat exchanger, the material temperature is raised to 105-120℃; activated carbon is selected as the adsorption material, with a dosage of 3% of the raw oil weight; after passing through the adsorption unit, pigments and polar components (such as glycidyl esters) in the crude product can be removed to a large extent, further improving the product quality. The dehydration unit can promptly remove the water generated during the reaction, promoting the enzyme-catalyzed transesterification reaction towards the formation of diglycerides, thereby increasing the conversion rate of diglycerides. Attached Figure Description
[0023] To more clearly illustrate the technical solutions in the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0024] Figure 1 This is a schematic diagram of the structure of the first reaction unit provided by the present invention.
[0025] Figure 2 This is a schematic diagram of the dehydration unit provided by the present invention.
[0026] Figure 3 This is a schematic diagram of the structure of the second reaction unit provided by the present invention.
[0027] Figure 4 This is a schematic diagram of the structure of the first separation unit provided by the present invention.
[0028] Figure 5 This is a schematic diagram of the structure of the second separation unit provided by the present invention.
[0029] Figure 6 This is a schematic diagram of the adsorption unit provided by the present invention.
[0030] Figure 7 This is a schematic diagram of the deodorization unit provided by the present invention.
[0031] In the diagram: 1. First reaction unit; 101. First transfer pump; 102. First heat exchanger; 103. First stirred tank; 104. First feed tank; 105. Second transfer pump; 106. First enzyme reactor; 107. Transfer tank; 108. Third transfer pump; 2. Dehydration unit; 201. Fourth transfer pump; 202. Second heat exchanger; 203. First thin-film evaporator; 204. First receiving tank; 205. Fifth transfer pump; 206. Third heat exchanger; 207. Second stirring tank; 208. Seventh transfer pump; 209. First condenser; 210. Second receiving tank; 211. Sixth transfer pump; 212. First vacuum unit; 213. First cold trap; 214. First buffer tank; 3. Second reaction unit; 301. Second enzyme reactor; 302. Eighth transfer pump; 303. Third stirred tank; 304. Ninth transfer pump; 3041. First discharge port; 3042. Second discharge port; 3043. Third discharge port; 4. First Separation Unit; 401. Semi-finished Product Tank; 402. Tenth Transfer Pump; 403. Second Thin-Film Evaporator; 404. Third Receiving Tank; 405. Eleventh Transfer Pump; 406. First Distillation Unit; 407. Fifth Receiving Tank; 408. Thirteenth Transfer Pump; 409. Second Distillation Unit; 410. Seventh Receiving Tank; 411. Fifteenth Transfer Pump; 412. Second Condenser; 413. Second Vacuum Unit; 414. Fourth Receiving Tank; 415. Twelfth Transfer Pump; 416. Third Cold Trap; 417. Third Vacuum Unit; 418. Sixth Receiving Tank; 419. Fourteenth Transfer Pump; 420. Fourth Cold Trap; 421. Fourth Vacuum Unit; 422. Eighth Receiving Tank; 423. Sixteenth Transfer Pump; 424. Second Cold Trap; 425. Second Buffer Tank; 426. Third Buffer Tank; 427. Fourth Buffer Tank; 5. Crude product tank; 501. First crude product tank; 502. Second crude product tank; 503. Third crude product tank; 504. Fourth crude product tank; 6. Adsorption unit; 601. Twenty-second transfer pump; 602. Fourth heat exchanger; 603. Second feed tank; 604. Fourth mixing tank; 605. Twenty-third transfer pump; 606. Filter; 607. Twenty-fourth transfer pump; 608. Fifth heat exchanger; 7. Crude finished product tank; 701. First crude finished product tank; 702. Second crude finished product tank; 703. Third crude finished product tank; 704. Fourth crude finished product tank; 8. Deodorization Unit; 801. Twenty-fifth Transfer Pump; 802. Sixth Heat Exchanger; 8021. First Inlet; 8022. Fourth Outlet; 8023. Second Inlet; 8024. Fifth Outlet; 803. Seventh Heat Exchanger; 804. Deodorization Tower; 805. Twenty-sixth Transfer Pump; 806. Eighth Heat Exchanger; 807. Ninth Heat Exchanger; 808. Collector; 809. Vacuum Pump; 810. Collection Tank; 9. Finished product tank; 901. First finished product tank; 902. Second finished product tank; 903. Third finished product tank; 904. Fourth finished product tank; 10. Second Separation Unit; 1001. Seventeenth Transfer Pump; 1002. Third Distillation Unit; 1003. Ninth Receiving Tank; 1004. Eighteenth Transfer Pump; 1005. Fourth Distillation Unit; 1006. Eleventh Receiving Tank; 1007. Twentieth Transfer Pump; 1008. Fifth Cold Trap; 1009. Fifth Vacuum Unit; 1010. Tenth Receiving Tank; 1011. Nineteenth Transfer Pump; 1012. Sixth Cold Trap; 1013. Sixth Vacuum Unit; 1014. Twelfth Receiving Tank; 1015. Twenty-first Transfer Pump; 1016. Fifth Buffer Tank; 1017. Sixth Buffer Tank. Detailed Implementation
[0032] The technical solution of the present invention will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0033] In the description of this invention, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing the invention and for simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance. The terms "first position" and "second position" refer to two different positions.
[0034] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to fixed connections or detachable connections; mechanical connections or electrical connections; direct connections or indirect connections through an intermediate medium; and internal connections between two components. Those skilled in the art can understand the specific meaning of these terms in this invention based on the specific circumstances.
[0035] like Figures 1 to 7As shown, this invention provides a diglyceride oil production system. This device can significantly increase the diglyceride content in the diglyceride oil product and can produce products of various specifications based on the diglyceride content. Furthermore, byproducts from each stage of the production process can be sold externally, with no wastewater or waste residue discharge. The diglyceride oil production system includes a first reaction unit 1, a dehydration unit 2, a second reaction unit 3, a first separation unit 4, a crude product tank 5, an adsorption unit 6, a crude finished product tank 7, a deodorization unit 8, and a finished product tank 9. The first reaction unit 1 is connected to the dehydration unit 2, the dehydration unit 2 is connected to the second reaction unit 3, the first reaction unit 3 is connected to the first separation unit 4, and the crude product tank 5 is connected to the adsorption unit 6. The adsorption unit 6 is connected to the deodorization unit 8 through the crude finished product tank 7, and one end of the deodorization unit 8 is connected to the finished product tank 9. The connections between the units can be adjusted via pipelines and transfer pumps. The dehydration unit 2 can promptly remove water generated during the reaction process, promoting the enzyme-catalyzed transesterification reaction towards the formation of diglycerides, thereby increasing the conversion rate of diglycerides.
[0036] like Figure 1 As shown, in some embodiments, the first reaction unit 1 includes a first transfer pump 101, a first heat exchanger 102, a first stirred tank 103, a first feeding tank 104, a second transfer pump 105, a first enzyme reactor 106, and a transfer tank 107. The outlet of the first transfer pump 101 is connected to the inlet of the first heat exchanger 102, the outlet of the first heat exchanger 102 is connected to the inlet of the first stirred tank 103, and the outlet of the first feeding tank 104 is connected to the inlet of the first stirred tank 103. The outlet of the first stirred tank 103 is connected to the inlet of the second transfer pump 105, the outlet of the second transfer pump 105 is connected to the inlet of the first enzyme reactor 106, and the outlet of the first enzyme reactor 106 is connected to the inlet of the transfer tank 107. The first reaction unit 1 is also equipped with a third transfer pump 108. The inlet of the third transfer pump 108 is connected to the inlet of the first enzyme reactor 106, and the outlet of the third transfer pump 108 is connected to the inlet of the transfer tank 107.
[0037] like Figure 2As shown, in some embodiments, the dehydration unit 2 includes a fourth transfer pump 201, a second heat exchanger 202, a first thin-film evaporator 203, a first receiving tank 204, a fifth transfer pump 205, a third heat exchanger 206, a second stirring tank 207, a seventh transfer pump 208, a first condenser 209, a second receiving tank 210, a sixth transfer pump 211, and a first vacuum unit 212. The inlet of the fourth transfer pump 201 is connected to the outlet of the transfer tank 107; the outlet of the fourth transfer pump 201 is connected to the inlet of the second heat exchanger 202; the outlet of the second heat exchanger 202 is connected to the inlet of the first thin-film evaporator 203; the outlet of the first thin-film evaporator 203 is connected to the inlet of the first receiving tank 204; the outlet of the first receiving tank 204 is connected to the inlet of the fifth transfer pump 205; the outlet of the fifth transfer pump 205 is connected to the inlet of the third heat exchanger 206; the third The outlet of heat exchanger 206 is connected to the inlet of the second mixing tank 207; the outlet of the second mixing tank 207 is connected to the inlet of the seventh transfer pump 208; the vacuum interface of the first thin film evaporator 203 is connected to the upper vacuum interface of the first condenser 209; the lower vacuum interface of the first condenser 209 is connected to the first vacuum unit 212; the outlet of the first condenser 209 is connected to the inlet of the second receiving tank 210; the outlet of the second receiving tank 210 is connected to the inlet of the sixth transfer pump 211.
[0038] like Figure 3As shown, in some embodiments, the second reaction unit 3 includes a second enzyme reactor 301, an eighth transfer pump 302, a third stirred tank 303, and a ninth transfer pump 304. The outlet of the seventh transfer pump 208 is connected to the inlet of the second enzyme reactor 301; the outlet of the second enzyme reactor 301 is connected to the inlet of the third stirred tank 303, and the outlet of the third stirred tank 303 is connected to the inlet of the ninth transfer pump 304. The ninth transfer pump 304 includes a first outlet 3041, a second outlet 3042, and a third outlet 3043. The first outlet 3041 is connected to the inlet of the transfer tank 107, and the second outlet 3042 is connected to the inlet of the first enzyme reactor 106. The discharge port of the ninth transfer pump 304 has three paths, which can be selected according to the product requirements. The third discharge port 3043 of the ninth transfer pump 304 is connected to the inlet of the semi-finished product tank 401, which can produce products with low diglyceride content, i.e., diglyceride content less than 20%. The first discharge port 3041 of the ninth transfer pump 304 is connected to the inlet of the transfer tank 107, and after completing the dehydration operation through the dehydration unit 2, it returns to the second enzyme reactor 301, which can produce products with medium diglyceride content, i.e., diglyceride content between 20% and 50%. The second discharge port 3042 of the ninth transfer pump 304 is connected to the inlet of the first enzyme reactor 106, which can extend the enzyme catalytic reaction time and further improve the diglyceride yield, which can produce products with high diglyceride content, i.e., diglyceride content greater than 50%.
[0039] In this embodiment, the third transfer pump 108 and the eighth transfer pump 302 can drain the material remaining in the enzyme reactor when the reactor is shut down for maintenance or enzyme replacement, thus avoiding material waste during production.
[0040] like Figure 4As shown, in some embodiments, the first separation unit 4 includes a semi-finished product tank 401, a tenth transfer pump 402, a second thin-film evaporator 403, a third receiving tank 404, an eleventh transfer pump 405, a first distillation apparatus 406, a fifth receiving tank 407, a thirteenth transfer pump 408, a second distillation apparatus 409, a seventh receiving tank 410, a fifteenth transfer pump 411, a second condenser 412, a second vacuum unit 413, a fourth receiving tank 414, a twelfth transfer pump 415, a third cold trap 416, a third vacuum unit 417, a sixth receiving tank 418, a fourteenth transfer pump 419, a fourth cold trap 420, a fourth vacuum unit 421, an eighth receiving tank 422, and a sixteenth transfer pump 423. The third outlet 3043 of the ninth conveying pump 304 is connected to the inlet of the semi-finished product tank 401; the outlet of the semi-finished product tank 401 is connected to the inlet of the tenth conveying pump 402; the outlet of the tenth conveying pump 402 is connected to the inlet of the second thin-film evaporator 403; the outlet of the second thin-film evaporator 403 is connected to the inlet of the third receiving tank 404; the outlet of the third receiving tank 404 is connected to the inlet of the eleventh conveying pump 405; the outlet of the eleventh conveying pump 405 is connected to the inlet of the first distillation unit 406. The residue outlet of the first distillation apparatus 406 is connected to the inlet of the fifth receiving tank 407; the outlet of the fifth receiving tank 407 is connected to the inlet of the thirteenth transfer pump 408; the outlet of the thirteenth transfer pump 408 is connected to the inlet of the second distillation apparatus 409; the residue outlet of the second distillation apparatus 409 is connected to the inlet of the seventh receiving tank 410; the outlet of the seventh receiving tank 410 is connected to the inlet of the fifteenth transfer pump 411; and the outlet of the fifteenth transfer pump 411 is connected to the inlet of the by-product tank. The vacuum interface of the second thin-film evaporator 403 is connected to the upper vacuum interface of the second condenser 412; the lower vacuum interface of the second thin-film evaporator 403 is connected to the second vacuum unit 413; the outlet of the second condenser 412 is connected to the inlet of the fourth receiving tank 414; the outlet of the fourth receiving tank 414 is connected to the inlet of the twelfth transfer pump 415. The vacuum interface of the first distillation unit 406 is connected to the lower vacuum interface of the third cold trap 416; the upper vacuum interface of the third cold trap 416 is connected to the third vacuum unit 417; the distillate outlet of the first distillation unit 406 is connected to the inlet of the sixth receiving tank 418; the outlet of the sixth receiving tank 418 is connected to the inlet of the fourteenth transfer pump 419; the vacuum interface of the second distillation unit 409 is connected to the lower vacuum interface of the fourth cold trap 420; the upper vacuum interface of the fourth cold trap 420 is connected to the fourth vacuum unit 421. The distillate outlet of the second distillation unit 409 is connected to the feed inlet of the eighth receiving tank 422; the outlet of the eighth receiving tank 422 is connected to the feed inlet of the sixteenth transfer pump 423; and the outlet of the sixteenth transfer pump 423 is connected to the feed inlet of the crude product tank 5.The material in the semi-finished product tank 401 is separated by a separation unit to remove reactants (fatty acids, glycerol, or monoglycerides), byproducts (water, fatty acids, or monoglycerides), and raw material oil (partial or most of triglycerides) to obtain diglyceride oil. The second thin-film evaporator 403 mainly removes water, fatty acids, and low molecular weight substances; the first distillation unit 406 mainly removes glycerol and / or monoglycerides.
[0041] In some embodiments, the crude product tank 5 includes a first crude product tank 501, a second crude product tank 502, a third crude product tank 503, and a fourth crude product tank 504, with the outlet of the sixteenth transfer pump 423 connected to the inlet of the first crude product tank 501. The material composition in the first crude product tank 501 is mainly diglycerides, followed by triglycerides; the material composition in the by-product tank is mainly triglycerides, followed by diglycerides.
[0042] like Figure 6 As shown, in some embodiments, the adsorption unit 6 includes a twenty-second delivery pump 601, a fourth heat exchanger 602, a second feeding tank 603, a fourth stirring tank 604, a twenty-third delivery pump 605, a filter 606, a twenty-fourth delivery pump 607, and a fifth heat exchanger 608. The inlet of the 22nd transfer pump 601 is connected to the outlet of the first crude product tank 501; the outlet of the 22nd transfer pump 601 is connected to the inlet of the fourth heat exchanger 602; the outlet of the fourth heat exchanger 602 is connected to the inlet of the fourth mixing tank 604; the outlet of the fourth mixing tank 604 is connected to the inlet of the 23rd transfer pump 605; the outlet of the 23rd transfer pump 605 is connected to the inlet of the filter 606; the outlet of the filter 606 is connected to the inlet of the 24th transfer pump 607; the outlet of the 24th transfer pump 607 is connected to the inlet of the fifth heat exchanger 608; the outlet of the fifth heat exchanger 608 is connected to the inlet of the crude product tank 7; and the outlet of the second feeding tank 603 is connected to the inlet of the fourth mixing tank 604.
[0043] In some embodiments, the crude product tank 7 includes a first crude product tank 701, a second crude product tank 702, a third crude product tank 703 and a fourth crude product tank 704, and the outlet of the fifth heat exchanger 608 is connected to the inlet of the first crude product tank 701. In some embodiments, the finished product tank 9 includes a first finished product tank 901, a second finished product tank 902, a third finished product tank 903, and a fourth finished product tank 904.
[0044] like Figure 7As shown, in some embodiments, the deodorization unit 8 includes a 25th transfer pump 801, a 6th heat exchanger 802, a 7th heat exchanger 803, a deodorization tower 804, a 26th transfer pump 805, an 8th heat exchanger 806, a 9th heat exchanger 807, a collector 808, a vacuum pump 809, and a collection tank 810. The inlet of the 25th transfer pump 801 is connected to the outlet of the 2nd crude product tank 702; the inlet of the 25th transfer pump 801 is connected to the first inlet 8021 of the 6th heat exchanger 802; the fourth outlet 8022 of the 6th heat exchanger 802 is connected to the inlet of the 7th heat exchanger 803; the outlet of the 7th heat exchanger 803 is connected to the inlet of the deodorization tower 804; the outlet of the deodorization tower 804 is connected to the inlet of the 26th transfer pump 805; and the outlet of the 26th transfer pump 805 is connected to the inlet of the 6th heat exchanger 802. The second inlet 8023 is connected; the fifth outlet 8024 of the sixth heat exchanger 802 is connected to the inlet of the eighth heat exchanger 806; the outlet of the eighth heat exchanger 806 is connected to the inlet of the ninth heat exchanger 807; the outlet of the ninth heat exchanger 807 is connected to the inlet of the third finished product tank 903; the vacuum interface of the deodorization tower 804 is connected to the upper vacuum interface of the collector 808; the top vacuum interface of the collector 808 is connected to the vacuum pump 809; the outlet of the collector 808 is connected to the inlet of the collection tank 810.
[0045] like Figure 5As shown, in some embodiments, the second separation unit 10 includes a seventeenth transfer pump 1001, a third distiller 1002, a ninth receiving tank 1003, an eighteenth transfer pump 1004, a fourth distiller 1005, an eleventh receiving tank 1006, a twentieth transfer pump 1007, a fifth cold trap 1008, a fifth vacuum unit 1009, a tenth receiving tank 1010, a nineteenth transfer pump 1011, a sixth cold trap 1012, a sixth vacuum unit 1013, a twelfth receiving tank 1014, and a twenty-first transfer pump 1015. The second separation unit 10 can further purify diglycerides and increase the diglyceride content in the product. The outlet of the first crude product tank 501 is connected to the inlet of the seventeenth transfer pump 1001; the outlet of the seventeenth transfer pump 1001 is connected to the inlet of the third distillation apparatus 1002; the outlet of the residue of the third distillation apparatus 1002 is connected to the inlet of the ninth receiving tank 1003; the outlet of the ninth receiving tank 1003 is connected to the inlet of the eighteenth transfer pump 1004; the outlet of the eighteenth transfer pump 1004 is connected to the inlet of the fourth distillation apparatus 1005; the outlet of the residue of the fourth distillation apparatus 1005 is connected to the inlet of the eleventh receiving tank 1006; the outlet of the eleventh receiving tank 1006 is connected to the inlet of the twentieth transfer pump 1007; and the outlet of the twentieth transfer pump 1007 is connected to the inlet of the fourth crude product tank 504. The vacuum port of the third distiller 1002 is connected to the lower vacuum port of the fifth cold trap 1008; the upper vacuum port of the fifth cold trap 1008 is connected to the fifth vacuum unit 1009; the distillate outlet of the second distiller 409 is connected to the feed inlet of the tenth receiving tank 1010; the outlet of the tenth receiving tank 1010 is connected to the feed inlet of the nineteenth transfer pump 1011; and the outlet of the nineteenth transfer pump 1011 is connected to the feed inlet of the second crude product tank 502. The vacuum port of the fourth distiller 1005 is connected to the lower vacuum port of the sixth cold trap 1012; the upper vacuum port of the sixth cold trap 1012 is connected to the sixth vacuum unit 1013; the distillate outlet of the fourth distiller 1005 is connected to the feed inlet of the twelfth receiving tank 1014; the outlet of the twelfth receiving tank 1014 is connected to the feed inlet of the twenty-first transfer pump 1015; and the outlet of the twenty-first transfer pump 1015 is connected to the feed inlet of the third crude product tank 503.
[0046] In some embodiments, the materials in the second crude product tank 502, the third crude product tank 503, or the fourth crude product tank 504 are processed by the adsorption unit 6 and then enter the second crude finished product tank 702, the third crude finished product tank 703, or the fourth crude finished product tank 704, respectively. The materials in the second crude finished product tank 702, the third crude finished product tank 703, or the fourth crude finished product tank 704 are processed by the deodorization unit 8 and then enter the second finished product tank 902, the third finished product tank 903, or the fourth finished product tank 904, respectively. The product stored in the finished product tank 9 is diglyceride oil.
[0047] In some embodiments, a first cold trap 213 and a first buffer tank 214 are provided between the first condenser 209 and the first vacuum unit 212. The vacuum interface at the lower part of the first condenser 209 is sequentially connected to the first cold trap 213, the first buffer tank 214, and the first vacuum unit 212. A second cold trap 424 and a second buffer tank 425 are provided between the second condenser 412 and the second vacuum unit 413. The vacuum interface at the lower part of the second condenser 412 is sequentially connected to the second cold trap 424, the second buffer tank 425, and the second vacuum unit 413. A vacuum third buffer tank 426 is also provided between the third cold trap 416 and the third vacuum unit 417; a vacuum fourth buffer tank 427 is also provided between the fourth cold trap 420 and the fourth vacuum unit 421; a vacuum fifth buffer tank 1016 is also provided between the fifth cold trap 1008 and the fifth vacuum unit 1009; and a vacuum sixth buffer tank 1017 is also provided between the sixth cold trap 1012 and the sixth vacuum unit 1013.
[0048] In some embodiments, in the first reaction unit 1, after heat exchange by the first heat exchanger 102, the material temperature rises to 50-70°C; in the dehydration unit 2, the evaporation surface temperature of the first thin-film evaporator 203 is 90-110°C, and the vacuum degree of the first vacuum unit 212 is 1-150 Pa. After heat exchange by the second heat exchanger 202, the material temperature rises to 80-90°C. After heat exchange by the third heat exchanger 206, the material temperature drops to 50-70°C. The dehydration unit 2 removes water generated during the reaction, promoting the enzyme-catalyzed transesterification reaction towards the formation of diglycerides, thereby increasing the conversion rate of diglycerides. The discharge port of the ninth delivery pump 304 has three paths, allowing the material to follow the appropriate path according to product requirements.
[0049] In some embodiments, the first distiller 406 and the second distiller 409 in the first separation unit 4 are both short-path distillers; the evaporation surface temperature of the first distiller 406 is 200–250°C, and the evaporation surface temperature of the second distiller 409 is 290–295°C. The vacuum degree of the third vacuum unit 417 and the fourth vacuum unit 421 is 0.1–5 Pa; the evaporation surface temperature of the second thin-film evaporator 403 is 120–170°C, and the vacuum degree of the second vacuum unit 413 is 0.1–50 Pa. The material in the semi-finished product tank 401 passes through the first separation unit to remove reactants (fatty acids, glycerol, or monoglycerides), byproducts (water, fatty acids, or monoglycerides), and raw material oil (partial or most of triglycerides) to obtain diglyceride oil. The second thin-film evaporator 403 mainly removes water, fatty acids, and low molecular weight substances; the first distillation unit 406 mainly removes glycerol and / or monoglycerides; the material in the first crude product tank 501 mainly consists of diglycerides, followed by triglycerides; the material in the by-product tank mainly consists of triglycerides, followed by diglycerides.
[0050] In some embodiments, the second separation unit 10, the third distillation unit 1002, and the fourth distillation unit 1005 are all short-path distillations; the evaporation surface temperature of the third distillation unit 1002 is 270–280°C, the evaporation surface temperature of the fourth distillation unit 1005 is 280–290°C, and the vacuum degree of the fifth vacuum unit 1009 and the sixth vacuum unit 1013 is 0.1–5 Pa; after passing through the second separation unit 10, diglycerides can be further purified, increasing the diglyceride content in the product.
[0051] In some embodiments, the adsorption unit 6 uses a filter 606 to complete the filtration operation; after heat exchange in the fourth heat exchanger 602, the material is heated to 105-120°C; the adsorption material is activated carbon, and the amount used is 3% of the weight of the raw oil; after passing through the adsorption unit 6, pigments and polar components (such as glycidyl esters) in the crude product can be removed to a large extent, further improving the quality of the product.
[0052] In some embodiments, the deodorization unit 8 utilizes direct steam in a packed deodorization tower, with a deodorization temperature of 170~240℃ and a vacuum degree of 10~300Pa. The deodorized diglyceride oil product is cooled to below 50℃ by passing through the sixth heat exchanger 802, the eighth heat exchanger 806, and the ninth heat exchanger 807 in sequence before entering the diglyceride oil product tanks, namely the first finished product tank 901, the second finished product tank 902, the third finished product tank 903, and the fourth finished product tank 904. After passing through the deodorization unit 8, odor components and a small amount of fatty acids can be removed, further improving the quality of the product.
[0053] In this embodiment, the material in the second crude product tank 502 has the highest diglyceride content in the first separation unit 4 and the second separation unit 10. The relationship of diglyceride content in the four crude product tanks is: second crude product tank 502 > third crude product tank 503 ≥ first crude product tank 501 > fourth crude product tank 504. The installation of a cold trap and a buffer tank between the condenser and the vacuum unit ensures stable vacuum conditions during production. The cold trap further condenses the vaporized components extracted by vacuum, and the buffer tank stores the material condensed in the cold trap, discharges it periodically, and prevents liquid material from being drawn back into the system. Adsorption unit 6 primarily removes pigments and polar components (such as glycidyl esters) from the crude product, further improving product quality. Deodorization unit 8 primarily removes odor components and a small amount of fatty acids, further improving product quality. The deodorized diglyceride oil product from deodorization unit 8 exchanges heat with the crude diglyceride oil awaiting deodorization in the sixth heat exchanger 802. The temperature of the deodorized diglyceride oil product decreases, while the temperature of the crude diglyceride oil awaiting deodorization increases, fully utilizing thermal energy and saving energy. The diglyceride oil production system provided by this invention can significantly increase the diglyceride content in the diglyceride oil product, allowing for the production of multiple product specifications based on the diglyceride content. Furthermore, the byproducts of each stage in this invention can be sold externally, with no wastewater or waste residue discharge, making it more economical, environmentally friendly, and suitable for industrial production.
[0054] Furthermore, the present invention also provides a method for producing diglyceride oil, using the aforementioned diglyceride oil production system, the method of which is as follows: S1. Material enters the first reaction unit: The raw material first enters the first reaction unit 1. After being heated to 50-70°C by the first heat exchanger 102 via the first transfer pump 101, the raw material enters the first stirring tank 103. The first feeding tank 104 adds material to the first stirring tank 103. After being fully mixed with the raw material, the material enters the first enzyme reactor 106 via the second transfer pump 105 to carry out the reaction. The material that has completed the reaction enters the transfer tank 107 through the outlet of the first enzyme reactor 106. S2. Material enters dehydration unit 2: The material in transfer tank 107 enters the second heat exchanger 202 via the fourth transfer pump 201. After being heated to 80-90°C, it enters the first thin-film evaporator 203. The evaporation surface temperature is 90-110°C. After dehydration, the material enters the first receiving tank 204 via the outlet of the first thin-film evaporator 203. Then, it is sent to the third heat exchanger 206 by the fifth transfer pump 205 for cooling. After being cooled to 50-70°C, it enters the second stirring tank 207. After being fully stirred and mixed in the second stirring tank 207, it enters the second enzyme reactor 301 via the seventh transfer pump 208. The vacuum interface of the first thin-film evaporator 203 is connected in sequence to the first condenser 209, the first cold trap 213, the first buffer tank 214 and the first vacuum unit 212, with a vacuum degree of 1 to 150 Pa. The condensed material in the first condenser 209 enters the second receiving tank 210 through the discharge port, and is then discharged by the sixth delivery pump 211, which can be sold directly as a by-product.
[0055] S3, Entering the second reaction unit 3: The material in the second enzyme reactor 301 continues to react in the second reaction unit 3: The material in the second enzyme reactor 301 undergoes reaction with lipase TL. Under the catalysis of IM, the transesterification reaction continues to produce diglycerides. After 12 hours of reaction, the material enters the third stirred tank 303 through the outlet of the second enzyme reactor 301. When producing a product with low diglyceride content, the material in the third stirred tank 303 enters the semi-finished product tank 401 through the ninth transfer pump 304. When producing a product with medium diglyceride content, the material in the third stirred tank 303 enters the transfer tank 107 through the ninth transfer pump 304, and then returns to the second enzyme reactor 301 after dehydration in the dehydration unit 2, and then enters the semi-finished product tank 401. When producing a product with high diglyceride content, the material in the third stirred tank 303 enters the inlet of the first enzyme reactor 106 through the ninth transfer pump 304, and then repeats the process of entering the first reaction unit 1, the dehydration unit 2, and the second reaction unit 3 once. After reacting for 24 hours, it enters the semi-finished product tank 401 for subsequent operations.
[0056] S4. Entering the first separation unit 4: The material in the semi-finished product tank 401 enters the second thin-film evaporator 403 via the tenth transfer pump 402. The evaporation surface temperature is 120-170℃. The distillate enters the third receiving tank 404 through the outlet of the second thin-film evaporator 403, and is then sent to the first distiller 406 by the eleventh transfer pump 405. The evaporation surface temperature is 200-250℃. The distillate from the first distiller 406 enters the fifth receiving tank 40 through the distillate outlet of the first distiller 406. 7. Then, it enters the second distillation unit 409 via the thirteenth transfer pump 408. The evaporation surface temperature is 290-295℃. The residue from the second distillation unit 409 enters the seventh receiving tank 410 via the residue outlet of the second distillation unit 409, and then enters the by-product tank via the fifteenth transfer pump 411. The vacuum interface of the second thin film evaporator 403 is connected in sequence to the second condenser 412, the second cold trap 424, the second buffer tank 425, and the second vacuum unit 413, with a vacuum degree of 0.1-50 Pa. The condensed material in the second condenser 412 enters the fourth receiving tank 414 through the outlet, and is then discharged by the twelfth transfer pump 415. The vacuum interface of the first distiller 406 is sequentially connected to the third cold trap 416, the third buffer tank 426, and the third vacuum unit 417, with a vacuum degree of 0.1-5 Pa. The distillate from the first distiller 406 enters the sixth receiving tank 418 through the distillate outlet of the first distiller 406, and is then discharged by the fourteenth transfer pump 419. The vacuum interface of the second distiller 409 is sequentially connected to the fourth cold trap 420, the fourth buffer tank 427, and the fourth vacuum unit 421, with a vacuum degree of 0.1-5 Pa. The distillate from the second distiller 409 enters the eighth receiving tank 422 through the distillate outlet of the second distiller 409, and is then discharged by the sixteenth transfer pump 423 into the first crude product tank 501.
[0057] The second separation unit 10 can further purify diglycerides and increase the content of diglycerides in the product. When the content of diglycerides in the crude product produced by the first separation unit 4 does not meet the production requirements (the content of diglycerides is lower than the production requirements), the second separation unit 10 needs to be added to further purify the crude product in the first separation unit 4, thereby increasing the content of diglyceride oil in the final product.
[0058] S5. Entering Adsorption Unit 6: The material in the first crude product tank 501 enters the adsorption unit 6 for adsorption treatment. The adsorption unit 6 uses a filter 606 to complete the filtration operation: The material in the first crude product tank 501 enters the fourth heat exchanger 602 via the twenty-second transfer pump 601 and is heated to 105-120°C before entering the fourth mixing tank 604. The second feeding tank 603 feeds the material into the fourth mixing tank 604. After being fully mixed with the material, the material enters the filter 606 via the twenty-third transfer pump 605. After the activated carbon is removed by filtration, the material enters the fifth heat exchanger 608 via the twenty-fourth transfer pump 607 and is cooled to below 50°C before entering the first crude finished product tank 701.
[0059] S6. The material in the first crude product tank 701 enters the deodorization unit 8 for deodorization treatment: The material in the first crude product tank 701 enters the sixth heat exchanger 802 after passing through the twenty-fifth conveying pump 801 and the first inlet 8021 of the sixth heat exchanger 802. After exchanging heat with the deodorized material, it enters the seventh heat exchanger 807 through the fourth outlet 8022 of the sixth heat exchanger 802. After being heated to 170~240℃, it enters the deodorization tower and completes the deodorization treatment with the participation of direct steam. Then, the material passes through the 26th conveying pump 805 and the second inlet 8023 of the 6th heat exchanger 802 in sequence, and then enters the 6th heat exchanger 802. After exchanging heat with the material waiting for deodorization, it passes through the fifth outlet 8024 of the 6th heat exchanger 802 in sequence, and then enters the 8th heat exchanger 806 and the 9th heat exchanger 807 to be cooled to below 50°C before entering the first finished product tank 901. The vacuum interface of the deodorization tower is connected to the collector 808 and the vacuum pump 809 in sequence, and the vacuum degree is 10~300Pa. The deodorized distillate enters the collection tank 810 through the outlet of the collector 808.
[0060] Example 1 This embodiment uses the aforementioned diglyceride oil production system. The raw material used is refined rice bran oil (hereinafter referred to as rice bran oil) whose color meets the first-grade standard of GB / T 19112-2003. The auxiliary materials are fatty acids (oleic acid) and glycerol, and the catalyst is immobilized lipase TL IM. Both the first enzyme reactor 106 and the second enzyme reactor 301 are immobilized enzyme reactors.
[0061] Rice bran oil first enters the first reaction unit 1 for reaction: 1 ton of rice bran oil enters the first heat exchanger 102 via the first transfer pump 101 and is heated to 50-70°C, then enters the first stirring tank 103. Oleic acid (150 kg) and glycerol (75 kg) enter the first stirring tank 103 via the first feeding tank 104. After being thoroughly mixed with the rice bran oil, the mixture enters the first enzyme reactor 106 via the second transfer pump 105 (the loading amount of immobilized lipase TL IM is 30 kg). In the presence of immobilized lipase TL IM and glycerol, the rice bran oil undergoes an ester exchange reaction to generate diglycerides. The material that has completed the reaction enters the transfer tank 107 through the outlet of the first enzyme reactor 106.
[0062] The material in the transfer tank 107 enters the dehydration unit 2 for dehydration treatment: the material in the transfer tank 107 enters the second heat exchanger 202 via the fourth transfer pump 201, and after being heated to 80-90°C, it enters the first thin film evaporator 203 (evaporation surface temperature is 90-110°C). After dehydration, the material enters the first receiving tank 204 through the outlet of the first thin film evaporator 203, and is then sent to the third heat exchanger 206 by the fifth transfer pump 205 for cooling. After being cooled to 50-70°C, it enters the second stirring tank 207. After being fully stirred and mixed in the second stirring tank 207, it enters the second enzyme reactor 301 via the seventh transfer pump 208. The vacuum interface of the first thin-film evaporator 203 is connected in sequence to the first condenser 209, the first cold trap 213, the first buffer tank 214 and the first vacuum unit 212 (vacuum degree of 1 to 150 Pa); the condensed material in the first condenser 209 enters the second receiving tank 210 through the discharge port, and is then discharged by the sixth delivery pump 211 (sold directly as a by-product).
[0063] The material in the second enzyme reactor 301 continues to react in the second reaction unit 3: Under the catalysis of the lipase TL IM, the material in the second enzyme reactor 301 (with a loading of 20 kg of immobilized lipase TL IM) continues to undergo transesterification to generate diglycerides. The material after 12 hours of reaction (the cumulative reaction time in the first enzyme reactor 106 and the second enzyme reactor 301) enters the third stirred tank 303 through the outlet of the second enzyme reactor 301, and then enters the semi-finished product tank 401 through the ninth transfer pump 304.
[0064] The material in the semi-finished product tank 401 enters the first separation unit 4 for separation: the material in the semi-finished product tank 401 enters the second thin-film evaporator 403 (evaporation surface temperature is 120-170℃, mainly removing water, fatty acids and low molecular weight substances) via the tenth transfer pump 402; the distillate enters the third receiving tank 404 through the outlet of the second thin-film evaporator 403, and is then sent to the first distiller 406 (evaporation surface temperature is 200-250℃, mainly removing glycerol and monoglycerides) by the eleventh transfer pump 405; the distillate from the first distiller 406 enters the fifth distiller 406 through the distillate outlet of the first distiller 406. The material is received in tank 407 and then enters the second distillation unit 409 (evaporation surface temperature is 290-295℃) via the thirteenth transfer pump 408. The residue of the second distillation unit 409 (the material composition is mainly triglycerides, followed by diglycerides) enters the seventh receiving tank 410 through the residue outlet of the second distillation unit 409, and then enters the by-product tank (sold directly as a by-product) via the fifteenth transfer pump 411. The vacuum interface of the second thin film evaporator 403 is connected in sequence to the second condenser 412, the second cold trap 424, the second buffer tank 425, and the second vacuum unit 413 (vacuum degree is 0.1-50Pa). The condensed material in the second condenser 412 enters the fourth receiving tank 414 through the outlet, and is then discharged by the twelfth transfer pump 415 (sold directly as a by-product). The vacuum interface of the first distiller 406 is sequentially connected to the third cold trap 416, the third buffer tank 426, and the third vacuum unit 417 (vacuum degree of 0.1-5 Pa). The distillate of the first distiller 406 enters the sixth receiving tank 418 through the distillate outlet of the first distiller 406, and is then discharged by the fourteenth transfer pump 419 (sold directly as a by-product). The vacuum interface of the second distiller 409 is sequentially connected to the fourth cold trap 420, the fourth buffer tank 427, and the fourth vacuum unit 421 (vacuum degree of 0.1-5 Pa). The distillate of the second distiller 409 (the material composition is mainly diglycerides, followed by triglycerides) enters the eighth receiving tank 422 through the distillate outlet of the second distiller 409, and is then discharged by the sixteenth transfer pump 423 into the first crude product tank 501. Tests showed that the diglyceride content in the first crude product tank 501 was 45.6%.
[0065] The material in the first crude product tank 501 enters the adsorption unit 6 for adsorption treatment. The adsorption unit 6 uses a filter 606 to complete the filtration operation: the material in the first crude product tank 501 enters the fourth heat exchanger 602 via the twenty-second transfer pump 601 and is heated to 105-120°C before entering the fourth mixing tank 604. Activated carbon (15 kg, accounting for 3% of the material weight) enters the fourth mixing tank 604 via the second feeding tank 603. After being fully mixed with the material, it enters the filter 606 via the twenty-third transfer pump 605. After the activated carbon is removed, the material enters the fifth heat exchanger 608 via the twenty-fourth transfer pump 607 and is cooled to below 50°C before entering the first crude finished product tank 701. After passing through the adsorption unit 6, pigments and polar components (such as glycidyl esters) in the crude product can be removed to a large extent, further improving the quality of the product.
[0066] The material in the first crude product tank 701 enters the deodorization unit 8 for deodorization treatment: The material in the first crude product tank 701 passes through the twenty-fifth conveying pump 801 and the first inlet 8021 of the sixth heat exchanger 802 in sequence, and then enters the sixth heat exchanger 802. After exchanging heat with the deodorized material, it enters the seventh heat exchanger 807 through the fourth outlet 8022 of the sixth heat exchanger 802. After being heated to 170~240℃, it enters the deodorization tower, where the deodorization treatment is completed with the participation of direct steam. Then, the material passes through the 26th conveying pump 805 and the second inlet 8023 of the 6th heat exchanger 802, and enters the 6th heat exchanger 802. After exchanging heat with the material waiting for deodorization, it passes through the fifth outlet 8024 of the 6th heat exchanger 802 and enters the 8th heat exchanger 806 and the 9th heat exchanger 807 to be cooled to below 50°C before entering the first finished product tank 901. The vacuum interface of the deodorization tower is connected to the collector 808 and the vacuum pump 809 (vacuum degree of 10~300Pa) in sequence. The deodorized distillate enters the collection tank 810 through the outlet of the collector 808 (to be sold directly as a by-product). After passing through the deodorization unit 8, odor components and a small amount of fatty acids can be removed, further improving the quality of the product.
[0067] The product specifications in the first finished product can 901 were as follows: color (Lovibond colorimeter 133.4mm): yellow 35, red 3.2, and diglyceride content: 45.9%.
[0068] Example 2 Similar to Example 1, the only difference is that the material entering the third stirred tank 303 through the outlet of the second enzyme reactor 301 first enters the transfer tank 107 through the ninth transfer pump 304, and then repeats the process of entering the dehydration unit 2 and the second reaction unit 10 once. The material reacts for 18 hours (the cumulative reaction time in the first enzyme reactor 106 and the second enzyme reactor 301) and then enters the third stirred tank 303 through the outlet of the second enzyme reactor 301, and then enters the semi-finished product tank 401 through the ninth transfer pump 304.
[0069] Tests showed that the diglyceride content in the first crude product tank 501 was 60.4%.
[0070] The final product data for the first finished product can 901 were as follows: color (Lovibond colorimeter 133.4mm): yellow 35, red 3.2, and diglyceride content: 60.6%.
[0071] Example 3 Similar to Example 1, the only difference is that the material entering the third stirred tank 303 through the outlet of the second enzyme reactor 301 first enters the first enzyme reactor 106 through the ninth transfer pump 304, and then repeats the process of entering the first reaction unit 1, the dehydration unit 2, and the second reaction unit 3 once. The material that has reacted for 24 hours (the cumulative reaction time in the first enzyme reactor 106 and the second enzyme reactor 301) enters the third stirred tank 303 through the outlet of the second enzyme reactor 301 first enters the semi-finished product tank 401 through the ninth transfer pump 304.
[0072] Tests showed that the diglyceride content in the first crude product tank 501 was 77.5%.
[0073] The final product data for the first finished product can 901 were as follows: color (Lovibond colorimeter 133.4mm): yellow 35, red 3.2, and diglyceride content: 77.8%.
[0074] Example 4 Similar to Example 1, the only difference is that the raw material used in this example is rice bran oil (hereinafter referred to as rice bran oil) with an acid value of 31 mgKOH / g that has undergone degumming, decolorization and dewaxing treatment, and the excipient is glycerin.
[0075] Tests showed that the diglyceride content in the first crude product tank 501 was 41.3%.
[0076] According to the test results, the product specifications of the first finished product can 901 are as follows: color (Lovibond colorimeter 133.4mm) yellow 35 red 3.2, and diglyceride content is 41.7%.
[0077] Example 5 Similar to Example 3, except that the material in the first crude product tank 501 enters the second separation unit 10 before entering the adsorption unit 6: the material in the first crude product tank 501 is fed into the third distillation unit 1002 (evaporation surface temperature is 270-280°C) by the seventeenth transfer pump 1001; the residue of the third distillation unit 1002 enters the ninth receiving tank 1003 through the residue outlet of the third distillation unit 1002, and then enters the fourth distillation unit 1005 (evaporation surface temperature is 280-290°C) by the eighteenth transfer pump 1004; the residue of the fourth distillation unit 1005 enters the eleventh receiving tank 1006 through the residue outlet of the fourth distillation unit 1005, and then enters the fourth crude product tank 504 by the twentieth transfer pump 1007; and is then fed into the third distillation unit 1002. The vacuum interface of distiller 1002 is sequentially connected to the fifth cold trap 1008, the fifth buffer tank 1016, and the fifth vacuum unit 1009 (vacuum degree 0.1-5 Pa). The distillate from the third distiller 1002 enters the tenth receiving tank 1010 through the distillate outlet of the third distiller 1002, and then enters the second crude product tank 502 via the nineteenth transfer pump 1011. The vacuum interface of the fourth distiller 1005 is sequentially connected to the sixth cold trap 1012, the sixth buffer tank 1017, and the sixth vacuum unit 1013 (vacuum degree 0.1-5 Pa). The distillate from the fourth distiller 1005 enters the twelfth receiving tank 1014 through the distillate outlet of the fourth distiller 1005, and then enters the third crude product tank 503 via the twenty-first transfer pump 1015. After passing through the second separation unit 10, diglycerides can be further purified to increase the diglyceride content in the product. Tests showed that the diglyceride content in the second crude product tank 502 was 95.3%, the diglyceride content in the third crude product tank 503 was 82.4%, and the diglyceride content in the fourth crude product tank 504 was 20.8%.
[0078] The materials in the second crude product tank 502, the third crude product tank 503, and the fourth crude product tank 504 respectively enter the adsorption unit for adsorption treatment. After the adsorption treatment is completed, the materials enter the second crude finished product tank 702, the third crude finished product tank 703, and the fourth crude finished product tank 704 respectively.
[0079] The materials in the second crude finished product tank 702, the third crude finished product tank 703, and the fourth crude finished product tank 704 are respectively fed into the deodorization unit 8 for deodorization treatment. After the deodorization treatment is completed, the materials are respectively fed into the second finished product tank 902, the third finished product tank 903, and the fourth finished product tank 904.
[0080] The product specifications for the second finished product can 902 were as follows: color (Lovibond colorimeter 133.4mm): yellow 35, red 3.2, and diglyceride content: 95.4%; the product specifications for the third finished product can 903 were as follows: color (Lovibond colorimeter 133.4mm): yellow 35, red 3.2, and diglyceride content: 82.6%; the product specifications for the fourth finished product can 904 were as follows: color (Lovibond colorimeter 133.4mm): yellow 35, red 3.3, and diglyceride content: 20.9%.
[0081] When the evaporation surface temperature of the third still 1002 is 270–280°C, the majority of the distilled light components are diglycerides (second crude product tank 502, corresponding to the second finished product tank 902), while the majority of unreacted triglycerides remain in the residue of the third still 1002 at this time. When the evaporation surface temperature of the fourth still 1005 is 280–290°C, the distilled light components will contain a small amount of low-boiling triglycerides (third crude product tank 503, corresponding to the third finished product tank 903). Therefore, compared with the second finished product tank 902, the diglyceride content of the product in the third finished product tank 903 will be lower. When the evaporation surface temperature of the fourth still 1005 is 280–290°C, the residue mainly consists of unreacted triglycerides and a small amount of high-boiling diglycerides (fourth crude product tank 704, corresponding to the fourth finished product tank 904). Therefore, the diglyceride content in the residue is the lowest.
[0082] Example 6 Similar to Example 5, the only difference is that the raw material used in this example is refined soybean oil (hereinafter referred to as soybean oil) that meets the first-grade standard of GB / T 1535-2017, and the auxiliary materials are fatty acids (oleic acid) and monoglycerides, with an amount of 435 kg of monoglycerides added.
[0083] Tests showed that the diglyceride content in the second crude product tank 502 was 85.7%, the diglyceride content in the third crude product tank 503 was 73.8%, and the diglyceride content in the fourth crude product tank 504 was 25.6%.
[0084] The product specifications for the second finished product can 902 were as follows: color (Lovibond colorimeter 133.4mm): yellow 35, red 3.3, and diglyceride content: 85.8%; the product specifications for the third finished product can 903 were as follows: color (Lovibond colorimeter 133.4mm): yellow 35, red 3.3, and diglyceride content: 73.8%; the product specifications for the fourth finished product can 904 were as follows: color (Lovibond colorimeter 133.4mm): yellow 35, red 3.4, and diglyceride content: 25.7%.
[0085] Through the above embodiments 1 to 3, it is known that repeatedly feeding the material into the first reaction unit 1, dehydration unit 2, and second reaction unit 10, and extending the reaction time of the enzyme reactor, can increase the content of diglyceride oil. Therefore, the present invention uses the first reaction unit 1, dehydration unit 2, and second reaction unit 10 to carry out the conversion reaction of raw material oil into diglyceride oil in the presence of catalyst and reactants (fatty acids, glycerol, or monoglycerides), which can improve the conversion efficiency of diglycerides. Through embodiments 1 and 4, it is known that using rice bran oil with a high acid value (31 mgKOH / g) and having undergone degumming, decolorization, and dewaxing treatment as raw material for the production of diglyceride oil can also yield ideal diglyceride oil products. The method of the present invention can be applied to a wide range of oil raw materials. Through embodiments 5 and 6, it is known that commercially available vegetable oils can all be used as raw materials for the production of diglyceride oil. Due to differences in fatty acid composition, the content of diglycerides in the product will fluctuate, but overall it can meet the product requirements of diglyceride oil. Soybean oil is the cheapest commercially available vegetable oil with a high market share. Its fatty acid composition is characterized by high levels of both linoleic acid and oleic acid (linoleic acid accounts for a higher percentage than oleic acid, and together they make up about 80%), making it representative of vegetable oils. Rice bran oil, on the other hand, has lower levels of oleic acid and linoleic acid than soybean oil (oleic acid accounts for a higher percentage than linoleic acid, and together they make up about 70%), and its palmitic acid content is approximately 16%. It is precisely because of these significant differences in fatty acid composition that the resulting diglyceride oil exhibits a difference in fatty acid composition, leading to differences in boiling points (palmitic acid has a lower boiling point than oleic acid, and oleic acid has a lower boiling point than linoleic acid). Ultimately, this results in lower diglyceride content in the second finished product tank 902 and the third finished product tank 903 compared to Example 5, while the diglyceride content in the fourth crude product tank 504 is higher than in Example 5.
[0086] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention, and should all be included within the protection scope of the present invention.
Claims
1. A diglyceride oil production system, characterized in that, include: First reaction unit (1); The dehydration unit (2) is connected to the first reaction unit (1); The second reaction unit (3) is connected to the dehydration unit (2) and can also be connected to the first reaction unit (1); The first separation unit (4) is connected to the second reaction unit (3); Adsorption unit (6), which is connected to the first separation unit (4) through crude product tank (5); The deodorization unit (8) is connected to the adsorption unit (6) through the crude product tank (7). The deodorization unit (8) is connected to the finished product tank (9) on the side away from the adsorption unit (6). When the content of diglycerides in the produced product is low, the material after the reaction in the second reaction unit (3) directly enters the first separation unit (4). When the diglyceride content in the produced product is moderate, the material after being reacted in the second reaction unit (3) re-enters the dehydration unit (2) and the second reaction unit (3) for further reaction, and after the material is reacted again, it enters the first separation unit (4); When the product has a high content of diglycerides, the material after being reacted in the second reaction unit (3) enters the first reaction unit (1), the dehydration unit (2), and the second reaction unit (3) again. After the material reacts again, it enters the first separation unit (4).
2. The diglyceride oil production system according to claim 1, characterized in that, The first reaction unit (1) includes a first delivery pump (101), a first heat exchanger (102), a first stirring tank (103), a second delivery pump (105), a first enzyme reactor (106), and a transfer tank (107) connected in sequence. A first feeding tank (104) is connected to one side of the first stirring tank (103), and the outlet of the transfer tank (107) is connected to the dehydration unit (2).
3. The diglyceride oil production system according to claim 2, characterized in that, The dehydration unit (2) includes a fourth transfer pump (201), a second heat exchanger (202), a first thin film evaporator (203), a first receiving tank (204), a fifth transfer pump (205), a third heat exchanger (206), a second stirring tank (207), and a seventh transfer pump (208) connected in sequence. The seventh transfer pump (208) is connected to the second reaction unit (3), and the fourth transfer pump (201) is connected to the transfer tank (107). The dehydration unit (2) further includes a first condenser (209), a second receiving tank (210), a sixth delivery pump (211), and a first vacuum unit (212). The vacuum interface of the first thin-film evaporator (203) is connected to the upper vacuum interface of the first condenser (209); the lower vacuum interface of the first condenser (209) is connected to the first vacuum unit (212); the first condenser (209) is connected to the second receiving tank (210); and the second receiving tank (210) is connected to the sixth delivery pump (211).
4. The diglyceride oil production system according to claim 3, characterized in that, The second reaction unit (3) includes a second enzyme reactor (301), a third stirring tank (303), and a ninth delivery pump (304) connected in sequence. The second enzyme reactor (301) is connected to the seventh delivery pump (208). The ninth delivery pump includes a first outlet (3041), a second outlet (3042), and a third outlet (3043). The first outlet (3041) is connected to the inlet of the transfer tank (107). The second outlet (3042) is connected to the inlet of the first enzyme reactor (106). The third outlet (3043) is connected to the first separation unit (4). It also includes an eighth delivery pump (302), the two ends of which are connected to the second enzyme reactor (301) and the transfer tank (107), respectively.
5. The diglyceride oil production system according to claim 4, characterized in that, The first separation unit (4) includes a semi-finished product tank (401), a tenth transfer pump (402), a second thin film evaporator (403), a third receiving tank (404), an eleventh transfer pump (405), a first distillation apparatus (406), a fifth receiving tank (407), a thirteenth transfer pump (408), a second distillation apparatus (409), a seventh receiving tank (410), and a fifteenth transfer pump (411) connected in sequence. The inlet of the semi-finished product tank (401) is connected to the third outlet (3043), and the fifteenth transfer pump (411) is connected to the by-product tank. The second thin film evaporator (403) is connected in sequence to a second condenser (412) and a second vacuum unit (413) on one side, and its outlet is connected in sequence to a fourth receiving tank (414) and a twelfth delivery pump (415). The outlet of the first distiller (406) is connected to the sixth receiving tank (418) and the fourteenth delivery pump (419), and the outlet of the second distiller (409) is connected to the eighth receiving tank (422) and the sixteenth delivery pump (423). The sixteenth delivery pump (423) is connected to the crude product tank (5).
6. The diglyceride oil production system according to claim 5, characterized in that, The adsorption unit (6) includes a 22nd delivery pump (601), a 4th heat exchanger (602), a 4th mixing tank (604), a 23rd delivery pump (605), a filter (606), a 24th delivery pump (607), and a 5th heat exchanger (608) connected in sequence. A 2nd feeding tank (603) is connected to one side of the 4th mixing tank (604). The 22nd delivery pump (601) is connected to the 1st crude product tank (501) of the crude product tank (5). The outlet of the 5th heat exchanger (608) is connected to the crude finished product tank (7).
7. The diglyceride oil production system according to claim 6, characterized in that, The deodorization unit (8) includes a 25th transfer pump (801), a 6th heat exchanger (802), a 7th heat exchanger (803), a deodorization tower (804), a 26th transfer pump (805), an 8th heat exchanger (806), a 9th heat exchanger (807), a collector (808), a vacuum pump (809), and a collection tank (810). The inlet of the 25th transfer pump (801) is connected to the outlet of the 2nd crude product tank (702); the inlet of the 25th transfer pump (801) is connected to the first inlet (8021) of the 6th heat exchanger (802); the fourth outlet (8022) of the 6th heat exchanger (802) is connected to the inlet of the 7th heat exchanger (803); the 7th heat exchanger (803) is connected to the deodorization tower (804); the outlet of the deodorization tower (804) is connected to the first inlet (8021) of the 6th heat exchanger (802); the outlet of the deodorization tower (804) is connected to the first inlet (8021) of the 6th heat exchanger (802); the fourth outlet (8022) of the 6th heat exchanger (802) is connected to the inlet of the 7th heat exchanger (803); the 803 of the 7th heat exchanger (803) is connected to the deodorization tower (804); the outlet of the deodorization tower (804) is connected to the first inlet (8021) of the 6th heat exchanger (802); the fourth outlet (8022) of the 6th heat exchanger (802) is connected to the inlet (802) of the 7th heat exchanger (803); the fourth outlet (8022) of the 6th heat exchanger (8 The feed inlet is connected to the feed inlet of the 26th conveying pump (805); the discharge outlet of the 26th conveying pump (805) is connected to the second feed inlet (8023) of the 6th heat exchanger (802); the fifth discharge outlet (8024) of the 6th heat exchanger (802) is connected to the feed inlet of the 8th heat exchanger (806); the discharge outlet of the 8th heat exchanger (806) is connected to the feed inlet of the 9th heat exchanger (807); the discharge outlet of the 9th heat exchanger (807) is connected to the feed inlet of the 3rd finished product tank (903); the vacuum interface of the deodorization tower (804) is connected to the upper vacuum interface of the trap (808); the top vacuum interface of the trap (808) is connected to the vacuum pump (809); the discharge outlet of the trap (808) is connected to the feed inlet of the collection tank (810).
8. The diglyceride oil production system according to claim 7, characterized in that, It also includes a second separation unit (10), which includes a seventeenth transfer pump (1001), a third distillation apparatus (1002), a ninth receiving tank (1003), an eighteenth transfer pump (1004), a fourth distillation apparatus (1005), an eleventh receiving tank (1006), and a twentieth transfer pump (1007) connected in sequence. The seventeenth transfer pump (1001) is connected to the first crude product tank (501) of the crude product tank (5), and the twentieth transfer pump (1007) is connected to the fourth crude product tank (504) of the crude product tank (5). The tenth receiving tank (1010), the nineteenth transfer pump (1011), and the second crude product tank (502) are sequentially connected to one side of the third distiller (1002). The fourth distiller (1005) is connected in sequence to the twelfth receiving tank (1014), the twenty-first transfer pump (1015), and the third crude product tank (503).
9. A method for producing diglyceride oil, characterized in that, The diglyceride oil production system according to any one of claims 1-8 is used, and the production method includes: S1. The material enters the first reaction unit (1) and enters the transfer tank (107) after being reacted by the first heat exchanger (102), the first stirred tank (103) and the first enzyme reactor (106). S2. The material enters the dehydration unit (2) from the transfer tank (107), and flows into the second reaction unit (3) after being heated by the second heat exchanger (202), evaporated by the first thin film evaporator (203), cooled by the third heat exchanger (206), and stirred by the second stirring tank (207). S3. After the material is dehydrated by the dehydration unit (2), it enters the second reaction unit (3), and after being reacted and stirred by the second enzyme reactor (301) and the third stirring tank (303), it enters the ninth delivery pump (304). When the content of diglycerides in the produced product is low, the material after the reaction in the second reaction unit (3) directly enters the first separation unit (4). When the diglyceride content in the produced product is moderate, the material after being reacted in the second reaction unit (3) re-enters the dehydration unit (2) and the second reaction unit (3) for further reaction, and after the material is reacted again, it enters the first separation unit (4); When the product has a high content of diglycerides, the material after being reacted in the second reaction unit (3) enters the first reaction unit (1), the dehydration unit (2), and the second reaction unit (3) again. After the material is reacted again, it enters the first separation unit (4). S4. The material is fed into the semi-finished product tank (401) through the ninth delivery pump (304), and after being evaporated by the second thin film evaporator (403) and distilled by the first distiller (406) and the second distiller (409), it enters the by-product tank and the first crude product tank (501). When the diglyceride content in the crude product produced by the first separation unit (4) cannot meet the production requirements, the second separation unit (10) needs to be added to further purify the crude product in the first separation unit (4). S5. The material in the first crude product tank (501) enters the adsorption unit (6) for adsorption treatment, and after adsorption treatment, it enters the first crude finished product tank (701). S6. The material in the first crude finished product tank (701) enters the deodorization unit (8) for deodorization treatment, and after deodorization treatment, it enters the first finished product tank (901) to complete the production of diglyceride oil.
10. The diglyceride oil production system according to claim 9, characterized in that, The first heat exchanger (102) is heated to 50~70℃; the evaporation surface temperature of the first thin film evaporator (203) is 90~110℃; the second heat exchanger (202) is heated to 80~90℃; the third heat exchanger (206) is cooled to 50~70℃; the evaporation surface temperature of the second thin film evaporator (403) is 120~170℃; the evaporation surface temperature of the first distillation apparatus (406) is 200~250℃; and the evaporation surface temperature of the second distillation apparatus (409) is 290~295℃.
Citation Information
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