CN210885878U - Production device for synthesizing galbanum ester spice by solid acid catalysis - Google Patents
Production device for synthesizing galbanum ester spice by solid acid catalysis Download PDFInfo
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- CN210885878U CN210885878U CN201921454803.9U CN201921454803U CN210885878U CN 210885878 U CN210885878 U CN 210885878U CN 201921454803 U CN201921454803 U CN 201921454803U CN 210885878 U CN210885878 U CN 210885878U
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Abstract
The utility model discloses a production device of solid acid catalytic synthesis galbanum ester spices adopts this device can obtain high-purity galbanum ester spices, has shortened process flow, improves the productivity of reaction. Ethyl diazoacetate and isoamylol are used as starting materials, after O-H insertion reaction, saponification and acidification are carried out to obtain isopentyloxy acetic acid, and then the isopentyloxy acetic acid is condensed with allyl alcohol under the catalysis of solid acid, so that the reaction time is greatly shortened and the intrinsic safety is improved. The solid-liquid separation of the anhydrous sodium carbonate drying and dehydrating operation is realized by adopting an automatic backwashing filtering technology, and the process flow is relatively short.
Description
Technical Field
The utility model belongs to the technical field of organic synthesis's apparatus for producing, concretely relates to apparatus for producing of solid acid catalytic synthesis galbanum ester spices.
Background
Galbanum ester, CAS number 67634-00-8, chemical name allyl isoamyloxyacetate, is an important synthetic perfume with fruity, delicate fragrance and galbanum and pineapple fragrance, and is widely used for perfuming various products such as perfumes, cosmetics, perfumed soaps, air fresheners, detergents and the like.
The traditional production method of the galbanum ester comprises the steps of firstly preparing isopentyloxy acetic acid through Williamson reaction, wherein the yield is about 80%, and then carrying out esterification reaction on the isoamyloxy acetic acid and allyl alcohol by using sulfuric acid, perchloric acid, p-toluenesulfonic acid and the like as catalysts to obtain the galbanum ester; firstly, metal sodium is used as a reaction reagent to react with isoamyl alcohol for dehydrogenation to prepare sodium isoamyl alcohol, and then xylene is used as a solvent to react with chloroacetic acid for sodium chloride removal to prepare the isopentyloxy acetic acid, the reaction is required to be carried out in an anhydrous system, the process difficulty is high, the risk of using the metal sodium is high, and the industrial production is difficult to realize; secondly, sodium hydride is used as a reaction reagent, reacts with isoamyl alcohol to produce sodium alkoxide in tetrahydrofuran as a solvent, then reacts with chloroacetic acid in a dimethyl sulfoxide solution to produce sodium isopentoxy acetate, and then is acidified to prepare the isopentoxy acetic acid in a strong acid condition, wherein the sodium hydride is adopted in the reaction, so that the reaction system has strict requirements, the reaction system is required to be anhydrous and low-temperature, a large amount of organic solvent is used, hydrogen is generated, the reaction condition is harsh, the operation is complex, the raw material cost is high, and the method is not suitable for industrial scale production; and thirdly, NaOH is used as a reaction catalyst, sodium chloroacetate and isoamylol react to generate sodium isopentyloxy acetate, and then the sodium isopentyloxy acetate is obtained after acidification. In addition, acid catalysts such as sulfuric acid and the like adopted in the esterification reaction step are low in price and good in catalytic effect as traditional esterification catalysts which are used up to now, but the acid catalysts severely corrode equipment and pollute the environment by acid-containing wastewater.
SUMMERY OF THE UTILITY MODEL
To the problem among the prior art, the utility model aims to provide a production device of solid acid catalytic synthesis galbanum ester spices shortens process flow, improves the productivity of reaction.
The purpose of the utility model can be realized by the following technical scheme:
a production device for synthesizing a galbanum ester spice by solid acid catalysis comprises a batching pot, a diazoacetic acid ethyl ester elevated tank, a dichloroethane elevated tank, a material transfer pump A, a 30% diazoacetic acid ethyl ester-dichloroethane elevated tank, an isoamyl alcohol elevated tank, a dripping pump, a reaction kettle, an automatic backwashing precision filter A, a dichloroethane transfer pump A, a kettle-type distillation tower, a condenser A, a dichloroethane receiving tank, an isoamyl alcohol vacuum receiving tank, an isoamyl alcohol transfer pump, a dichloroethane transfer pump B, a material transfer pump B, a sodium hydroxide solution preparation kettle, an anticorrosive material pump, a sodium hydroxide solution elevated tank, a 15% hydrochloric acid elevated tank, a saturated sodium chloride elevated tank, an acidification kettle, a sodium chloride transfer pump, a material transfer pump C, a dehydration kettle, an automatic backwashing precision filter B, a dichloroethane transfer pump C, an isopentyloxy acetic acid elevated tank, an allyl alcohol elevated tank, A cyclohexane elevated tank, a condensation reaction kettle, a spiral plate heat exchanger, a cyclohexane/water receiving tank, an automatic back-flushing precision filter C, a cyclohexane transfer pump, a kettle-type rectifying tower, a condenser B, an allyl alcohol vacuum receiving tank, a product vacuum receiving tank, an allyl alcohol transfer pump and a product temporary storage tank;
the batching pot is respectively connected with the ethyl diazoacetate head tank and the dichloroethane head tank through pipelines; the 30% ethyl diazoacetate-dichloroethane head tank is respectively connected with the batching kettle and the reaction kettle through a material transfer pump A and a dropping pump; the reaction kettle is provided with a solid-phase catalyst hand-hole feeding port and a nitrogen interface; the reaction kettle is respectively connected with a dichloroethane head tank and an isoamylol head tank through pipelines; the automatic back-flushing precision filter A is respectively connected with the reaction kettle, the dichloroethane receiving tank and the distillation kettle of the kettle-type distillation tower through a U-shaped pipe in the reaction kettle, a dichloroethane transfer pump A and a pipeline; the dichloroethane receiving tank is respectively connected with the top of the kettle-type distillation tower and the dichloroethane head tank through a condenser A and a dichloroethane transfer pump B; the isoamyl alcohol vacuum receiving tank is respectively connected with the top of the kettle-type distillation tower and an isoamyl alcohol head tank through a condenser A and an isoamyl alcohol transfer pump; the sodium hydroxide solution elevated tank is respectively connected with the sodium hydroxide solution preparation kettle and the acidification kettle through a corrosion-proof material pump and a pipeline; the acidification kettle is respectively connected with the kettle bottom of the kettle-type distillation tower, the dehydration kettle and the 15% hydrochloric acid elevated tank through a material transfer pump B, a material transfer pump C and a pipeline; the saturated sodium chloride elevated tank is respectively connected with the kettle top and the kettle bottom of the acidification kettle through a pipeline and a sodium chloride transfer pump; the automatic back-flushing precision filter B is respectively connected with the dehydration kettle, the dichloroethane head tank and the condensation reaction kettle through a U-shaped pipe, a dichloroethane transfer pump C and an isopentyloxy acetic acid head tank in the dehydration kettle; the condensation reaction kettle is provided with a distillation tower and a solid-phase catalyst feeding hand hole, and the cyclohexane/water receiving tank is connected with the top of the condensation reaction kettle through a spiral plate heat exchanger; the allyl alcohol head tank and the cyclohexane head tank are respectively connected with the condensation reaction kettle through pipelines; the automatic back-flushing precision filter C is respectively connected with the condensation reaction kettle, the cyclohexane head tank and the distillation kettle of the kettle-type rectifying tower through a U-shaped pipe, a cyclohexane transfer pump and a pipeline in the condensation reaction kettle; the allyl alcohol vacuum receiving tank is respectively connected with the top of the kettle type rectifying tower and the allyl alcohol head tank through a condenser B and an allyl alcohol transfer pump; the product vacuum receiving tank is respectively connected with the tower top of the kettle type rectifying tower and the product temporary storage tank through a condenser B and a pipeline.
Furthermore, the dehydration kettle is provided with a saturated steam inlet for drying, and anhydrous sodium sulfate is filled in the dehydration kettle.
Further, the tank-type distillation tower is filled with cy500 stainless steel corrugated filler, and the tank-type rectification tower is filled with cy700 stainless steel corrugated filler.
Furthermore, after collecting the azeotrope of cyclohexane and water into a cyclohexane/water receiving tank, the azeotrope is subjected to extraction, rectification and water separation treatment and then is pumped into a cyclohexane head tank for recycling.
The automatic back-washing filtration of the solid-phase catalyst adopts the following treatment modes:
the automatic back-flushing filtration of the solid rhodium catalyst and the solid acid catalyst adopts the following treatment modes: and pumping the reaction solvent into the automatic back-flushing precision filter of the dehydration kettle from the solvent elevated tank by using a chemical material-pumping pump, introducing nitrogen through a nitrogen inlet of the reaction liquid temporary storage tank, and pressurizing and back-flushing the solid rhodium catalyst or the solid acid catalyst into the kettle for the next batch of operation.
The utility model has the advantages that:
the utility model provides a production device of solid acid catalytic synthesis galbanum ester spices adopts this device can obtain high-purity galbanum ester spices, has shortened process flow, improves the productivity of reaction. Ethyl diazoacetate and isoamylol are used as starting materials, after O-H insertion reaction, saponification and acidification are carried out to obtain isopentyloxy acetic acid, and then the isopentyloxy acetic acid is condensed with allyl alcohol under the catalysis of solid acid, so that the reaction time is greatly shortened and the intrinsic safety is improved. The solid-liquid separation of the anhydrous sodium carbonate drying and dehydrating operation is realized by adopting an automatic backwashing filtering technology, and the process flow is relatively short.
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 schematic diagram of a production apparatus for synthesizing a galbanum ester spice by solid acid catalysis;
in the drawings, the components represented by the respective reference numerals are listed below:
1. a batching pot, 2, an ethyl diazoacetate elevated tank, 3, an ethylene dichloride elevated tank, 4, a material transfer pump A, 5, 30 percent ethyl diazoacetate-ethylene dichloride elevated tank, 6, an isoamyl alcohol elevated tank, 7, a dropping pump, 8, a reaction kettle, 9, an automatic back-flushing precision filter A, 10, an ethylene dichloride transfer pump A, 11, a kettle-type distillation tower, 12, a condenser A, 13, an ethylene dichloride receiving tank, 14, an isoamyl alcohol vacuum receiving tank, 15, an isoamyl alcohol transfer pump, 16, an ethylene dichloride transfer pump B, 17, a material transfer pump B, 18, a sodium hydroxide solution preparation kettle, 19, a corrosion-proof material pump, 20, a sodium hydroxide solution elevated tank, 21, 15 percent hydrochloric acid elevated tank, 22 back-flushing, a saturated sodium chloride elevated tank, 23, an acidification kettle, 24, a sodium chloride transfer pump, 25, a material transfer pump C, 26, a dehydration kettle, 27 and an automatic precision filter B, 28. dichloroethane transfer pump C, 29, isopentyloxy acetic acid elevated tank, 30, allyl alcohol elevated tank, 31, cyclohexane elevated tank, 32, condensation reaction kettle, 33, spiral plate heat exchanger, 34, cyclohexane/water receiving tank, 35, automatic back-flushing precision filter C, 36, cyclohexane transfer pump, 37, kettle type rectifying tower, 38, condenser B, 39, allyl alcohol vacuum receiving tank, 40, product vacuum receiving tank, 41, allyl alcohol transfer pump, 42 and product temporary storage tank.
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 a solid acid-catalyzed synthesis of galbanum ester spice comprises a batching kettle 1, a diazoacetic acid ethyl ester head tank 2, a dichloroethane head tank 3, a material transfer pump A4, a 30% diazoacetic acid ethyl ester-dichloroethane head tank 5, an isoamyl alcohol head tank 6, a dropping pump 7, a reaction kettle 8, an automatic back-flushing precision filter A9, a dichloroethane transfer pump A10, a kettle-type distillation tower 11, a condenser A12, a dichloroethane receiving tank 13, an isoamyl alcohol vacuum receiving tank 14, an isoamyl alcohol transfer pump 15, a dichloroethane transfer pump B16, a material transfer pump B17, a sodium hydroxide solution preparation kettle 18, a corrosion-resistant material pump 19, a sodium hydroxide solution head tank 20, a 15% hydrochloric acid head tank 21, a saturated sodium chloride head tank 22, an acidification kettle 23, a sodium chloride transfer pump 24, a material transfer pump C25, a dehydration kettle 26, an automatic back-flushing precision filter B27, A dichloroethane transfer pump C28, an isopentyloxy acetic acid elevated tank 29, an allyl alcohol elevated tank 30, a cyclohexane elevated tank 31, a condensation reaction kettle 32, a spiral plate heat exchanger 33, a cyclohexane/water receiving tank 34, an automatic backwashing precision filter C35, a cyclohexane transfer pump 36, a kettle type rectifying tower 37, a condenser B38, an allyl alcohol vacuum receiving tank 39, a product vacuum receiving tank 40, an allyl alcohol transfer pump 41 and a product temporary storage tank 42;
the batching pot 1 is respectively connected with a diazoacetic acid ethyl ester elevated tank 2 and a dichloroethane elevated tank 3 through pipelines; the 30% ethyl diazoacetate-dichloroethane head tank 5 is respectively connected with the batching pot 1 and the reaction kettle 8 through a material transfer pump A4 and a dripping pump 7; the reaction kettle 8 is provided with a solid-phase catalyst hand-hole feeding port and a nitrogen interface; the reaction kettle 8 is respectively connected with the dichloroethane head tank 3 and the isoamylol head tank 6 through pipelines; the automatic back-flushing precision filter A9 is respectively connected with the reaction kettle 8, the dichloroethane receiving tank 13 and the distillation kettle of the kettle-type distillation tower 11 through a U-shaped pipe in the reaction kettle 8, a dichloroethane transfer pump A10 and pipelines; the dichloroethane receiving tank 13 is respectively connected with the top of the kettle-type distillation tower 11 and the dichloroethane head tank 3 through a condenser A12 and a dichloroethane transfer pump B16; the isoamyl alcohol vacuum receiving tank 14 is respectively connected with the top of the kettle-type distillation tower 11 and the isoamyl alcohol head tank 6 through a condenser A12 and an isoamyl alcohol transfer pump 15; the sodium hydroxide solution elevated tank 20 is respectively connected with the sodium hydroxide solution preparation kettle 18 and the acidification kettle 23 through a corrosion-proof material pump 19 and a pipeline; the acidification kettle 23 is respectively connected with the kettle bottom of the kettle-type distillation tower 11, the dehydration kettle 26 and the 15% hydrochloric acid elevated tank through a material transfer pump B17, a material transfer pump C25 and pipelines; the saturated sodium chloride elevated tank 22 is respectively connected with the kettle top and the kettle bottom of the acidification kettle 23 through a pipeline and a sodium chloride transfer pump 24; the automatic back-flushing precision filter B27 is respectively connected with the dehydration kettle 26, the dichloroethane head tank 3 and the condensation reaction kettle 32 through a U-shaped pipe in the dehydration kettle 26, a dichloroethane transfer pump C28 and an isopentyloxy acetic acid head tank 29; the condensation reaction kettle 32 is provided with a distillation tower and a solid-phase catalyst feeding hand hole, and a cyclohexane/water receiving tank 34 is connected with the top of the condensation reaction kettle 32 through a spiral plate heat exchanger 33; the allyl alcohol head tank 30 and the cyclohexane head tank 31 are respectively connected with the condensation reaction kettle through pipelines; the automatic back-flushing precision filter C35 is respectively connected with the condensation reaction kettle 32, the cyclohexane head tank 31 and the distillation kettle of the kettle-type rectifying tower 37 through a U-shaped pipe, a cyclohexane transfer pump 36 and a pipeline in the condensation reaction kettle 32; the allyl alcohol vacuum receiving tank 39 is respectively connected with the top of the kettle-type rectifying tower 37 and the allyl alcohol head tank 30 through a condenser B38 and an allyl alcohol transfer pump 41; the product vacuum receiving tank 40 is connected with the top of the tank rectifying tower 37 and the product temporary storage tank 42 through a condenser B38 and a pipeline respectively.
The device for producing the galbanum ester spice has the following specific application:
s1: adding ethyl diazoacetate and dichloroethane into a batching pot 1 from an ethyl diazoacetate head tank 2 and a dichloroethane head tank 3, starting a stirrer, uniformly stirring, preparing a 30% ethyl diazoacetate-dichloroethane solution, and pumping into a 30% ethyl diazoacetate-dichloroethane head tank 5 for later use by a material transfer pump A4;
s2: firstly, solid rhodium catalyst Rh is put into a reaction kettle 8 through a hand hole2(OAc)4Then, ethylene dichloride and isoamylol are metered into a reaction kettle 8 through a dichloroethane elevated tank 3 and an isoamylol elevated tank 6 respectively, a stirrer is started, and nitrogen is continuously introduced into the reaction kettle 8 from a nitrogen inlet of the reaction kettle 8;
s3: opening a steam valve of the reaction kettle 8, starting heating to the kettle temperature of 60-80 ℃, dropwise adding the ethyl diazoacetate-dichloroethane solution prepared in the step S1 into the reaction kettle 8 from the 30% ethyl diazoacetate-dichloroethane head tank 5 through the dropwise adding pump 7, controlling the dropwise adding time to be 4-8 h, continuing carrying out heat preservation reaction for 2-4 h after dropwise adding is finished, finishing the reaction, and starting circulating cooling water to reduce the kettle temperature of the reaction kettle 8 to room temperature;
s4: filtering the reaction liquid by an automatic back-flushing precision filter A9, pumping the liquid-phase reaction liquid into a distillation kettle of the kettle-type distillation tower 11 under the pressure of nitrogen, and back-flushing the dichloroethane to the solid-phase catalyst in the reaction kettle 8 from the dichloroethane head tank 3 by a dichloroethane transfer pump A10 for the reaction of the next batch;
s5: opening a distillation method steam valve of the kettle type distillation tower 11, raising the temperature of the kettle to 57-60 ℃, recovering dichloroethane under normal pressure, condensing the dichloroethane by using a condenser A12, collecting the dichloroethane into a dichloroethane receiving tank 13, pumping the dichloroethane into a dichloroethane overhead tank 3 by using a dichloroethane transfer pump B16 for recycling, and ending the dichloroethane recovery when no material is discharged from the top of the tower or the temperature of the top of the tower is reduced; starting low vacuum, decompressing and recovering excessive isoamyl alcohol, condensing by a condenser A12, collecting to an isoamyl alcohol vacuum receiving tank 14, and pumping into an isoamyl alcohol head tank 6 by an isoamyl alcohol transfer pump 15 for cyclic utilization;
s6: pumping the kettle bottom reaction liquid in the kettle type distillation tower 11 into the acidification kettle 23 through a material feeding transfer pump B17;
s7: firstly, adding tap water into a sodium hydroxide solution preparation kettle 18 in a metering manner, starting a stirrer, weighing and metering sodium hydroxide from a hand hole, uniformly stirring to prepare a 10% sodium hydroxide solution, and pumping the sodium hydroxide solution into a sodium hydroxide solution head tank 20 by using a corrosion-resistant material pump 19 for later use;
s8: adding the sodium hydroxide solution obtained in the step S7 into the acidification kettle 23 in a metering manner, opening a steam valve of the acidification kettle 23, raising the kettle temperature to 60 ℃, finishing the reaction after reacting for 3-5 hours, and reducing the kettle temperature to room temperature;
s9: adding 15% hydrochloric acid into the acidification kettle 23 from the hydrochloric acid head tank 21 in a metering manner, and adjusting the pH value of the reaction liquid in the acidification kettle 23 until the pH value of the reaction liquid is 2.5-3.0;
s10: standing and layering for 2h, and separating out a water layer and sending to a sewage treatment station for treatment. Adding saturated sodium chloride solution into an oil layer in an acidification kettle 23 from a saturated sodium chloride head tank 22 for washing for 3 times, separating out a first washing water layer, conveying the first washing water layer to a sewage treatment station for treatment, and pumping the second washing layered water layer into the saturated sodium chloride head tank 22 through a sodium chloride transfer pump 24 for recycling;
s11: pumping the layered oil layer obtained in the step S10 into a dehydration kettle 26 filled with anhydrous sodium sulfate by using a material transfer pump C25, and dehydrating for 1-2 hours; filtering the oil layer by an automatic back-flushing precision filter B27, and then pumping the oil layer into an isopentyloxy acetic acid head tank 29;
s12: firstly, solid acid catalyst Yb-MoO is put into the condensation reaction kettle through 32 hand holes3/Al2O3-ZrO2Then separately from the allyl alcohol head tank 30Metering allyl alcohol and cyclohexane into a condensation reaction kettle 32 in a cyclohexane head tank 31, starting a stirrer, uniformly stirring, metering isopentyloxy acetic acid into the condensation reaction kettle 32 from an isopentyloxy acetic acid head tank 29, starting a steam valve of the condensation reaction kettle 32, raising the temperature of the kettle to 60-65 ℃, reacting for 2-4 hours, separating an azeotrope of cyclohexane and water from a reaction system through a spiral plate heat exchanger 33 at the top of a distillation tower carried by the condensation reaction kettle 32 in the reaction process, collecting the azeotrope into a cyclohexane/water receiving tank 34, and performing extraction, rectification and separation to recover cyclohexane;
the preparation method of the solid acid catalyst comprises the following steps:
preparing 100ml of 20-30% zirconium oxychloride octahydrate solution, sequentially adding 10g of aluminum hydroxide and 10-12g of ammonium molybdate while stirring, stirring for 10-15min for complete dissolution, and then adding 1.35-2g of Yb (NO)3)3·5H2O, stirring and dissolving, adding the prepared solution and 8mol/L ammonia water into 300ml of ammonia water solution with the pH value of 9.00 at the same time, keeping the pH value of the solution between 8.95 and 9.10 in the dropwise adding process, continuing stirring for 20 to 30min after the dropwise adding is finished, aging for 24h at room temperature, performing suction filtration, washing the solid by deionized water until no chloride ions exist in the washing liquid (detected by 0.1mol/L silver nitrate solution), drying for 8 to 10h at 105 ℃, finally roasting for 2h at 800 ℃ in an atmosphere protection box type furnace (nitrogen protection), taking out and cooling to room temperature to obtain the acid catalyst Yb-MoO3/Al2O3-ZrO2Wherein the mass ratio of Yb to Mo to Al to Zr is 0.5-0.7: 4.5-5.8: 3.0-3.5: 5.4-8.2;
s13: after the reaction is finished, filtering the reaction liquid through an automatic back-flushing precision filter C35, pumping the liquid-phase reaction liquid into a distillation kettle of the kettle-type rectifying tower 37 under the pressure of nitrogen, and back-flushing the cyclohexane back-flushing solid-phase catalyst from the cyclohexane head tank 31 into the condensation reaction kettle 32 through the cyclohexane transfer pump 36 for the reaction of the next batch;
s14: opening a distillation kettle steam valve of the kettle type rectifying tower 37, opening low vacuum, recovering excessive allyl alcohol under reduced pressure, condensing by a condenser B38, transferring the allyl alcohol to an allyl alcohol head tank 30 by an allyl alcohol transfer pump 41 through an allyl alcohol vacuum receiving tank 39 for recovery and reuse, after the temperature of the top of the tower is reduced or the top of the tower is not discharged, recovering allyl alcohol, opening high vacuum, distilling under reduced pressure to collect galbanum ester, condensing by a condenser B38, collecting distillate by a product vacuum receiving tank 40, and transferring to a product temporary storage tank 42 to obtain a galbanum ester spice product;
s15: through detecting, adopt the utility model provides a purity of the galbanum ester perfume product of apparatus for producing production reaches more than 98%, and allyl alcohol content is below 0.1%.
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 (4)
1. A production device for synthesizing a galbanum ester spice by solid acid catalysis is characterized in that: comprises a proportioning pot (1), a diazoacetic acid ethyl ester elevated tank (2), a dichloroethane elevated tank (3), a material transfer pump A (4), a 30% diazoacetic acid ethyl ester-dichloroethane elevated tank (5), an isoamyl alcohol elevated tank (6), a dripping pump (7), a reaction kettle (8), an automatic backwashing precision filter A (9), a dichloroethane transfer pump A (10), a kettle-type distillation tower (11), a condenser A (12), a dichloroethane receiving tank (13), an isoamyl alcohol vacuum receiving tank (14), an isoamyl alcohol transfer pump (15), a dichloroethane transfer pump B (16), a material transfer pump B (17), a sodium hydroxide solution preparation kettle (18), an anticorrosive material pump (19), a sodium hydroxide solution elevated tank (20), a 15% hydrochloric acid elevated tank (21), a saturated sodium chloride elevated tank (22), an acidification kettle (23), a sodium chloride transfer pump (24), A material transfer pump C (25), a dehydration kettle (26), an automatic back-flushing precision filter B (27), a dichloroethane transfer pump C (28), an isopentyloxy acetic acid elevated tank (29), an allyl alcohol elevated tank (30), a cyclohexane elevated tank (31), a condensation reaction kettle (32), a spiral plate heat exchanger (33), a cyclohexane/water receiving tank (34), an automatic back-flushing precision filter C (35), a cyclohexane transfer pump (36), a kettle type rectifying tower (37), a condenser B (38), an allyl alcohol vacuum receiving tank (39), a product vacuum receiving tank (40), an allyl alcohol transfer pump (41) and a product temporary storage tank (42);
the batching pot (1) is respectively connected with the ethyl diazoacetate head tank (2) and the dichloroethane head tank (3) through pipelines; the 30% ethyl diazoacetate-dichloroethane head tank (5) is respectively connected with the batching pot (1) and the reaction kettle (8) through a material transfer pump A (4) and a dripping pump (7); the reaction kettle (8) is provided with a solid-phase catalyst hand-hole feeding port and a nitrogen interface; the reaction kettle (8) is respectively connected with the dichloroethane elevated tank (3) and the isoamylol elevated tank (6) through pipelines; the automatic back-flushing precision filter A (9) is respectively connected with the reaction kettle (8), the dichloroethane receiving tank (13) and the distillation kettle of the kettle-type distillation tower (11) through a U-shaped pipe in the reaction kettle (8), a dichloroethane transfer pump A (10) and a pipeline; the dichloroethane receiving tank (13) is respectively connected with the top of the kettle-type distillation tower (11) and the dichloroethane head tank (3) through a condenser A (12) and a dichloroethane transfer pump B (16); the isoamyl alcohol vacuum receiving tank (14) is respectively connected with the top of the kettle-type distillation tower (11) and the isoamyl alcohol head tank (6) through a condenser A (12) and an isoamyl alcohol transfer pump (15); the sodium hydroxide solution elevated tank (20) is respectively connected with the sodium hydroxide solution preparation kettle (18) and the acidification kettle (23) through an antiseptic material pump (19) and a pipeline; the acidification kettle (23) is respectively connected with the kettle bottom of the kettle-type distillation tower (11), the dehydration kettle (26) and the 15% hydrochloric acid elevated tank (21) through a material transfer pump B (17), a material transfer pump C (25) and a pipeline; the saturated sodium chloride elevated tank (22) is respectively connected with the kettle top and the kettle bottom of the acidification kettle (23) through a pipeline and a sodium chloride transfer pump (24); the automatic back-flushing precision filter B (27) is respectively connected with the dehydration kettle (26), the dichloroethane head tank (3) and the condensation reaction kettle (32) through a U-shaped pipe in the dehydration kettle (26), a dichloroethane transfer pump C (28) and an isopentyloxy acetic acid head tank (29); the condensation reaction kettle (32) is provided with a distillation tower and a solid-phase catalyst feeding hand hole, and the cyclohexane/water receiving tank (34) is connected with the top of the condensation reaction kettle (32) through a spiral plate heat exchanger (33); the allyl alcohol elevated tank (30) and the cyclohexane elevated tank (31) are respectively connected with the condensation reaction kettle through pipelines; the automatic back-flushing precision filter C (35) is respectively connected with the condensation reaction kettle (32), the cyclohexane elevated tank (31) and the distillation kettle of the kettle-type rectifying tower (37) through a U-shaped pipe, a cyclohexane transfer pump (36) and a pipeline in the condensation reaction kettle (32); the allyl alcohol vacuum receiving tank (39) is respectively connected with the top of the kettle-type rectifying tower (37) and the allyl alcohol head tank (30) through a condenser B (38) and an allyl alcohol transfer pump (41); the product vacuum receiving tank (40) is respectively connected with the top of the kettle-type rectifying tower (37) and the product temporary storage tank (42) through a condenser B (38) and a pipeline.
2. The apparatus for producing a solid acid catalyzed synthesis of galaxolide flavor according to claim 1, wherein: the dehydration kettle (26) is attached with a saturated steam inlet for drying, and anhydrous sodium sulfate is filled in the dehydration kettle (26).
3. The apparatus for producing a solid acid catalyzed synthesis of galaxolide flavor according to claim 1, wherein: the kettle-type distillation tower (11) is filled with cy500 stainless steel corrugated filler, and the kettle-type rectification tower (37) is filled with cy700 stainless steel corrugated filler.
4. The apparatus for producing a solid acid catalyzed synthesis of galaxolide flavor according to claim 1, wherein: after collecting the azeotrope of cyclohexane and water in a cyclohexane/water receiving tank (34), the azeotrope is sent into a cyclohexane head tank (31) for recycling after being subjected to extraction, rectification and water separation treatment.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201921454803.9U CN210885878U (en) | 2019-09-03 | 2019-09-03 | Production device for synthesizing galbanum ester spice by solid acid catalysis |
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| CN201921454803.9U CN210885878U (en) | 2019-09-03 | 2019-09-03 | Production device for synthesizing galbanum ester spice by solid acid catalysis |
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| CN210885878U true CN210885878U (en) | 2020-06-30 |
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