A kind of production device and method of natural butyl decalactone fragrance

Abstract

The invention discloses a production device and method of natural butyl-decanolide fragrance, belonging to the technical field of fragrance production. The method comprises the following steps: respectively adding natural amyl alcohol and hydrochloric acid to a chlorination reaction kettle, heating the kettle for chlorination reaction, adjusting the pH value to be neutral, separating a water layer, and obtaining chloropentane; adding tetrahydrofuran, bromopentane, and a magnesium strip under nitrogen, then successively dropping chloropentane and furfural for Grignard reaction, and distilling and recovering tetrahydrofuran after neutralization and water washing to obtain 2-furanyl hexanol; reacting deionized water and 2-furanyl hexanol under high temperature and high pressure conditions, and then performing hydrogenation reaction to obtain pentylcyclopentanone, oxidizing the pentylcyclopentanone, and separating and purifying to obtain a natural butyl-decanolide fragrance product. The method uses natural amyl alcohol and biomass-based furfural as main raw materials, and prepares the natural butyl-decanolide fragrance after chlorination reaction, Grignard reaction, and the like. The process flow is relatively short, the raw materials are easily available, the total yield is improved, and the production cost can be effectively reduced.

Description

Technical Field

[0001] The invention relates to the technical field of perfume production, in particular to a production device and method of natural butyl decalactone perfume. Background Art

[0002] Natural butyl-decanoic acid lactone is widely used in daily chemical flavors, such as margarine, various pastry flavors, and some daily chemical flavors and tobacco flavors. The existing production of natural butyl-decanoic acid lactone mainly adopts the following two methods: one is to react cyclohexanedione with n-hexane bromide, and then oxidize, reduce and cyclize to obtain δ-decanoic acid lactone. The synthesis process of this method is relatively cumbersome and the yield is low; the other is to use diethyl glutarate for Dickmann condensation reaction, and then use anhydrous potassium carbonate in acetone to react with n-heptane bromide, and then deacidify and oxidize to obtain δ-decanoic acid lactone. This method has reasonable cost, but the steps are long and the yield is not high. Summary of the invention

[0003] The object of the present invention is to provide a production device and method for natural butyl-decanoic acid fragrance to solve the problems raised in the above background technology.

[0004] To achieve the above object, the present invention provides the following technical solutions:

[0005] A production device for natural butyl-decanolide fragrance, comprising a chlorination reaction kettle and a Grignard reaction kettle, wherein the chlorination reaction kettle and the Grignard reaction kettle are respectively provided with a graphite condenser A and a graphite condenser B, and a hydrochloric acid absorption liquid receiving tank is respectively connected to the chlorination reaction kettle and the Grignard reaction kettle through the graphite condenser A and the graphite condenser B;

[0006] The chlorination reaction kettle is fixedly connected with a natural amyl alcohol high-level tank and a hydrochloric acid high-level tank through a pipeline. The chlorination reaction kettle is connected to the static kettle through a material pump and a pipeline. The top of the static kettle is connected to the sodium bicarbonate solution high-level tank through a pipeline. The bottom of the static kettle is connected to the distillation kettle A through a material pump and a pipeline. The distillation kettle tower section on the distillation kettle A is connected to the spiral plate heat exchanger A through a pipeline.

[0007] The chloropentane vacuum receiving tank is connected to the spiral plate heat exchanger A through a pipeline, and the chloropentane vacuum receiving tank is connected to the chloropentane high-level tank through a material pump;

[0008] The natural amyl alcohol vacuum receiving tank is connected to the spiral plate heat exchanger A through a pipeline, and the natural amyl alcohol vacuum receiving tank is connected to the natural amyl alcohol high-level tank through a material pump; the bromopentane high-level tank and the tetrahydrofuran high-level tank are respectively connected to the Grignard reactor through pipelines, and the chloropentane high-level tank and the furfural high-level tank are respectively connected to the Grignard reactor through a dripping pump A;

[0009] The water washing kettle A is connected to the Grignard reactor through a material pump, and the water washing kettle A is connected to the sodium hydroxide solution high-level tank through a pipeline; the distillation kettle B is connected to the water washing kettle A through a material pump, and the distillation kettle B is connected to the spiral plate heat exchanger B through the distillation kettle tower section; the 2-furanyl hexanol vacuum receiving tank is connected to the spiral plate heat exchanger B through pipelines, and the 2-furanyl hexanol vacuum receiving tank is connected to the high-pressure reactor through a material pump; the tetrahydrofuran vacuum receiving tank is connected to the spiral plate heat exchanger B through a pipeline, and the tetrahydrofuran vacuum receiving tank is connected to the tetrahydrofuran high-level tank through a material pump; the hydrogenation reactor is connected to the petroleum ether high-level tank through a pipeline, and the hydrogenation reactor is connected to the high-pressure reactor through a material pump, and the hydrogenation reactor is provided with an automatic backwashing filter and is connected to the petroleum ether high-level tank and the distillation kettle C through the automatic backwashing filter;

[0010] The bottom of the hydrogenation reactor is connected to the high-pressure reactor through a material pump; the pentylcyclopentanone vacuum receiving tank is connected to the distillation kettle C through a spiral plate heat exchanger C, and the pentylcyclopentanone vacuum receiving tank is connected to the pentylcyclopentanone high-level tank through a material pump; the petroleum ether vacuum receiving tank is connected to the distillation kettle C through a spiral plate heat exchanger C, and the petroleum ether vacuum receiving tank is connected to the petroleum ether high-level tank through a material pump; the pentylcyclopentanone high-level tank and the sulfuric acid high-level tank are respectively connected to the oxidation reactor through pipelines; the peracetic acid high-level tank is connected to the oxidation reactor through a drip pump B; the washing kettle B is respectively connected to the oxidation reactor and the distillation kettle through material pumps; the product vacuum receiving tank is connected to the distillation kettle through a distillation tower spiral plate heat exchanger, and the product vacuum receiving tank is connected to the product temporary storage tank through a pipeline.

[0011] As a further solution of the present invention: the automatic backwash filter is connected to the hydrogenation reactor through a U-shaped elbow, the material is pressed from the hydrogenation reactor to the automatic backwash filter, the liquid phase material is transferred to the distillation kettle C, and the solid phase hydrogenation catalyst uses nitrogen pressure to pressurize the petroleum ether in the petroleum ether high-level tank into the hydrogenation reactor for backwashing.

[0012] As a further solution of the present invention: the distillation towers on the distillation kettles A, B and C are all filled with cy500 stainless steel corrugated packing, and the distillation tower on the distillation kettle is filled with cy700 stainless steel corrugated packing.

[0013] The present invention also provides a method for producing natural butyl-decanoic acid flavor, comprising the following steps:

[0014] S1: add natural amyl alcohol and 35% hydrochloric acid from the natural amyl alcohol high-level tank and the hydrochloric acid high-level tank to the chlorination reactor respectively, open the steam valve of the chlorination reactor and stir, heat the chlorination reactor to 80-120°C, react for 12-24 hours, and the hydrogen chloride gas generated by the volatilization of hydrochloric acid during the reaction is condensed by graphite condenser A and collected in the hydrochloric acid absorption liquid receiving tank;

[0015] S2: After the reaction is completed, the material obtained in step S1 is transferred to a static kettle, and 5% sodium bicarbonate solution is metered into the static kettle from the sodium bicarbonate solution high-level tank, and the pH value of the reaction solution is adjusted to 7-8, and the reaction solution is allowed to stand for 2-4 hours. The water layer is separated and sent to the sewage treatment station for wastewater treatment, and the oil layer is transferred to the distillation kettle A;

[0016] S3: Open the steam valve of distillation kettle A, start the vacuum pump, raise the temperature to 60-80°C, and recover the unreacted natural amyl alcohol under the vacuum pressure of 3000-6666Pa. After condensation by spiral plate heat exchanger A, the natural amyl alcohol is transferred to the natural amyl alcohol high-level tank by the material pump through the natural amyl alcohol vacuum receiving tank for recovery and application. When the top temperature of the tower drops or no material is discharged from the top of the tower, the recovery of natural amyl alcohol is completed, and then the distillation kettle A is heated to 80-100°C, and the chloropentane is collected under the vacuum pressure of 3000-6666Pa. After condensation by spiral plate heat exchanger A, the chloropentane is transferred to the bromopentane high-level tank by the material pump through the chloropentane vacuum receiving tank;

[0017] S4: Under nitrogen protection and strong stirring conditions, bromopentane and tetrahydrofuran are metered into the Grignard reactor from the bromopentane header tank and the tetrahydrofuran header tank, respectively, and then magnesium strips are metered into the Grignard reactor from the hand hole, and the reaction temperature is controlled at 25±5°C;

[0018] S5: raising the temperature of the Grignard reactor in step S4 to 60-80° C., and adding chloropentane from the chloropentane header tank to the Grignard reactor by a dropping pump A, with the dropping time controlled at 4-8 hours;

[0019] S6: After the addition of chloropentane is completed, the temperature of the Grignard reactor in step S5 is lowered to 25±5° C., and furfural is metered into the Grignard reactor from the furfural header tank via a dropping pump A, and the dropping time is controlled to be 4 to 8 hours;

[0020] S7: Transfer the reaction liquid of step S6 to the water washing kettle A, add 2% sodium hydroxide solution from the sodium hydroxide solution high-level tank 19 to the water washing kettle A, adjust the pH of the reaction liquid to neutral, separate the water layer, add clean water to the oil layer and wash it twice, stir for 2 hours each time and then stand for 2 hours to separate the water layer, and transfer the water layer to the sewage treatment station for treatment;

[0021] S8: transferring the oil layer obtained in step S7 to a distillation kettle B, opening the steam valve of the distillation kettle B, heating the distillation kettle to 60-70° C., recovering tetrahydrofuran at normal pressure, condensing the tetrahydrofuran through a spiral plate heat exchanger B, and transferring the tetrahydrofuran to a tetrahydrofuran high-level tank by a material pump for recovery and application. When the temperature at the top of the tower drops or no material is discharged from the top of the tower, the recovery of tetrahydrofuran is completed, and then the distillation kettle is heated to 80-120° C., and the vacuum pump is opened. 2-furanylhexanol is collected under a vacuum pressure of 3000-6667 Pa, and condensed by a spiral plate heat exchanger B, and then transferred to a high-pressure reactor by a material pump through a 2-furanylhexanol vacuum receiving tank;

[0022] S9: add deionized water to the high-pressure reactor, open the stirring and steam valves, raise the temperature to 120-150°C, control the reactor pressure at 0.5-1.0 MPa, and react for 10-20 hours. After cooling, transfer the reaction liquid to the hydrogenation reactor through a material pump;

[0023] S10: Petroleum ether is metered into the hydrogenation reactor from the petroleum ether high-level tank. After the nitrogen replacement is qualified, hydrogen is introduced for hydrogenation. The hydrogenation reaction pressure is controlled at 1.0-1.6 MPa and the reaction temperature is 30±2°C. The hydrogenation reaction is terminated after 24-40 hours of reaction time. After the nitrogen replacement is qualified, p-toluenesulfonic acid is metered into the reactor through the hand hole. The reactor is heated to 80-120°C. The reaction time is 4-8 hours. After the reaction is completed, the reaction fluid is sent to the distillation kettle C through the automatic backwashing filter by nitrogen pressure. The solid-phase hydrogenation catalyst is backwashed by the pressure of the petroleum ether high-level tank into the hydrogenation reactor for application;

[0024] S11: Open the steam valve of the distillation kettle C, raise the temperature to 60-90°C, recover petroleum ether at normal pressure, condense it through the spiral plate heat exchanger C, and transfer it to the petroleum ether high-level tank by the material pump through the petroleum ether vacuum receiving tank for recovery and application. When the temperature at the top of the tower drops or no material is discharged from the top of the tower, the recovery of petroleum ether is completed, and then the distillation kettle is heated to 70-120°C, and the vacuum pump is turned on. Under the condition of vacuum pressure of 1333-3333Pa, pentylcyclopentanone is collected, condensed it through the spiral plate heat exchanger C, and transferred it to the pentylcyclopentanone high-level tank by the material pump through the pentylcyclopentanone vacuum receiving tank;

[0025] S12: adding pentylcyclopentanone and sulfuric acid from the pentylcyclopentanone header tank and the sulfuric acid header tank to the oxidation reactor, then controlling the reactor temperature at 20-40° C., and dripping peracetic acid from the peracetic acid header tank to the oxidation reactor through a dripping pump B, and controlling the dripping time to be 10-20 hours;

[0026] S13: After the oxidation reaction is completed, the reaction solution obtained in step S12 is transferred to a water washing kettle B, and washed twice with clean water. After stirring for 2 hours each time, the mixture is allowed to stand for 2 hours to separate the water layer, which is transferred to a sewage treatment station for treatment, and the oil layer is transferred to a distillation kettle;

[0027] S14: Open the steam valve of the distillation kettle, start the high vacuum, raise the temperature to 80~120℃, collect butyl-decanoic acid under the vacuum pressure of 1333~3000Pa, condense it in the spiral plate heat exchanger of the distillation tower, pass through the product vacuum receiving tank, collect it in the product temporary storage tank, and obtain the natural butyl-decanoic acid fragrance product.

[0028] As a further solution of the present invention: the mass ratio of the natural amyl alcohol to 35% hydrochloric acid is 1:0.5-1:1.5, and the preferred mass ratio is 1:0.9-1:1.1.

[0029] As a further embodiment of the present invention, the mass ratio of the magnesium rod, tetrahydrofuran and bromopentane is 1-10:1-10:1, preferably 7.5-10:7.5-10:1, and the molar ratio of furfural and chloropentane is 1:0.5-1:1.5, preferably 1:0.9-1:1.1.

[0030] As a further solution of the present invention: the mass ratio of the 2-furanylhexanol to deionized water is 1:5-1:20, preferably 1:10-1:15; the volume ratio of petroleum ether to the reaction liquid used in the hydrogenation reaction is 1:1-10, preferably 1:3-1:5.

[0031] As a further embodiment of the present invention, the mass ratio of the peracetic acid to pentylcyclopentanone is 1:1-1:10, preferably 1:1.5-1:2.0; when sulfuric acid is added, the mass ratio of sulfuric acid to peracetic acid is 1-10:1, preferably 1:7.5-10.

[0032] Compared with the prior art, the beneficial effects of the present invention are as follows: the present invention uses natural amyl alcohol and biomass-based furfural as main raw materials, and produces natural butyl-decanoic acid lactone fragrance after chlorination reaction, Grignard reaction and other reactions, with lower cost and higher yield, and adopts automatic backwashing filtration technology to realize solid-liquid separation of hydrogenation catalyst filtration operation, and the process flow is relatively simple and the operation is easier. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 is a flowchart of the method of the present invention;

[0034] Figure 2 It is a schematic diagram of the device structure of the present invention.

[0035] In the figure: 1, chlorination reaction kettle; 2, natural amyl alcohol high-level tank; 3, hydrochloric acid high-level tank; 4-1, graphite condenser A; 5, hydrochloric acid absorption liquid receiving tank; 6, static kettle; 7, sodium bicarbonate solution high-level tank; 8, distillation kettle A; 9, spiral plate heat exchanger A; 10, chloropentane vacuum receiving tank; 11, natural amyl alcohol vacuum receiving tank; 12, Grignard reaction kettle; 4-2, graphite condenser B; 13, bromopentane high-level tank; 14, chloropentane high-level tank; 15, tetrahydrofuran high-level tank; 16, furfural high-level tank; 17, dripping pump A; 18, water washing kettle A; 19, sodium hydroxide solution high-level tank; 20, distillation kettle B; 21, spiral plate heat exchanger Heater B; 22. 2-furanylhexanol vacuum receiving tank; 23. Tetrahydrofuran vacuum receiving tank; 24. High-pressure reactor; 25. Hydrogenation reactor; 26. Automatic backwash filter; 27. Petroleum ether high-level tank; 28. Distillation kettle C; 29. ​​Spiral plate heat exchanger C; 30. Pentylcyclopentanone vacuum receiving tank; 31. Petroleum ether vacuum receiving tank; 32. Oxidation reactor; 33. Pentylcyclopentanone high-level tank; 34. Sulfuric acid high-level tank; 35. Peracetic acid high-level tank; 36. Drip pump B; 37. Water washing kettle B; 38. Distillation kettle; 39. Distillation tower spiral plate heat exchanger; 40. Product vacuum receiving tank; 41. Product temporary storage tank. DETAILED DESCRIPTION

[0036] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0037] See also Figure 1-2 In an embodiment of the present invention, a production device for natural butyl-decanolide fragrance includes a chlorination reaction kettle 1 and a Grignard reaction kettle 12, wherein the chlorination reaction kettle 1 and the Grignard reaction kettle 12 are respectively provided with a graphite condenser A4-1 and a graphite condenser B4-2, and a hydrochloric acid absorption liquid receiving tank 5 is respectively connected to the chlorination reaction kettle 1 and the Grignard reaction kettle 12 through the graphite condenser A4-1 and the graphite condenser B4-2;

[0038] The chlorination reaction kettle 1 is fixedly connected to the natural amyl alcohol high-level tank 2 and the hydrochloric acid high-level tank 3 through a pipeline, the chlorination reaction kettle 1 is connected to the static kettle 6 through a material pump and a pipeline, the top of the static kettle 6 is connected to the sodium bicarbonate solution high-level tank 3 through a pipeline, the bottom of the static kettle 6 is connected to the distillation kettle A8 through a material pump and a pipeline, and the distillation kettle tower section on the distillation kettle A8 is connected to the spiral plate heat exchanger 9 through a pipeline;

[0039] The chloropentane vacuum receiving tank 10 is connected to the spiral plate heat exchanger A9 through a pipeline, and the chloropentane vacuum receiving tank 10 is connected to the chloropentane high-level tank 14 through a material pump;

[0040] The natural amyl alcohol vacuum receiving tank 11 is connected to the spiral plate heat exchanger A9 through a pipeline, and the natural amyl alcohol vacuum receiving tank 11 is connected to the natural amyl alcohol high-level tank 2 through a material pump; the bromopentane high-level tank 13 and the tetrahydrofuran high-level tank 15 are respectively connected to the Grignard reactor 12 through pipelines, and the chloropentane high-level tank 14 and the furfural high-level tank 16 are respectively connected to the Grignard reactor 12 through a drip pump A17;

[0041] The washing kettle A18 is connected to the Grignard reactor 12 through a material pump, and the washing kettle A18 is connected to the sodium hydroxide solution high-level tank 19 through a pipeline; the distillation kettle B20 is connected to the washing kettle A18 through a material pump, and the distillation kettle B20 is connected to the spiral plate heat exchanger B21 through a distillation kettle tower section; the 2-furanyl hexanol vacuum receiving tank 22 is connected to the spiral plate heat exchanger B21 through pipelines, and the 2-furanyl hexanol vacuum receiving tank 22 is connected to the high-pressure reactor 24 through a material pump; the tetrahydrofuran vacuum receiving tank 23 is connected to the spiral plate heat exchanger B21 through a pipeline, and the tetrahydrofuran vacuum receiving tank 23 is connected to the tetrahydrofuran high-level tank 15 through a material pump; the hydrogenation reactor 25 is connected to the petroleum ether high-level tank 27 through a pipeline, and the hydrogenation reactor 25 is connected to the high-pressure reactor 24 through a material pump, and the hydrogenation reactor 25 is provided with an automatic backwashing filter 26 and is connected to the petroleum ether high-level tank 27 and the distillation kettle C28 through the automatic backwashing filter 26;

[0042] The bottom of the hydrogenation reactor 25 is connected to the high-pressure reactor 24 through a material pump; the pentylcyclopentanone vacuum receiving tank 30 is connected to the distillation kettle C28 through a spiral plate heat exchanger C29, and the pentylcyclopentanone vacuum receiving tank 30 is connected to the pentylcyclopentanone high-level tank 33 through a material pump; the petroleum ether vacuum receiving tank 31 is connected to the distillation kettle C28 through a spiral plate heat exchanger C29, and the petroleum ether vacuum receiving tank 31 is connected to the petroleum ether high-level tank 27 through a material pump; the pentylcyclopentanone high-level tank 33 and the sulfuric acid high-level tank 34 are respectively connected to the oxidation reactor 32 through pipelines; the peracetic acid high-level tank 35 is connected to the oxidation reactor 32 through a drip pump B36; the washing kettle B37 is respectively connected to the oxidation reactor 32 and the distillation kettle 38 through material pumps; the product vacuum receiving tank 40 is connected to the distillation kettle 38 through a distillation tower spiral plate heat exchanger 39, and the product vacuum receiving tank 40 is connected to the product temporary storage tank 41 through a pipeline.

[0043] Working principle of the present invention:

[0044] First, natural amyl alcohol and 35% hydrochloric acid are metered into the chlorination reaction kettle 1 from the natural amyl alcohol high-level tank 2 and the hydrochloric acid high-level tank 3, respectively, the steam valve of the chlorination reaction kettle 1 is opened and stirred, the chlorination reaction kettle 1 is heated to 80-120° C., and the reaction is carried out for 12-24 hours. During the reaction, the hydrogen chloride gas generated by the volatilization of the hydrochloric acid is condensed by the graphite condenser A4-1 and then collected in the hydrochloric acid absorption liquid receiving tank 5;

[0045] After the reaction is completed, the material obtained in step S1 is transferred to the static kettle 6, and 5% sodium bicarbonate solution is metered into the static kettle 6 from the sodium bicarbonate solution high-level tank 7, and the pH value of the reaction solution is adjusted to 7-8, and the reaction solution is allowed to stand for 2 to 4 hours. The water layer is separated and sent to the sewage treatment station for wastewater treatment, and the oil layer is transferred to the distillation kettle A8;

[0046] Open the steam valve of the distillation kettle A8, start the vacuum pump, raise the temperature to 60-80° C., and under the condition of vacuum pressure of 3000-6666Pa, recover the unreacted natural amyl alcohol, condense it through the spiral plate heat exchanger A9, pass through the natural amyl alcohol vacuum receiving tank 11, and transfer it to the natural amyl alcohol high-level tank 2 by the material pump for recovery and application. When the tower top temperature drops or no material is discharged from the tower top, the recovery of natural amyl alcohol is completed, and then the distillation kettle A8 is heated to 80-100° C., and under the condition of vacuum pressure of 3000-6666Pa, chloropentane is collected, and after condensation by the spiral plate heat exchanger A9, it is transferred to the bromopentane high-level tank 13 by the material pump through the chloropentane vacuum receiving tank 10;

[0047] Under nitrogen protection and strong stirring, bromopentane and tetrahydrofuran are metered into the Grignard reactor 12 from the bromopentane high-level tank 13 and the tetrahydrofuran high-level tank 15, respectively, and then magnesium bars are metered into the hand hole of the Grignard reactor 12 to control the reaction temperature at 25±5°C;

[0048] The temperature of the Grignard reactor 12 in step S4 is raised to 60-80° C., and chloropentane is metered into the Grignard reactor 12 from the chloropentane header tank 14 through a drip pump A17, and the dripping time is controlled to be 4-8 hours;

[0049] After the addition of chloropentane is completed, the temperature of the Grignard reactor 12 in step S5 is lowered to 25±5° C., and furfural is metered into the Grignard reactor 12 from the furfural header tank 16 through a drip pump A17, and the dripping time is controlled to be 4 to 8 hours;

[0050] The reaction liquid of step S6 is transferred to the water washing kettle A18, and 2% sodium hydroxide solution is added to the water washing kettle A18 from the sodium hydroxide solution high-level tank 19, and the pH of the reaction liquid is adjusted to be neutral. The separated water layer is then washed twice with clean water added to the oil layer, and each time it is stirred for 2 hours and then allowed to stand for 2 hours to separate the water layer, and the water layer is transferred to the sewage treatment station for treatment;

[0051] The oil layer obtained in step S7 is transferred to the distillation kettle B20, the steam valve of the distillation kettle B20 is opened, the temperature is raised to 60-70° C., tetrahydrofuran is recovered at normal pressure, and after condensation by the spiral plate heat exchanger B21, it is transferred to the tetrahydrofuran high-level tank 15 by a material pump for recovery and application through a tetrahydrofuran vacuum receiving tank. When the tower top temperature drops or no material is discharged from the tower top, the recovery of tetrahydrofuran is completed, the distillation kettle is heated to 80-120° C., the vacuum pump is opened, and 2-furanylhexanol is collected under a vacuum pressure of 3000-6667Pa. After condensation by the spiral plate heat exchanger B21, it is transferred to the high-pressure reactor 24 by a material pump through a 2-furanylhexanol vacuum receiving tank;

[0052] Deionized water is added to the high-pressure reactor 24, and the stirring and steam valves are opened. The temperature is raised to 120-150° C., and the pressure of the reactor is controlled at 0.5-1.0 MPa. The reaction time is 10-20 hours. After cooling, the reaction liquid is transferred to the hydrogenation reactor 25 through a material pump;

[0053] Petroleum ether is metered into the hydrogenation reactor 25 from the petroleum ether high-level tank 27. After the nitrogen replacement is qualified, hydrogen is introduced for hydrogenation. The hydrogenation reaction pressure is controlled at 1.0-1.6MPa and the reaction temperature is 30±2°C. The hydrogenation reaction is terminated after 24-40 hours of reaction time. After the nitrogen replacement is qualified, p-toluenesulfonic acid is metered into the reactor through the hand hole. The reactor is heated to 80-120°C and the reaction time is 4-8 hours. After the reaction is completed, the reaction fluid is sent to the distillation kettle C28 through the automatic backwashing filter 26 by nitrogen pressure. The solid-phase hydrogenation catalyst is backwashed by the pressure of the petroleum ether high-level tank 27 and enters the hydrogenation reactor 25 for application;

[0054] Open the steam valve of the distillation kettle C28, raise the temperature to 60-90°C, recover petroleum ether at normal pressure, condense it through the spiral plate heat exchanger C29, and transfer it to the petroleum ether high-level tank 27 by the material pump for recovery and application. When the temperature at the top of the tower drops or there is no material at the top of the tower, the recovery of petroleum ether is completed, and then the distillation kettle is heated to 70-120°C, and the vacuum pump is turned on. Under the condition of vacuum pressure of 1333-3333Pa, pentylcyclopentanone is collected, condensed it through the spiral plate heat exchanger C29, and transferred it to the pentylcyclopentanone high-level tank 33 by the material pump through the pentylcyclopentanone vacuum receiving tank;

[0055] Add pentylcyclopentanone and sulfuric acid from the pentylcyclopentanone high-level tank 33 and the sulfuric acid high-level tank 34 to the oxidation reaction kettle 32, then control the temperature of the reaction kettle at 20-40° C., and drip peracetic acid from the peracetic acid high-level tank 35 to the oxidation reaction kettle 32 through a drip pump B36, and the dripping time is controlled to be 10-20 hours;

[0056] After the oxidation reaction is completed, the reaction solution obtained in step S12 is transferred to a water washing kettle B37, and washed twice with clean water. After stirring for 2 hours each time, the mixture is allowed to stand for 2 hours to separate the water layer, which is then transferred to a sewage treatment station for treatment, and the oil layer is transferred to a distillation kettle 38;

[0057] Open the steam valve of the distillation kettle 38, start the high vacuum, raise the temperature to 80-120°C, collect butyl-decanoic acid under the vacuum pressure of 1333-3000Pa, condense it through the distillation tower spiral plate heat exchanger 39, pass through the product vacuum receiving tank 40, collect it in the product temporary storage tank 41, and obtain the natural butyl-decanoic acid fragrance product.

[0058] The natural butyl-decanolide fragrance product prepared by the invention has the following GC detection conditions: chromatographic column HP-5 (30m x 0.32mm x 0.25um); detector FID, temperature 250°C; injection: injection volume about 0.2ul, split ratio 1:100, injection port temperature 250°C; carrier gas: N2, flow rate 20L / min, column front pressure 34.47kPa; chromatographic oven temperature: linear program temperature rise from 80°C to 220°C, rate 10°C / min, retention 20min.

[0059] The natural butyl decanolactone flavor detected has a coconut-like aroma, and a creamy aroma at low concentrations after dilution. The purity of the product is 98.53% by gas chromatography analysis, the refractive index (20°C) is 1.457, the relative density (25°C) is 0.968, and the naturalness is 99% bio-based carbon by isotope mass spectrometry C14.

[0060] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Although the present invention has been disclosed as a preferred embodiment as above, it is not used to limit the present invention. Any technical personnel in this field can make some changes or modify the technical contents disclosed above into equivalent embodiments without departing from the scope of the technical solution of the present invention. However, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention without departing from the content of the technical solution of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A method for producing natural butyl-decanoic acid fragrance, characterized in that: The following steps are involved: Step 1: natural amyl alcohol and 35% hydrochloric acid are added to a chlorination reaction kettle (1), the temperature is raised to carry out a chlorination reaction, the pH of the reaction solution is adjusted to neutral with a sodium bicarbonate solution, and the water layer is separated to obtain chloropentane; Step 2: under nitrogen protection, tetrahydrofuran and pentyl bromide are added to a Grignard reaction kettle (12), and then a magnesium bar is added to react to obtain a Grignard reagent, and then pentyl chloride and furfural are added dropwise in sequence to carry out a Grignard reaction. After neutralization and water washing, tetrahydrofuran is recovered by distillation to obtain 2-furanylhexanol; Step 3: adding deionized water and 2-furanylhexanol into a high-pressure reactor (24), reacting under high temperature and high pressure conditions to obtain oxopentylcyclopentenol, and then introducing hydrogen to carry out hydrogenation reaction to obtain pentylcyclopentanone; Step 4: using peracetic acid as an oxidant to carry out an oxidation reaction on amylcyclopentanone, and obtaining a natural butyl-decanolide fragrance product after a series of separation and purification.

2. The method for producing a natural butyl-decanoic acid fragrance according to claim 1, characterized in that: In step 1, the mass ratio of the natural amyl alcohol to 35% hydrochloric acid is 1:0.5 to 1:1.

5.

3. The method for producing a natural butyl-decanoic acid fragrance according to claim 1, characterized in that: In step 2, the mass ratio of the magnesium bar, tetrahydrofuran and bromopentane is 1-10:1-10:1, and the molar ratio of furfural and chloropentane is 1:0.5-1:1.

5.

4. The method for producing a natural butyl-decanolide fragrance according to claim 1, characterized in that: In step three, the mass ratio of the 2-furanylhexanol to deionized water is 1:5 to 1:

20.

5. The method for producing a natural butyl-decanolide fragrance according to claim 1, characterized in that: In step 4, the mass ratio of the peracetic acid to pentylcyclopentanone is 1:1 to 1:

10.

6. A production device for natural butyl-decanoic acid flavor, comprising a chlorination reactor (1) and a Grignard reactor (12), characterized in that: A graphite condenser A (4-1) and a graphite condenser B (4-2) are respectively provided on the chlorination reaction kettle (1) and the Grignard reaction kettle (12); and a hydrochloric acid absorption liquid receiving tank (5) is connected to the chlorination reaction kettle (1) and the Grignard reaction kettle (12) via the graphite condenser A (4-1) and the graphite condenser B (4-2); The chlorination reaction kettle (1) is fixedly connected to a natural amyl alcohol high-level tank (2) and a hydrochloric acid high-level tank (3) through a pipeline. The chlorination reaction kettle (1) is connected to a static kettle (6) through a material pump and a pipeline. The top of the static kettle (6) is connected to a sodium bicarbonate solution high-level tank (7) through a pipeline. The bottom of the static kettle (6) is connected to a distillation kettle A (8) through a material pump and a pipeline. The distillation kettle tower section on the distillation kettle A (8) is connected to a spiral plate heat exchanger A (9) through a pipeline. The chloropentane vacuum receiving tank (10) is connected to the spiral plate heat exchanger A (9) via a pipeline, and the chloropentane vacuum receiving tank (10) is connected to the chloropentane high-level tank (14) via a material pump; The natural amyl alcohol vacuum receiving tank (11) is connected to the spiral plate heat exchanger A (9) through a pipeline, and the natural amyl alcohol vacuum receiving tank (11) is connected to the natural amyl alcohol high-level tank (2) through a material pump; the bromopentane high-level tank (13) and the tetrahydrofuran high-level tank (15) are respectively connected to the Grignard reactor (12) through pipelines, and the chloropentane high-level tank (14) and the furfural high-level tank (16) are respectively connected to the Grignard reactor (12) through a drip pump A (17); The water washing kettle A (18) is connected to the Grignard reactor (12) through a material pump, and the water washing kettle A (18) is connected to the sodium hydroxide solution high-level tank (19) through a pipeline; the distillation kettle B (20) is connected to the water washing kettle A (18) through a material pump, and the distillation kettle B (20) is connected to the spiral plate heat exchanger B (21) through a distillation kettle tower section; the 2-furanylhexanol vacuum receiving tank (22) is connected to the spiral plate heat exchanger B (21) through a pipeline, and the 2-furanylhexanol vacuum receiving tank (22) is connected to the high-pressure reactor (24) through a material pump; The tetrahydrofuran vacuum receiving tank (23) is connected to the spiral plate heat exchanger B (21) through a pipeline, and the tetrahydrofuran vacuum receiving tank (23) is connected to the tetrahydrofuran high-level tank (15) through a material pump; the hydrogenation reactor (25) is connected to the petroleum ether high-level tank (27) through a pipeline, and the hydrogenation reactor (25) is connected to the high-pressure reactor (24) through a material pump. The hydrogenation reactor (25) is equipped with an automatic backwashing filter (26) and is connected to the petroleum ether high-level tank (27) and the distillation kettle C (28) through the automatic backwashing filter (26); The bottom of the hydrogenation reactor (25) is connected to the high-pressure reactor (24) via a material pump; the pentylcyclopentanone vacuum receiving tank (30) is connected to the distillation kettle C (28) via a spiral plate heat exchanger C (29), and the pentylcyclopentanone vacuum receiving tank (30) is connected to the pentylcyclopentanone high-level tank (33) via a material pump; the petroleum ether vacuum receiving tank (31) is connected to the distillation kettle C (28) via a spiral plate heat exchanger C (29), and the petroleum ether vacuum receiving tank (31) is connected to the petroleum ether high-level tank (27) via a material pump; The cyclopentanone high-level tank (33) and the sulfuric acid high-level tank (34) are respectively connected to the oxidation reaction kettle (32) through pipelines; the peracetic acid high-level tank (35) is connected to the oxidation reaction kettle (32) through a drip pump B (36); the water washing kettle B (37) is respectively connected to the oxidation reaction kettle (32) and the distillation kettle (38) through a material pump; the product vacuum receiving tank (40) is connected to the distillation kettle (38) through a distillation tower spiral plate heat exchanger (39), and the product vacuum receiving tank (40) is connected to the product temporary storage tank (41) through a pipeline.

7. The production device of a natural butyl-decanoic acid fragrance according to claim 6, characterized in that: The automatic backwash filter (26) is connected to the hydrogenation reactor (25) via a U-shaped elbow, and the material is pressed from the hydrogenation reactor (25) to the automatic backwash filter (26), and the liquid phase material is transferred to the distillation kettle C (28). The solid phase hydrogenation catalyst uses nitrogen pressure to pressurize the petroleum ether in the petroleum ether high-level tank (27) into the hydrogenation reactor (25) for backwashing.

8. The production device of natural butyl-decanoic acid fragrance according to claim 6, characterized in that: The distillation towers on the distillation kettle A (8), distillation kettle B (20) and distillation kettle C (28) are all filled with CY500 stainless steel corrugated packing, and the distillation tower on the distillation kettle (38) is filled with CY700 stainless steel corrugated packing.

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