CN211445579U - Production device of bisabolol alkene ester spice - Google Patents
Production device of bisabolol alkene ester spice Download PDFInfo
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- CN211445579U CN211445579U CN201922093809.4U CN201922093809U CN211445579U CN 211445579 U CN211445579 U CN 211445579U CN 201922093809 U CN201922093809 U CN 201922093809U CN 211445579 U CN211445579 U CN 211445579U
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Abstract
The utility model discloses a production device of bisabolol ester spice, which adopts nicotinamide and P2S5The production device has a relatively simple process flow, adopts an automatic back-flushing filtration solid acid catalyst, and is easy to separate from a liquid phase reaction system,Does not corrode equipment, has simple post-treatment, and overcomes the problems that the existing liquid acid corrodes the equipment and the acid-containing wastewater pollutes the environment.
Description
Technical Field
The utility model belongs to the technical field of organic synthetic apparatus for producing, concretely relates to apparatus for producing of bisabolol alkene ester perfume material.
Background
Acylthiazoles are flavorants having a nut bean, milk, egg, meat flavor, and are therefore approved for use in nuts, milk-flavored meats, and flavoring essences, and are approved for use in the united states (FEMA accession No. 3328). Although the content of the compound is very low in a food system, the compound can often endow the food with characteristic flavor due to a small threshold value, and can be used in meat and nut essences, wherein the dosage is 0.0002 per mill in beverage, 0.0009 per mill in ice cream, 0.0006 per mill in chewing gum and 0.0014 per mill in candy; meanwhile, the unique structural characteristics of the thiazole ring have good pharmacological activity and antibacterial and antiviral biological activity.
Nicotinamide, also known as nicotinamide, vitamin B3 or vitamin PP, is a water-soluble vitamin belonging to the B group, is a composition of coenzyme I (nicotinamide adenine dinucleotide, NAD) and coenzyme II (nicotinamide adenine dinucleotide phosphate, NADP), nicotinamide moiety in the two coenzyme structures in human body has reversible hydrogenation and dehydrogenation characteristics, plays a hydrogen transfer role in biological oxidation, can promote tissue respiration, biological oxidation process and metabolism, has important significance for maintaining the integrity of normal tissues, particularly skin, digestive tract and nervous system, is used for medicine, food and feed additives, is a nutrient necessary for mammals, can obtain pellagra when the nicotinamide is lack in vivo, and plays a role in improving the metabolism of protein and sugar, and can improve the nutrition of human and animals. Can be used as nutritional additive in cosmetics.
Bisabolol is also called as sweet bisabolol and ledebouriella seseloides, is one of more sesquiterpene compounds existing in nature, has the efficacies of diminishing inflammation, sterilizing, healing ulcer, dissolving gallstone and the like, can protect and cure skin, prevents the skin from being influenced by daily tension, can accelerate the healing process of the skin, is particularly suitable for being used as sensitive skin and body, is widely applied to the formula of personal care (skin and body care solution, after-shave care water and after-sun care products), and becomes a common active ingredient for skin care by adding the characteristics of inflammation resistance, naturalness and safety; the bisabolol has light and pleasant fragrance, is a fixative with good stability, and can be used for animal spice feeding in feed spice catalogue.
In the prior art, the acid catalyst adopted in the esterification reaction is sulfuric acid and the like, which are used as the traditional esterification catalyst, has low price and good catalytic effect and are used up to now, but the acid catalyst seriously corrodes equipment and pollutes the environment by acid-containing wastewater.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a apparatus for producing of bisabolol ester perfume can shorten process flow, improves the productivity of reaction.
The purpose of the utility model can be realized by the following technical scheme:
comprises a stirring pot, a tetrahydrofuran elevated tank, a nicotinamide-tetrahydrofuran solution elevated tank, a substitution reaction kettle, a dropping pump, a washing kettle, a kettle type distillation tower A, a spiral plate heat exchanger A, a tetrahydrofuran/water receiving tank, an ethyl acetate elevated tank, a washing kettle A, an automatic back-flushing filter A, a 10% sodium hydroxide solution elevated tank, a kettle type distillation tower B, a spiral plate heat exchanger B, an ethyl acetate receiving tank A, an absolute ethyl alcohol elevated tank, a cyclization reaction kettle, an ethyl chloroacetate elevated tank, a kettle type distillation tower C, a spiral plate heat exchanger C, an ethanol receiving tank, a washing kettle B, an automatic back-flushing filter B, a 10% sodium carbonate solution elevated tank, a kettle type distillation tower D, a spiral plate heat exchanger D, an ethyl acetate receiving tank B, a methanol elevated tank, an acidification kettle, a 30% hydrochloric acid elevated tank, a dichloromethane elevated tank, a condensation reaction kettle, a spiral plate heat exchanger E, a, A dichloromethane receiving tank, a cyclohexane/water receiving tank, a bisabolol head tank, a cyclohexane head tank, an automatic back-flushing filter C and an industrial chromatographic column;
the stirring pot is respectively connected with the tetrahydrofuran elevated tank and the nicotinamide-tetrahydrofuran solution elevated tank through a pipeline and a pump, and is provided with a hand-hole feeding port of nicotinamide; the substitution reaction kettle is respectively connected with the tetrahydrofuran head tank and the nicotinamide-tetrahydrofuran head tank through a pipeline and a dropping pump, and is provided with a hand-hole feed inlet of P2S 5; the water washing kettle is respectively connected with the substitution reaction kettle and the distillation kettle of the kettle type distillation tower A through a pump; the top and the bottom of a distillation kettle of the kettle-type distillation tower A are respectively connected with the ethyl acetate elevated tank and the washing kettle A through a pipeline and a pump; the tetrahydrofuran/water receiving tank is connected with the top of the kettle-type distillation tower A through a spiral plate heat exchanger A; the washing kettle A is provided with a hand hole feeding port of anhydrous sodium sulfate and is respectively connected with a 10% sodium hydroxide solution elevated tank and an automatic backwashing filter A through a pipeline and a U-shaped pipe in the kettle; the automatic back-washing filter A is respectively connected with a distillation kettle of the kettle-type distillation tower B and an ethyl acetate head tank through a pipeline and a pump; the top and the bottom of the kettle-type distillation tower B are respectively connected with an absolute ethyl alcohol head tank and a cyclization reaction kettle through a pipeline and a pump; the ethyl acetate receiving tank A is respectively connected with the top of the kettle type distillation tower B and the ethyl acetate head tank through a spiral plate heat exchanger B and a pump; the cyclization reaction kettle is respectively connected with an ethyl chloroacetate elevated tank and a kettle-type distillation tower C through a pipeline and a pump; the top and the bottom of the distillation kettle of the kettle-type distillation tower C are respectively connected with the ethyl acetate head tank and the washing kettle B through a pipeline and a pump; the ethanol receiving tank is respectively connected with the top of the kettle-type distillation tower C and the absolute ethanol head tank through a spiral plate heat exchanger C and a pump; the washing kettle B is provided with a hand hole feeding port of anhydrous sodium sulfate and is respectively connected with a 10% sodium carbonate solution elevated tank and an automatic backwashing filter B through a pipeline and a U-shaped pipe in the kettle; the automatic back-flushing filter B is respectively connected with a distillation kettle of the kettle-type distillation tower D and an ethyl acetate head tank through a pipeline and a pump; the top and the bottom of a distillation kettle of the kettle-type distillation tower D are respectively connected with a methanol elevated tank and an acidification kettle through a pipeline and a pump; the ethyl acetate receiving tank B is respectively connected with the top of the kettle-type distillation tower D and the ethyl acetate head tank through a spiral plate heat exchanger D and a pump; the top part of the acidification kettle is respectively connected with a 10% sodium hydroxide solution elevated tank, a 30% hydrochloric acid elevated tank and a dichloromethane elevated tank through pipelines; a condensation reaction kettle with a distillation tower is respectively connected with an acidification kettle and an automatic back-flushing filter through a pump and a U-shaped pipe in the kettle, the condensation reaction kettle is provided with a catalyst feeding hand hole, and the top of the condensation reaction kettle is respectively connected with a bisabolol elevated tank and a cyclohexane elevated tank through pipelines; the dichloromethane receiving tank is respectively connected with the top of the distillation tower of the condensation reaction kettle and the dichloromethane head tank through a spiral plate heat exchanger E and a pump; the cyclohexane/water receiving tank is connected with the top of the distillation tower of the condensation reaction kettle through a spiral plate heat exchanger E; the automatic back-washing filter C is respectively connected with the industrial chromatographic column and the cyclohexane head tank through a pipeline and a pump.
Further, the kettle type distillation tower is filled with cy500 stainless steel corrugated packing.
The utility model has the advantages that:
the utility model provides a 2-pyridyl-4-methylthiazole-5-formic acid bisabolene ester synthetic perfume' S apparatus for producing adopts niacinamide and P2S5 as starting material, obtain thioniacinamide after the substitution reaction, carry out cyclization reaction with 2-chloroacetoacetic acid ethyl ester again and obtained 2-pyridyl-4-methylthiazole-5-formic acid ethyl ester, obtain 2-pyridyl-4-methylthiazole-5-formic acid after saponification, the acidizing, then condense with bisabolol under the effect of solid acid catalyst, purify synthetic 2-pyridyl-4-methylthiazole-5-formic acid bisabolene ester perfume through industry chromatography separation, this apparatus for producing process is brief relatively, adopt automatic back flush to filter solid acid catalyst and have easily with liquid phase reaction system separation, the apparatus for producing is used for the solid acid catalyst, The method has the advantages of no corrosion to equipment and simple post-treatment, overcomes the problems of equipment corrosion caused by the existing liquid acid and environmental pollution caused by acid-containing wastewater, improves selectivity, can be carried out at a lower temperature, saves energy consumption, reduces the occurrence of side reactions, and can greatly improve production efficiency.
Other features and advantages of the present invention will be described in detail in the following detailed description.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a flow chart of a device for producing bisabolol ester perfume of the present invention;
in the drawings, the components represented by the respective reference numerals are listed below:
a stirred pot; 2. a tetrahydrofuran head tank; 3. a nicotinamide-tetrahydrofuran solution head tank; 4. replacing the reaction kettle; 5. a dropping pump; 6. washing the kettle with water; 7. a kettle-type distillation column A; 8. A spiral plate heat exchanger A; 9. a tetrahydrofuran/water receiving tank; 10. an ethyl acetate head tank; 11. washing the kettle A; 12. automatically backwashing the filter A; 13. a 10% sodium hydroxide solution head tank; 14. a still distillation column B; 15. a spiral plate heat exchanger B; 16. an ethyl acetate receiving tank A; 17. an absolute ethyl alcohol head tank; 18. a cyclization reaction kettle; 19. ethyl chloroacetate head tank; 20. a still distillation column C; 21. a spiral plate heat exchanger C; 22. an ethanol receiving tank; 23. washing the kettle B; 24. automatically backwashing the filter B; 25. a 10% sodium carbonate solution head tank; 26. a still distillation column D; 27. a spiral plate heat exchanger D; 28. an ethyl acetate receiving tank B; 29. a methanol head tank; 30. acidifying the kettle; 31. a 30% hydrochloric acid head tank; 32. a dichloromethane head tank; 33. a condensation reaction kettle; 34. a spiral plate heat exchanger E; 35. a dichloromethane receiving tank; 36. a cyclohexane/water receiving tank; 37. a bisabolol head tank; 38. a cyclohexane head tank; 39. automatically backwashing the filter C; 40. an industrial chromatographic column.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by a person of ordinary skill in the art without creative efforts belong to the protection scope of the present invention.
Referring to fig. 1, a device for producing bisabolene ester synthetic flavor comprises a stirring kettle 1, a tetrahydrofuran head tank 2, a nicotinamide-tetrahydrofuran solution head tank 3, a substitution reaction kettle 4, a dropping pump 5, a water washing kettle 6, a kettle-type distillation tower A7, a spiral plate heat exchanger A8, a tetrahydrofuran/water receiving tank 9, an ethyl acetate head tank 10, a washing kettle A11, an automatic backwashing filter A12, a 10% sodium hydroxide solution head tank 13, a kettle-type distillation tower B14, a spiral plate heat exchanger B15, an ethyl acetate receiving tank A16, an anhydrous ethanol head tank 17, a cyclization reaction kettle 18, an ethyl chloroacetate head tank 19, a kettle-type distillation tower C20, a spiral plate heat exchanger C21, an ethanol receiving tank 22, a washing kettle B23, an automatic backwashing filter B24, a 10% sodium carbonate solution head tank 25, a kettle-type distillation tower D26, a spiral plate heat exchanger D27, an ethyl acetate receiving tank B28, a kettle-type distillation tower B24, and a spiral plate heat exchanger B24, Methanol elevated tank 29, acidification tank 30, 30% hydrochloric acid elevated tank 31), dichloromethane elevated tank 32, condensation reaction tank 33, spiral plate heat exchanger E34, dichloromethane receiving tank 35, cyclohexane/water receiving tank 36, bisabolol elevated tank 37, cyclohexane elevated tank 38, automatic backwashing filter C39 and industrial chromatographic column 40;
the stirring pot 1 is respectively connected with the tetrahydrofuran elevated tank 2 and the nicotinamide-tetrahydrofuran solution elevated tank 3 through a pipeline and a pump, and the stirring pot 1 is provided with a hand-hole feeding port of nicotinamide; the substitution reaction kettle 4 is respectively connected with the tetrahydrofuran head tank 2 and the nicotinamide-tetrahydrofuran head tank 3 through a pipeline and a dropping pump 5, and the substitution reaction kettle 4 is provided with a hand-hole feed opening of P2S 5; the water washing kettle 6 is respectively connected with the substitution reaction kettle 4 and a distillation kettle of the kettle type distillation tower A7 through pumps; the top and the bottom of the distillation kettle of the kettle-type distillation tower A7 are respectively connected with the ethyl acetate head tank 10 and the washing kettle A11 through pipelines and pumps; the tetrahydrofuran/water receiving tank 9 is connected with the top of the kettle type distillation tower A7 through a spiral plate heat exchanger A8; the washing kettle A11 is provided with a hand-hole feed opening of anhydrous sodium sulfate, and the washing kettle A11 is respectively connected with the 10% sodium hydroxide solution elevated tank 13 and the automatic backwashing filter A12 through a pipeline and a U-shaped pipe in the kettle; the automatic back-flushing filter A12 is respectively connected with a distillation still of the still distillation tower B14 and the ethyl acetate head tank 10 through a pipeline and a pump; the top and the bottom of the kettle-type distillation tower B14 are respectively connected with the absolute ethyl alcohol head tank 17 and the cyclization reaction kettle 18 through pipelines and pumps; the ethyl acetate receiving tank A16 is respectively connected with the top of the kettle type distillation tower B14 and the ethyl acetate head tank 10 through a spiral plate heat exchanger B15 and a pump; the cyclization reaction kettle 18 is respectively connected with an ethyl chloroacetate elevated tank 19 and a kettle-type distillation tower C20 through a pipeline and a pump; the top and the bottom of the still distillation column C20 are respectively connected with the ethyl acetate head tank 10 and the washing still B23 through pipelines and pumps; the ethanol receiving tank 22 is respectively connected with the top of the kettle-type distillation tower C20 and the absolute ethanol head tank 17 through a spiral plate heat exchanger C21 and a pump; the washing kettle B23 is provided with a hand-hole feed opening of anhydrous sodium sulfate, and the washing kettle B23 is respectively connected with a 10% sodium carbonate solution elevated tank 25 and an automatic backwashing filter B24 through a pipeline and an in-kettle U-shaped pipe; the automatic back-flushing filter B24 is respectively connected with a distillation still of the still distillation tower D26 and the ethyl acetate head tank 10 through a pipeline and a pump; the top and the bottom of the distillation kettle of the kettle-type distillation tower D26 are respectively connected with the methanol elevated tank 29 and the acidification kettle 30 through pipelines and pumps; the ethyl acetate receiving tank B28 is respectively connected with the top of the kettle type distillation tower D26 and the ethyl acetate head tank 10 through a spiral plate heat exchanger D27 and a pump; the top of the acidification kettle 30 is respectively connected with a 10% sodium hydroxide solution elevated tank 13, a 30% hydrochloric acid elevated tank 31 and a dichloromethane elevated tank 32 through pipelines; a condensation reaction kettle 33 with a distillation tower is respectively connected with the acidification kettle 30 and the automatic back-flushing filter 39 through a pump and a U-shaped pipe in the kettle, the condensation reaction kettle 33 is provided with a catalyst feeding hand hole, and the top of the condensation reaction kettle 33 is respectively connected with a bisabolol elevated tank 37 and a cyclohexane elevated tank 38 through pipelines; the dichloromethane receiving tank 35 is respectively connected with the top of the distillation tower of the condensation reaction kettle 33 and the dichloromethane head tank 32 through a spiral plate heat exchanger E34 and a pump; the cyclohexane/water receiving tank is connected with the top of the distillation tower of the condensation reaction kettle 33 through a spiral plate heat exchanger E34; the automatic back-flushing filter C39 is respectively connected with the industrial chromatographic column 40 and the cyclohexane head tank 38 through pipelines and pumps.
The substitution reaction kettle is protected by nitrogen, and the reaction is carried out under the anhydrous condition in the cyclization reaction process.
And the kettle-type distillation tower is filled with cy500 stainless steel corrugated packing.
The automatic back-washing filtration of the solid-phase catalyst adopts the following treatment modes: pumping reaction solvent into the automatic back-flushing filter from a solvent elevated tank by using a material transfer pump, introducing nitrogen through a nitrogen inlet of the reaction liquid temporary storage tank, pressurizing and back-flushing the solid-phase catalyst into the kettle, and performing the next batch operation.
And after being collected and concentrated, the tetrahydrofuran/water and the cyclohexane/water are respectively pumped into a tetrahydrofuran elevated tank and a cyclohexane elevated tank for recycling after being subjected to extractive distillation and water separation.
The column chromatography is carried out, and the eluent is ethyl acetate: dichloromethane: petroleum ether =5:1: 7.
The production device of the pyridyl-4-methylthiazole-5-bisabolone formate synthetic perfume has the following specific application:
: adding 90L of tetrahydrofuran into the stirring pot 1 from the tetrahydrofuran head tank 2, starting the stirrer, then weighing and metering 14kg of nicotinamide, fully dissolving to prepare a nicotinamide-tetrahydrofuran solution, and transferring the nicotinamide-tetrahydrofuran solution into the nicotinamide-tetrahydrofuran head tank 3 for later use;
: adding 100L of tetrahydrofuran into a substitution reaction kettle 4 from a tetrahydrofuran head tank 2, starting a stirrer, then adding 19kg of P2S5 from a hand hole heavy meter, after stirring and dissolving, starting a reaction kettle steam valve, raising the kettle temperature to 70-75 ℃, dropwise adding the nicotinamide-tetrahydrofuran solution prepared in the step S1 into the reaction kettle through a dropwise adding pump 5, wherein the dropwise adding time is 2-4 hours. After the dropwise addition is finished, continuously preserving the heat, stirring and reacting for 2-4h to finish the reaction, cooling the kettle to room temperature, and transferring the reaction solution into a washing kettle 6;
: adding 50kg of clean water into the water washing kettle 6, stirring for 30min, standing and filtering, transferring the filtrate into a distillation kettle of a kettle-type distillation tower A7, distilling at 63-65 ℃ under normal pressure to recover tetrahydrofuran/water azeotrope, and performing extractive distillation separation and purification on tetrahydrofuran to recycle. Adding 100L of ethyl acetate into the kettle substrate, transferring the kettle substrate into a washing kettle A11, and transferring tetrahydrofuran and a water solution obtained after condensation by a spiral plate heat exchanger A8 into a tetrahydrofuran/water receiving tank 9 for centralized dehydration treatment;
: adding 50L of clear water into a washing kettle A11, adding 10% sodium hydroxide solution into a washing kettle A11 from a 10% sodium hydroxide solution head tank 13 to adjust the pH value to be alkaline, standing for layering, transferring a water layer to a sewage treatment station for treatment, adding 10kg of anhydrous sodium sulfate into an oil layer for dehydration, filtering by an automatic backwashing filter A12, the solid phase sodium sulfate is recycled after dehydration treatment, the filtrate is transferred to a distillation kettle of a kettle-type distillation tower, distilling at 76-79 deg.C under normal pressure to recover ethyl acetate, recovering ethyl acetate when the tower top is not discharged or the temperature of the tower top is reduced, condensing ethyl acetate in ethyl acetate receiving tank A16 by spiral plate heat exchanger B15, transferring to an ethyl acetate head tank 10 for recycling, collecting the kettle substrate to obtain thionicotinamide, adding 150L of absolute ethanol into the thionicotinamide from the absolute ethanol head tank 17, stirring for dissolving, and transferring to a cyclization reaction kettle 18;
: dropwise adding 16.5kg of ethyl chloroacetate into the cyclization reaction kettle 18 from an ethyl chloroacetate overhead tank 19, controlling the dropwise adding time to be 1-2h, raising the kettle temperature of the cyclization reaction kettle 18 to 70-75 ℃, continuously stirring for reaction for 2h, and after the reaction is finished, transferring the reaction liquid into a distillation kettle of a kettle type distillation tower C20;
: opening a distillation kettle steam valve of a kettle type distillation tower C20, distilling and recovering ethanol at normal pressure at 77-80 ℃, ending recovering ethanol when no material is discharged from the top of the tower or the temperature of the top of the tower is reduced, condensing the ethanol by a spiral plate heat exchanger C21, collecting the condensed ethanol into an ethanol receiving tank 22, transferring the condensed ethanol into an ethanol elevated tank 17 for recycling to obtain a kettle substrate 2-pyridyl-4-methylthiazole-5-ethyl formate crude product, adding 100L of ethyl acetate into the kettle substrate from an ethyl acetate elevated tank 10, and transferring the crude product into a washing kettle B23;
: adding 10% sodium carbonate solution into a washing kettle B23 from a 10% sodium carbonate solution head tank 25 to adjust the pH value to be neutral, standing for layering, transferring a water layer to a sewage treatment station for treatment, adding 10kg anhydrous sodium sulfate into an oil layer for dehydration, filtering by a back flush automatic filter B24, dehydrating solid phase sodium sulfate, recycling, transferring filtrate to a distillation kettle of a kettle type distillation tower D26, distilling and recovering ethyl acetate at normal pressure under the condition of 76-79 ℃, ending recovering ethyl acetate when the material is not discharged from the top of the tower or the temperature of the top of the tower is reduced, condensing by a spiral plate heat exchanger D27, collecting to an ethyl acetate receiving tank, transferring to an ethyl acetate head tank 10 for recycling after 28, obtaining a kettle substrate 2-pyridyl-4-methylthiazole-5-ethyl formate, adding 100L methanol from a methanol head tank 29 to a kettle substrate, stirring and dissolving, and transferring to an acidification kettle 30;
: adding 100L of 10% sodium hydroxide solution into an acidification kettle 30 from a 10% sodium hydroxide solution overhead tank 13, starting a stirrer and a steam valve of the acidification kettle 30, raising the kettle temperature to 85-90 ℃, and performing saponification reaction for 5-8h to obtain 2-pyridyl-4-methylthiazole-5-sodium formate;
: adding 30% hydrochloric acid solution into 2-pyridyl-4-methylthiazole-5-sodium formate obtained from a 30% hydrochloric acid head tank 31 to an acidification kettle 30 to adjust the pH of a reaction solution to be acidic, then adding 100L dichloromethane into the acidification kettle 30 from a dichloromethane head tank 32 to perform extraction, standing and layering, transferring a water layer to a sewage treatment station for treatment, and transferring an oil layer to a condensation reaction kettle 33 with a distillation tower;
: opening a steam valve of a condensation reaction kettle 33, distilling and recovering dichloromethane at normal pressure at 39-42 ℃, ending the recovery of dichloromethane when no material is discharged from the top of the tower or the temperature of the top of the tower is reduced, condensing the dichloromethane by using a spiral plate heat exchanger E34, collecting the dichloromethane into a dichloromethane receiving tank 35, and transferring the dichloromethane into a dichloromethane overhead tank 32 for cyclic utilization to obtain a kettle substrate 2-pyridyl-4-methylthiazole-5-formic acid;
: respectively adding 23kg of bisabolol and 20L of cyclohexane into the 2-pyridyl-4-methylthiazole-5-formic acid obtained in the step S10 from the bisabolol head tank 37 and the cyclohexane head tank 38 in a metering manner, adding 1.6kg of a solid acid catalyst from a hand hole of the condensation reaction kettle 33, starting a stirrer and a steam valve of the condensation reaction kettle 33, raising the temperature of the kettle to 70-80 ℃, carrying out heat preservation stirring reaction for 2-4h, condensing and collecting an azeotrope of cyclohexane and water to a cyclohexane/water receiving tank 36 through a spiral plate heat exchanger E34 in time in the reaction process, and then carrying out centralized dehydration treatment and recycling;
: after the reaction is finished, an automatic back-flushing filter C39 is adopted for filtering, the solid phase is recycled and reused when next batch of operation is carried out, the liquid phase is transferred to the industrial chromatographic column 40 for elution and separation, and the eluent is ethyl acetate: dichloromethane: petroleum ether =5:1:7, to give a 2-pyridyl-4-methylthiazole-5-carboxylic acid bisabolene ester fragrance product.
The utility model provides an use and adopt niacinamide and P2S5 as the starting material, obtain thioniacinamide after the substitution reaction, carry out the cyclization reaction with 2-chloroacetoacetic acid ethyl ester and obtained 2-pyridyl-4-methylthiazole-5-ethyl formate, obtain 2-pyridyl-4-methylthiazole-5-formic acid after saponification, the acidizing, then condense with bisabolol under the effect of solid acid catalyst, synthesize 2-pyridyl-4-methylthiazole-5-bisabolol formate perfume through industrial chromatography separation and purification, this apparatus for producing process flow is relatively brief, adopt automatic back flush filtration solid acid catalyst have easily with the separation of liquid phase reaction system, do not corrode equipment, the simple advantage of aftertreatment, overcome the problem that current liquid acid corrodes equipment and contains the acid waste water polluted environment, the selectivity is improved, the method can be carried out at a lower temperature, the energy consumption is saved, the side reaction is reduced, and the production efficiency can be greatly improved.
The foregoing is merely exemplary and illustrative of the structure of the invention, and various modifications, additions and substitutions as described in the detailed description may be made by those skilled in the art without departing from the structure or exceeding the scope of the invention as defined in the claims.
Claims (2)
1. The utility model provides a apparatus for producing of bisabolol ester perfume which characterized in that: comprises a stirring pot (1), a tetrahydrofuran elevated tank (2), a nicotinamide-tetrahydrofuran solution elevated tank (3), a substitution reaction kettle (4), a dropping pump (5), a washing kettle (6), a kettle-type distillation tower A (7), a spiral plate heat exchanger A (8), a tetrahydrofuran/water receiving tank (9), an ethyl acetate elevated tank (10), a washing kettle A (11), an automatic back-flushing filter A (12), a 10% sodium hydroxide solution elevated tank (13), a kettle-type distillation tower B (14), a spiral plate heat exchanger B (15), an ethyl acetate receiving tank A (16), an absolute ethyl alcohol elevated tank (17), a cyclization reaction kettle (18), a chloroacetic acid ethyl ester elevated tank (19), a kettle-type distillation tower C (20), a spiral plate heat exchanger C (21), an ethyl alcohol receiving tank (22), a washing kettle B (23), an automatic back-flushing filter B (24), A 10% sodium carbonate solution elevated tank (25), a kettle-type distillation tower D (26), a spiral plate heat exchanger D (27), an ethyl acetate receiving tank B (28), a methanol elevated tank (29), an acidification kettle (30), a 30% hydrochloric acid elevated tank (31), a dichloromethane elevated tank (32), a condensation reaction kettle (33), a spiral plate heat exchanger E (34), a dichloromethane receiving tank (35), a cyclohexane/water receiving tank (36), a bisabolol elevated tank (37), a cyclohexane elevated tank (38), an automatic backwashing filter C (39) and an industrial chromatographic column (40);
the stirring pot (1) is respectively connected with the tetrahydrofuran elevated tank (2) and the nicotinamide-tetrahydrofuran solution elevated tank (3) through a pipeline and a pump, and the stirring pot (1) is provided with a hand-hole feeding port of nicotinamide; the substitution reaction kettle (4) is respectively connected with the tetrahydrofuran head tank (2) and the nicotinamide-tetrahydrofuran head tank (3) through a pipeline and a dropping pump (5), and the substitution reaction kettle (4) is provided with P2S5The hand hole feeding port; the water washing kettle (6) is respectively connected with the substitution reaction kettle (4) and the distillation kettle of the kettle type distillation tower A (7) through a pump; the top and the bottom of a distillation kettle of the kettle-type distillation tower A (7) are respectively connected with an ethyl acetate elevated tank (10) and a washing kettle A (11) through a pipeline and a pump; the tetrahydrofuran/water receiving tank (9) is connected with the top of the kettle-type distillation tower A (7) through a spiral plate heat exchanger A (8); the washing kettle A (11) is provided with a hand hole feeding port of anhydrous sodium sulfate, and the washing kettle A (11) is respectively connected with a 10% sodium hydroxide solution elevated tank (13) and an automatic backwashing filter A (12) through a pipeline and an in-kettle U-shaped pipe; the automatic back-flushing filter A (12) is respectively connected with a distillation kettle of the kettle-type distillation tower B (14) and the ethyl acetate head tank (10) through a pipeline and a pump; the top and the bottom of the kettle type distillation tower B (14) are respectively communicated with an absolute ethyl alcohol head tank (17) and a cyclization reaction through pipelines and pumpsThe reaction kettle (18) is connected; an ethyl acetate receiving tank A (16) is respectively connected with the top of the kettle type distillation tower B (14) and an ethyl acetate head tank (10) through a spiral plate heat exchanger B (15) and a pump; the cyclization reaction kettle (18) is respectively connected with an ethyl chloroacetate elevated tank (19) and a kettle-type distillation tower C (20) through a pipeline and a pump; the top and the bottom of the distillation kettle of the kettle-type distillation tower C (20) are respectively connected with the ethyl acetate elevated tank (10) and the washing kettle B (23) through pipelines and pumps; the ethanol receiving tank (22) is respectively connected with the top of the kettle-type distillation tower C (20) and the absolute ethanol head tank (17) through a spiral plate heat exchanger C (21) and a pump; the washing kettle B (23) is provided with a hand hole feed opening of anhydrous sodium sulfate, and the washing kettle B (23) is respectively connected with a 10% sodium carbonate solution elevated tank (25) and an automatic backwashing filter B (24) through a pipeline and an in-kettle U-shaped pipe; the automatic back-flushing filter B (24) is respectively connected with a distillation kettle of the kettle-type distillation tower D (26) and the ethyl acetate head tank (10) through a pipeline and a pump; the top and the bottom of the distillation kettle of the kettle-type distillation tower D (26) are respectively connected with a methanol elevated tank (29) and an acidification kettle (30) through pipelines and pumps; the ethyl acetate receiving tank B (28) is respectively connected with the top of the kettle type distillation tower D (26) and the ethyl acetate head tank (10) through a spiral plate heat exchanger D (27) and a pump; the top of the acidification kettle (30) is respectively connected with a 10% sodium hydroxide solution elevated tank (13), a 30% hydrochloric acid elevated tank (31) and a dichloromethane elevated tank (32) through pipelines; a condensation reaction kettle (33) with a distillation tower is respectively connected with an acidification kettle (30) and an automatic back-flushing filter C (39) through a pump and a U-shaped pipe in the kettle, the condensation reaction kettle (33) is provided with a catalyst feeding hand hole, and the top of the condensation reaction kettle (33) is respectively connected with a bisabolol elevated tank (37) and a cyclohexane elevated tank (38) through pipelines; the dichloromethane receiving tank (35) is respectively connected with the top of the distillation tower of the condensation reaction kettle (33) and the dichloromethane head tank (32) through a spiral plate heat exchanger E (34) and a pump; the cyclohexane/water receiving tank is connected with the top of a distillation tower of the condensation reaction kettle (33) through a spiral plate heat exchanger E (34); the automatic back-flushing filter C (39) is respectively connected with an industrial chromatographic column (40) and a cyclohexane head tank (38) through pipelines and pumps.
2. The apparatus for producing bisabolene ester flavor according to claim 1, wherein: and the kettle-type distillation tower is filled with cy500 stainless steel corrugated packing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922093809.4U CN211445579U (en) | 2019-11-28 | 2019-11-28 | Production device of bisabolol alkene ester spice |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922093809.4U CN211445579U (en) | 2019-11-28 | 2019-11-28 | Production device of bisabolol alkene ester spice |
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| Publication Number | Publication Date |
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| CN211445579U true CN211445579U (en) | 2020-09-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201922093809.4U Active CN211445579U (en) | 2019-11-28 | 2019-11-28 | Production device of bisabolol alkene ester spice |
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