CN208776619U - A kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid - Google Patents
A kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid Download PDFInfo
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- CN208776619U CN208776619U CN201821391924.9U CN201821391924U CN208776619U CN 208776619 U CN208776619 U CN 208776619U CN 201821391924 U CN201821391924 U CN 201821391924U CN 208776619 U CN208776619 U CN 208776619U
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Abstract
The utility model discloses a kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid, including jacket type distributor stirred tank, sulfuric acid gauge tank, jacket type distributor emulsifying kettle, jacket type distributor product stirred tank, loop reactor with venturi-type eductors, cyclic suspension bed reactor, piperonyl cyclonene measuring tank, thermostat, filter plant, charge pump, air accumulator, filtrate receiver.Solution after emulsification is dispersed into fine drop using the loop reactor and cyclic suspension bed reactor with venturi-type eductors during the reaction by the utility model, form countless microresponse systems, independent reaction, increase heat and mass efficiency, inhibits to cause to lead to the problem of by-product due to heat transfer uneven two.
Description
Technical field
The utility model belongs to technical field of chemical engineering, and in particular to a kind of enhancing emulsification synthesis 3,4- methylene-dioxy
The device of mandelic acid.
Background technique
3,4- methylene-dioxy mandelic acid is the intermediary for synthesizing piperonal.Piperonal is widely used in perfume, fragrance, cherry
The flavoring agent of peach and vanilla flavored.Fragrance remaining time is long, be used as and pastil, fixastive, be the U.S.'s spice extract manufacture association approve
Safe fragrance, be widely used in space deodorant, fragrance for detergents, food flavor and tobacco essence.It can be also used in chemical life
In object pharmacy.It is one of the special commodity that country carries out export license.
The synthetic method of traditional 3,4- methylene-dioxy mandelic acid is to use piperonyl cyclonene, glyoxalic acid in acid condition
Carry out synthetic method, Dan Shao army etc. have studied molar ratio of reaction temperature, reaction time, glyoxalic acid and piperonyl cyclonene etc. reaction because
Element influence (Anhui study on the synthesis [J] the chemical industry of Dan Shaojun, Du Zhenmei .3,4- methylene-dioxy mandelic acid, 2007,2；
46-47.).Wang Shuai etc. (Wang Shuai, Li Yaoxian, Wang Hengguo air catalytic oxidation synthesizing piperonal [J] application chemical industry, 2009,
4:491-493.) and Zhang Kunshui etc. is (in silver nitrate technique study [J] of the medicinal jasminal synthesis of Zhang Kunshui, Huang Han, Chen Yisheng
State modern medicines application .2008,2:53-54.) when studying heliotropin synthetic method, and using similar preparation 3,4-
Methylene-dioxy mandelic acid.Xi Hongjuan has investigated the factors such as reaction temperature, catalyst concn, raw material proportioning and reaction time
It influences, (the ocean Xi Hongjuan, Gao Zhixian, Wang Jianguo jasmine is inquired into sulfuric acid catalyst mechanism of action and the possible reaction mechanism mechanism of reaction
Jasmine aldehyde intermediate 3, the synthesis of 4- methylene-dioxy mandelic acid and characterization [J] chemical research and application, 2009,21:396-
400.)。
The above-mentioned prior art has the following disadvantages；
Due to product 3,4- methylene-dioxy mandelic acid viscosity is big, in the synthesis process mobility
Difference has that mass-transfer efficiency is not high, and immiscible between piperonyl cyclonene and glyoxalic acid, and contact area is small between two-phase, institute
Cause low yield to lead to react insufficient, uneven effect of conducting heat is poor, is easy to appear the poor selectivity of reaction, more than by-product
Phenomenon
Utility model content
The purpose of the utility model is to overcome the deficiencies in the prior art, provide a kind of enhancing emulsification synthesis 3,4- methylene two
Two-phase object mixing efficiency in reaction system can be improved in the method and device of oxygroup mandelic acid, the utility model, improves reaction speed
Degree shortens the reaction time, improves reaction yield, and reduce the wastewater flow rate generated in reaction process.
The utility model is achieved through the following technical solutions:
A kind of method of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid, which is characterized in that according to the following steps
It carries out:
Step 1, be water by mass ratio: 50wt% glyoxalic acid solution=1:15~20 mixture carries out constant temperature stirring,
The constant temperature whipping temp is -30 DEG C~-20 DEG C, stirring rate 350rpm~450rpm；
Step 2, after starting stirring, the 98wt% concentrated sulfuric acid is added dropwise in Xiang Suoshu mixture, dripping quantity per minute is described mixed
0.03~0.1 times for closing amount of substance, the ratio that the 98wt% concentrated sulfuric acid total amount and the quality of water described in step 1 is added dropwise are
The 98wt% concentrated sulfuric acid: water=12~15:1, whipping temp are -30 DEG C~-20 DEG C；
Step 3, after all 98wt% concentrated sulfuric acids are added dropwise to complete, continue 20~40min of stirring, whipping temp -30
DEG C~-20 DEG C；
Step 4,3,4- methylene-dioxy mandelic acid is added into the solution after the completion of step 3,3,4- methylene two is added
The ratio of water quality described in the amount and step 1 of oxygroup mandelic acid is 3,4- methylene-dioxy mandelic acid: water=0.1~1:1；
Step 5, the solution after the completion of step 4 is emulsified, 10~15Kr/min of emulsifying rate, when emulsification is added dropwise simultaneously
Piperonyl cyclonene, dripping quantity per minute are 0.1~1 times of water quality described in step 1,3~10min of emulsification times；
Step 6, the step 5 is repeated as many times, every time between be spaced 3~10min, be added in piperonyl cyclonene total amount and step 1
The ratio of the water quality is piperonyl cyclonene: water=10~15:1；
Step 7, the solution after step 6 is passed through into the loop reactor with venturi-type eductors after mixing,
Into suspended-bed reactor, the reaction was continued, and temperature is 0 DEG C~10 DEG C in the suspended-bed reactor, described to have venturi injection
The loop reactor outer circulation circuit of device is provided with heat exchanger, and the taphole temperature of the heat exchanger is -30 DEG C~-20 DEG C,
Bubble diameter is 0.01~0.07mm in the loop reactor, and gas flow is institute in step 1 in the venturi-type eductors
100~200 times/min for stating volume of mixture, 3~10min of mixed reaction time in the suspended-bed reactor；
Step 8, terminate liquid is added into the solution after step 7, the terminate liquid is added described in total amount and step 1
The ratio of water quality is terminate liquid: water=15~30:1, terminates reaction, obtains product；
It further include the air-blowing process into solution during the step 1~step 6, air-blowing amount per minute is institute in step 1
7~20 times for stating volume of mixture.
In above-mentioned technical proposal, mass ratio is water: 50wt% glyoxalic acid solution=1:15~17 by the step 1
Mixture carries out constant temperature stirring, and the constant temperature whipping temp is -28 DEG C~-23 DEG C, stirring rate 380rpm~420rpm.
In above-mentioned technical proposal, the amount and the water quality of 3,4- methylene-dioxy mandelic acid is added in the step 4
Than for 3,4- methylene-dioxy mandelic acid: water=0.1~0.4:1.
In above-mentioned technical proposal, piperonyl cyclonene is added dropwise simultaneously when emulsification, often in the step 5,10~12Kr/min of emulsifying rate
Minute dripping quantity is 0.5~0.8 times of the water quality, 5~10min of emulsification times.
In above-mentioned technical proposal, the step 6, the step 5 is repeated 3~8 times, every time between be spaced 3~10min, add
The ratio for entering piperonyl cyclonene total amount and the water quality is piperonyl cyclonene: water=10~12:1.
In above-mentioned technical proposal, in the step 7, the heat transferring medium in the heat exchanger is ethylene glycol.
In above-mentioned technical proposal, the step 8, the terminate liquid of addition is water, and the terminate liquid is added in total amount and step 1
The ratio of the water quality is terminate liquid: water=15~25:1.
In above-mentioned technical proposal, follow the steps below:
Step 1, be water by mass ratio: 50wt% glyoxalic acid solution=1:14~16 mixture carries out constant temperature stirring,
The constant temperature whipping temp is -30 DEG C~-25 DEG C, stirring rate 400rpm；
Step 2, after starting stirring, the 98wt% concentrated sulfuric acid is added dropwise in Xiang Suoshu mixture, dripping quantity per minute is described mixed
0.03~0.07 times for closing amount of substance, is added dropwise the 98wt% concentrated sulfuric acid total amount and the mass ratio of water described in step 1 is
The 98wt% concentrated sulfuric acid: water=12~14:1, whipping temp are -30 DEG C~-20 DEG C；
Step 3, after all 98wt% concentrated sulfuric acids are added dropwise to complete, continue 20~30min of stirring, whipping temp -30
DEG C~-25 DEG C；
Step 4,3,4- methylene-dioxy mandelic acid is added into the solution after the completion of step 3,3,4- methylene two is added
The mass ratio of water described in the amount and step 1 of oxygroup mandelic acid is 3,4- methylene-dioxy mandelic acid: water=0.3~0.4:
1；
Step 5, the solution after the completion of step 4 is emulsified, 11~12Kr/min of emulsifying rate, when emulsification is added dropwise simultaneously
Piperonyl cyclonene, dripping quantity per minute are 0.5~0.6 times of water quality described in step 1,3~5min of emulsification times；
Step 6, the step 5 is repeated as many times, every time between be spaced 3~10min, be added in piperonyl cyclonene total amount and step 1
The mass ratio of the water is piperonyl cyclonene: water=10~11:1；
Step 7, the solution after step 6 is passed through into the loop reactor with venturi-type eductors after mixing,
Into suspended-bed reactor, the reaction was continued, and temperature is 0 DEG C~5 DEG C in the suspended-bed reactor, described to have venturi injection
The loop reactor outer circulation circuit of device is provided with heat exchanger, and the taphole temperature of the heat exchanger is -25 DEG C~-20
DEG C, bubble diameter is 0.03~0.05mm in the loop reactor, and gas flow is in step 1 in the venturi-type eductors
100~150 times/min of the volume of mixture, 4~8min of mixed reaction time in the suspended-bed reactor；
Step 8, terminate liquid is added into the solution after step 7, the terminate liquid is added described in total amount and step 1
The ratio of water quality is terminate liquid: water=15~20:1, terminates reaction, obtains product；
It further include the process of the air-blowing into solution during the step 1~step 6, air-blowing amount per minute is in step 1
12~20 times of the volume of mixture.
In above-mentioned technical proposal, the air-blowing medium that the air-blowing process uses is nitrogen.
A kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid, including jacket type distributor stirred tank,
Sulfuric acid gauge tank, jacket type distributor emulsifying kettle, jacket type distributor product stirred tank, the circuit with venturi-type eductors are anti-
Answer device, cyclic suspension bed reactor, piperonyl cyclonene measuring tank, thermostat, filter plant, charge pump, air accumulator, filtrate receiver is described
Sulfuric acid gauge tank outlet is connected with jacket type distributor stirred tank pipeline, and pipeline company is respectively adopted in the thermostat circulation fluid outlet
Connect the heat exchange of the jacket inlet of the jacket type distributor stirred tank, the jacket inlet, heat exchanger of jacket type distributor emulsifying kettle
Pipeline company is respectively adopted in the jacket inlet of medium inlet and jacket type distributor product stirred tank, the thermostat circulation fluid entrance
Connect the heat exchange of the jacket outlet of the jacket type distributor stirred tank, the jacket outlet, heat exchanger of jacket type distributor emulsifying kettle
The jacket outlet of media outlet and jacket type distributor product stirred tank, the outlet and charging of the jacket type distributor stirred tank
The inlet duct of pump is connected, and the outlet of the piperonyl cyclonene measuring tank is connected with jacket type distributor emulsifying kettle pipeline, the collet
The outlet of formula distributor emulsifying kettle is connected with the liquid phase inlet duct of the loop reactor with venturi-type eductors, the tool
There is the loop reactor outlet of venturi-type eductors to be connected with the inlet duct of the cyclic suspension bed reactor, the circulation is outstanding
The outlet of floating bed reactor is connected with the jacket type distributor product stirred tank inlet duct, the jacket type distributor product
Stirred tank outlet is connect with the feed inlet pipeline of the filter plant, and the outlet of the air accumulator is respectively adopted described in pipeline connection
The gas distribution tube entrance and folder of the gas distribution tube entrance of jacket type distributor stirred tank, the jacket type distributor emulsifying kettle
Shell type distributor product stirred tank gas distribution tube entrance, the filter plant liquid-phase outlet connect the filtrate receiver entrance.
In above-mentioned technical proposal, the loop reactor with venturi-type eductors includes venturi-type eductors, high pressure
Reaction kettle, loop circulator pump and heat exchanger, wherein the top in the autoclave is arranged in the venturi-type eductors, it is high
Pressure reaction kettle lower part is provided with material outlet and loop exit, and the loop exit is connect with the entrance of the loop circulator pump,
The outlet of the loop circulator pump connects the material inlet of the heat exchanger, and the material outlet of the heat exchanger connects the high pressure
Material inlet at the top of reaction kettle.
In above-mentioned technical proposal, the sulfuric acid gauge tank and piperonyl cyclonene measuring tank outlet are provided with flowmeter.
In above-mentioned technical proposal, the top of the jacket type distributor stirred tank is arranged in the sulfuric acid gauge tank, described
Piperonyl cyclonene measuring tank is arranged above the jacket type distributor emulsifying kettle.
In above-mentioned technical proposal, jacket inlet pipe, the jacket type distributor emulsifying kettle of the jacket type distributor stirred tank
Jacket inlet pipe, be all provided on the heat transferring medium inlet tube of heat exchanger and the jacket inlet pipe of jacket type distributor product stirred tank
It is equipped with fluid flowmeter.
In above-mentioned technical proposal, gas distribution tube inlet tube, the jacket type distributor of the jacket type distributor stirred tank
The gas distribution tube inlet tube of emulsifying kettle, the gas inlet pipe and jacket type distributor product stirred tank of the venturi-type eductors
Gas flowmeter is provided on gas distribution tube inlet tube.
In above-mentioned technical proposal, it is provided with emulsifier unit on the jacket type distributor emulsifying kettle and scrapes wall agitating device.
In above-mentioned technical proposal, it is provided with 2 sets of emulsifier units on the jacket type distributor emulsifying kettle and scrapes wall stirring dress
It sets.
In above-mentioned technical proposal, the filter plant can be multiple stage filter units.
In above-mentioned technical proposal, the filter plant can be 2 grades of filter plants.
In above-mentioned technical proposal, temperature is mounted on the jacket type distributor stirred tank and jacket type distributor emulsifying kettle
Degree detection instrument.
It the advantages of the utility model and has the beneficial effect that
1, the method that 3,4- methylene-dioxy mandelic acid is synthesized in the utility model is closed using enhancing emulsion process
At method, this method prepare nitration mixture and emulsification synthesis process in gas is all passed through into reaction system, make in reaction system
A large amount of bubbles are generated, so that reaction-ure surface product be made to increase, increase the contact area between reactant, turning for reaction can be improved
Rate and yield.
2, the utility model carries out the synthesis of 3,4- methylene-dioxy mandelic acid using the method for emulsification, sharp in synthesis
It is acted on the homogeneous of emulsion process, is uniformly dispersed in piperonyl cyclonene in glyoxalic acid with minimum drop, reactant can be improved
Between contacting efficiency, improve product purity and yield.
3, the emulsifier that the utility model uses is 3,4- methylene-dioxy mandelic acid, and this method is according to 3,4- methylene two
The existing lipophilic group of oxygroup mandelic acid has the principle of hydrophilic group again, stable newborn using product as can both be formed for emulsifier
Compound system and the substance outside reaction system is not introduced, makes product separation process is simpler to be easy.
4, the utility model is during the reaction using having the loop reactor of venturi-type eductors and cyclic suspension bed
Solution after emulsification is dispersed into fine drop by reactor, forms countless microresponse systems, and independent reaction increases heat and mass
Efficiency inhibits to cause to lead to the problem of by-product due to heat transfer uneven two.
5, using the loop reactor with venturi-type eductors in the utility model, wherein unique reinforcing mixing knot
Structure --- venturi-type eductors, venturi-type eductors (instead of gas distributor or other gas spreading systems) are a kind of high-performance
Liqiud-gas mixing device.It is made of four parts, turbulent flow nozzle, gas chamber, gas circulation line and Guan Zucheng.It is logical to pump liquid
It crosses nozzle and forms quick injection stream and take gas injection in gas chamber and go out, form energy consumption on hydraulic shock to tube wall.This wound
Strong mixing vibration area is made, in this each region, fierce turbulent flow makes the good spreading of foam.Impact the gas bubble generated
Foam is very small, and gas liquid ratio has reached 0.5~2.0 or more simultaneously.So this is the reason that loop reactor carries out gas liquid reaction
The initial main dispersal device thought has reached initial most important mass transfer function, and then, gas-fluid two-phase mixture is sprayed
In liquid storage into autoclave.Autoclave does not need setting baffle, and compared to for autoclave stirred reactor, it is logical
Often there is a big ratio of height to diameter, such ratio of height to diameter can reduce manufacturing cost, and the loop reactor for high pressure is manufactured with regard to phase
Work as saving.It is ejected into autoclave to cause by the spouting two-phase mixture of venturi-type eductors above and be swashed for the second time
Strong mixing, the mass transfer performance realized again.Current mass transfer is completed by the minute bubbles in reaction kettle, and the diameter of minute bubbles exists
Between 0.03~0.07mm, this bubble diameter is greater than the bubble in venturi injection gas, this is because venturi-type eductors
In minute bubbles the polymerization of bubble has occurred at this time.
External heat exchanger (instead of coil pipe or built-in heat exchanger) is, big compared with previous built-in heat exchanger
It is small not by the volumetric constraint of reaction vessel (reaction kettle).External heat exchanger heat exchange area can work entirely, or even reduce work
In the case where making volume, such as semi-batch operation or half kettle material reaction.
Loop circulator pump (instead of blender) reaches very high working volume output, is needed with reaching high mass transfer efficiency formation
It asks.New circulating pump can convey high solids content (more mass fraction 8%) and high airload (volume fraction 30% gas
Foam) reaction mixture.
Detailed description of the invention
Fig. 1 is a kind of flow diagram of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid.
Fig. 2 is the schematic diagram of the utility model embodiment 3.
Fig. 3 is the schematic diagram of the loop reactor in the utility model embodiment 3 with venturi-type eductors.
Fig. 4 is the schematic diagram of the utility model embodiment 4.
Wherein:
1: jacket type distributor stirred tank, 2: sulfuric acid gauge tank, 3: jacket type distributor emulsifying kettle, 4: piperonyl cyclonene metering
Slot, 5: thermostat, 6: filter plant, 7: charge pump, 8: air accumulator, 9: filtrate receiver；12: jacket type distributor product stirred tank,
13: the loop reactor with venturi-type eductors, 14: cyclic suspension bed reactor；
6-1: by-pass filtration equipment, 6-2: secondary filtration equipment, 10-1: first gas flowmeter, 10-2: second gas stream
Meter, 10-3: third gas flowmeter, the 10-4: the four gas flowmeter, the 11-1: the first fluid flowmeter, the 11-2: the second liquid
Flowmeter body, 11-3: third fluid flowmeter, the 11-4: the four fluid flowmeter, 13-1: autoclave, 13-2: circuit is followed
Ring pump, 13-3: heat exchanger, 13-4: venturi-type eductors.
It for those of ordinary skill in the art, without creative efforts, can be according to above attached
Figure obtains other relevant drawings.
Specific embodiment
In order to make those skilled in the art better understand the scheme of the utility model, combined with specific embodiments below into one
Step illustrates the technical solution of the utility model.
Comparative example
1. claiming piperonyl cyclonene 100g, water 10g, 50% glyoxalic acid solution 160g, 98% concentrated sulfuric acid 140g.
2. water 10g and 50% glyoxalic acid solution 160g is added in jacketed reactor.
It is 5 DEG C by thermostat set temperature 3. jacketed reactor is connect with thermostat, operation thermostat cooling half an hour
With in collet fluid temperature reach 5 DEG C.
4. electric mixer is connected, with the liquid in plastic stir blade stirring jacketed reactor, revolving speed 400r/min
5. the 140g concentrated sulfuric acid is at the uniform velocity added dropwise dropwise with constant pressure funnel, speed control is in 7g/min, after dripping, continues to stir
30min.Obtain nitration mixture.
6. the nitration mixture for accounting for nitration mixture gross mass 70% is removed jacketed reactor, refrigerated in 5 DEG C of environment.
7. 30g piperonyl cyclonene is at the uniform velocity added dropwise dropwise into jacketed reactor with constant pressure funnel, speed control is in 3g/min.It is added dropwise
After complete, continue to stir 30min.
8. 70% nitration mixture at the uniform velocity removed in a dropping step 6 dropwise with constant pressure funnel into jacketed reactor is (when dropwise addition
Between be 1h) and 70g piperonyl cyclonene (time for adding be in 0.5h).
9. after completion of dropwise addition, mixing plant speed being adjusted to 500r/min, continues to be stirred to react 35min
10. into jacketed reactor plus 200mL water terminates reaction.
11. being filtered with 1L bottle,suction, solid is obtained, is weighed, it is dry, it is detected with liquid chromatography.
12. through detecting yield 71.42%, purity 68.54%, total recovery 44.64%.
Embodiment 1
A kind of method of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid, follows the steps below:
Step 1, the mixture of water 10g, 50wt% glyoxalic acid solution 160g is subjected to constant temperature stirring, the constant temperature stirring
Temperature is -25 DEG C, stirring rate 400rpm；
Step 2, after starting stirring, the 98wt% concentrated sulfuric acid, dripping quantity 7g/min per minute, drop are added dropwise in Xiang Suoshu mixture
Add the 98wt% concentrated sulfuric acid total amount 140g, whipping temp is -25 DEG C, stirring rate 400rpm；
Step 3, after all 98wt% concentrated sulfuric acids are added dropwise to complete, continue stir 30min, -25 DEG C of whipping temp；
Step 4,3,4- methylene-dioxy mandelic acid and benzyl triethyl ammonium chlorination are added into the solution after the completion of step 3
Ammonium is added the amount 4g of 3,4- methylene-dioxy mandelic acid, the amount 8g of benzyltriethylammoinium chloride is added；
Step 5, the solution after the completion of step 4 is emulsified, emulsifying rate 12Kr/min, pepper is added dropwise when emulsification simultaneously
Ring, dripping quantity per minute are 5g, emulsification times 5min；
Step 6, the step 5 is repeated 4 times, every time between be spaced 3min, piperonyl cyclonene total amount 100g is added；
Step 7, the solution after step 6 is passed through into the loop reactor with venturi-type eductors after mixing,
Into suspended-bed reactor, the reaction was continued, and temperature is 5 DEG C in the suspended-bed reactor, the returning with venturi-type eductors
Road reactor outer circulation circuit is provided with heat exchanger, and the taphole temperature of the heat exchanger is -25 DEG C~-20 DEG C, institute
Stating bubble diameter in loop reactor is 0.03mm, and gas flow is 20L/min in the venturi-type eductors, in the suspension
Mixed reaction time 5min in bed reactor；
Step 8,200ml water is added into the solution after step 7, terminates reaction, obtains product；
It further include the air-blowing process into solution during the step 1~step 6, air-blowing amount per minute is 2.5L/min,
The air-blowing medium used is nitrogen.
Through detecting purity 98.00%, total recovery 95.20%.
Embodiment 2
A kind of method of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid, follows the steps below:
Step 1, the mixture of water 10g, 50wt% glyoxalic acid solution 200g is subjected to constant temperature stirring, the constant temperature stirring
Temperature is -30 DEG C, stirring rate 430rpm；
Step 2, after starting stirring, the 98wt% concentrated sulfuric acid, dripping quantity 9g/min per minute, drop are added dropwise in Xiang Suoshu mixture
Add the 98wt% concentrated sulfuric acid total amount 150g, whipping temp is -28 DEG C, stirring rate 430rpm；
Step 3, after all 98wt% concentrated sulfuric acids are added dropwise to complete, continue stir 30min, -28 DEG C of whipping temp；
Step 4,3,4- methylene-dioxy mandelic acid is added into the solution after the completion of step 3,3,4- methylene two is added
The amount 9g of oxygroup mandelic acid；
Step 5, the solution after the completion of step 4 is emulsified, emulsifying rate 15Kr/min, pepper is added dropwise when emulsification simultaneously
Ring, dripping quantity per minute are 5g, emulsification times 7min；
Step 6, step 5 step is repeated 4 times, every time between be spaced 3min, piperonyl cyclonene total amount 140g is added；
Step 7, the solution after step 6 is passed through into the loop reactor with venturi-type eductors after mixing,
Into suspended-bed reactor, the reaction was continued, and temperature is 7 DEG C in the suspended-bed reactor, the returning with venturi-type eductors
Road reactor outer circulation circuit is provided with heat exchanger, and the taphole temperature of the heat exchanger is -20 DEG C, and the circuit is anti-
Answering bubble diameter in device is 0.03mm, and gas flow is 25L/min in the venturi-type eductors, in the suspended-bed reactor
In mixed reaction time 4min；
Step 8,200ml water is added into the solution after step 7, terminates reaction, obtains product；
It further include the air-blowing process into solution during the step 1~step 6, air-blowing amount per minute is 2.5L/min,
The air-blowing medium used is nitrogen.
Through detecting purity 97.53%, total recovery 91.43%.
Embodiment 3
A kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid, including jacket type distributor stirred tank,
Sulfuric acid gauge tank, jacket type distributor emulsifying kettle, jacket type distributor product stirred tank, the circuit with venturi-type eductors are anti-
Answer device, cyclic suspension bed reactor, piperonyl cyclonene measuring tank, thermostat, filter plant, charge pump, air accumulator, filtrate receiver is described
Sulfuric acid gauge tank outlet is connected with jacket type distributor stirred tank pipeline, and the sulfuric acid gauge tank setting is distributed in the jacket type
The folder that pipeline connects the jacket type distributor stirred tank is respectively adopted in the top of device stirred tank, the thermostat circulation fluid outlet
Set entrance, the jacket inlet of jacket type distributor emulsifying kettle, the heat transferring medium entrance of heat exchanger and jacket type distributor product stir
The jacket inlet of kettle is mixed, the folder that pipeline connects the jacket type distributor stirred tank is respectively adopted in the thermostat circulation fluid entrance
Set outlet, the heat transferring medium outlet of the jacket outlet of jacket type distributor emulsifying kettle, heat exchanger and jacket type distributor product stir
The jacket outlet of kettle is mixed, the outlet of the jacket type distributor stirred tank is connected with the inlet duct of charge pump, the piperonyl cyclonene
The outlet of measuring tank is connected with jacket type distributor emulsifying kettle pipeline, and the setting of piperonyl cyclonene measuring tank is in the jacket type distributor cream
Change above kettle, the sulfuric acid gauge tank and piperonyl cyclonene measuring tank outlet are provided with flowmeter, the jacket type distributor cream
Change and is provided with 2 sets of emulsifier units on kettle and scrapes wall agitating device.The loop reactor with venturi-type eductors includes text
Injector, autoclave, loop circulator pump and heat exchanger in mound, wherein venturi-type eductors setting is anti-in the high pressure
The top in kettle is answered, autoclave lower part is provided with material outlet and loop exit, and the loop exit is followed with the circuit
The entrance connection of ring pump, the outlet of the loop circulator pump connect the material inlet of the heat exchanger, the material of the heat exchanger
Outlet connects the material inlet at the top of the autoclave.The jacket type distributor emulsifying kettle outlet has literary mound with described
In injector loop reactor the loop circulator pump entrance connection, the circuit with venturi-type eductors is reacted
The material outlet of the autoclave lower part setting of device is connected with the inlet duct of the cyclic suspension bed reactor, the circulation
The outlet of suspended-bed reactor is connected with the jacket type distributor product stirred tank inlet duct, and the jacket type distributor produces
The outlet of product stirred tank is connect with the feed inlet pipeline of the filter plant, and pipeline connection institute is respectively adopted in the outlet of the air accumulator
State the gas distribution tube entrance of jacket type distributor stirred tank, the gas distribution tube entrance of the jacket type distributor emulsifying kettle,
The gas access of the venturi-type eductors of loop reactor and jacket type distributor product stirred tank gas distribution tube entrance, it is described
Filter plant liquid-phase outlet connects the filtrate receiver entrance, the jacket type distributor stirred tank and jacket type distributor emulsifying kettle
On be mounted on temperature instrument.
The jacket inlet pipe of the jacket type distributor stirred tank, jacket type distributor emulsifying kettle jacket inlet pipe, change
Fluid flowmeter is provided on the heat transferring medium inlet tube of hot device and the jacket inlet pipe of jacket type distributor product stirred tank.
The gas distribution tube entrance of the gas distribution tube inlet tube of the jacket type distributor stirred tank, jacket type distributor emulsifying kettle
It manages, is all provided in the gas inlet pipe and jacket type distributor product stirred tank gas distribution tube inlet tube of the venturi-type eductors
It is equipped with gas flowmeter.
Embodiment 4
A kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid, including jacket type distributor stirred tank,
Sulfuric acid gauge tank, jacket type distributor emulsifying kettle, jacket type distributor product stirred tank, the circuit with venturi-type eductors are anti-
Answer device, cyclic suspension bed reactor, piperonyl cyclonene measuring tank, thermostat, filter plant, charge pump, air accumulator, filtrate receiver is described
Sulfuric acid gauge tank outlet is connected with jacket type distributor stirred tank pipeline, and the sulfuric acid gauge tank setting is distributed in the jacket type
The folder that pipeline connects the jacket type distributor stirred tank is respectively adopted in the top of device stirred tank, the thermostat circulation fluid outlet
Set entrance, the jacket inlet of jacket type distributor emulsifying kettle, the heat transferring medium entrance of heat exchanger and jacket type distributor product stir
The jacket inlet of kettle is mixed, the folder that pipeline connects the jacket type distributor stirred tank is respectively adopted in the thermostat circulation fluid entrance
Set outlet, the heat transferring medium outlet of the jacket outlet of jacket type distributor emulsifying kettle, heat exchanger and jacket type distributor product stir
The jacket outlet of kettle is mixed, the outlet of the jacket type distributor stirred tank is connected with the inlet duct of charge pump, the piperonyl cyclonene
The outlet of measuring tank is connected with jacket type distributor emulsifying kettle pipeline, and the setting of piperonyl cyclonene measuring tank is in the jacket type distributor cream
Change above kettle, the sulfuric acid gauge tank and piperonyl cyclonene measuring tank outlet are provided with flowmeter, the jacket type distributor cream
Change and is provided with 2 sets of emulsifier units on kettle and scrapes wall agitating device.The loop reactor with venturi-type eductors includes text
Injector, autoclave, loop circulator pump and heat exchanger in mound, wherein venturi-type eductors setting is anti-in the high pressure
The top in kettle is answered, autoclave lower part is provided with material outlet and loop exit, and the loop exit is followed with the circuit
The entrance connection of ring pump, the outlet of the loop circulator pump connect the material inlet of the heat exchanger, the material of the heat exchanger
Outlet connects the material inlet at the top of the autoclave.The jacket type distributor emulsifying kettle outlet has literary mound with described
In injector loop reactor the loop circulator pump entrance connection, the circuit with venturi-type eductors is reacted
The material outlet of the autoclave lower part setting of device is connected with the inlet duct of the cyclic suspension bed reactor, the circulation
The outlet of suspended-bed reactor is connected with the jacket type distributor product stirred tank inlet duct, and the jacket type distributor produces
Product stirred tank outlet connect with the feed inlet pipeline of the by-pass filtration equipment, the discharge port of the by-pass filtration equipment with it is described
The feed inlet pipeline of secondary filtration equipment connects, and the outlet of the air accumulator is respectively adopted pipeline and connects the jacket type distributor
The gas distribution tube entrance of stirred tank, the gas distribution tube entrance of the jacket type distributor emulsifying kettle, loop reactor text
The gas access of injector and jacket type distributor product stirred tank gas distribution tube entrance, the secondary filtration equipment liquid in mound
Mutually outlet connects the filtrate receiver entrance, is mounted on the jacket type distributor stirred tank and jacket type distributor emulsifying kettle
Temperature instrument.
The jacket inlet pipe of the jacket type distributor stirred tank, jacket type distributor emulsifying kettle jacket inlet pipe, change
Fluid flowmeter is provided on the heat transferring medium inlet tube of hot device and the jacket inlet pipe of jacket type distributor product stirred tank.
The gas distribution tube entrance of the gas distribution tube inlet tube of the jacket type distributor stirred tank, jacket type distributor emulsifying kettle
It manages, is all provided in the gas inlet pipe and jacket type distributor product stirred tank gas distribution tube inlet tube of the venturi-type eductors
It is equipped with gas flowmeter.
By-pass filtration equipment and secondary filtration equipment use the filter medium of different accuracy, use in by-pass filtration equipment
Filtration media pore diameters are larger, the product of granularity larger in product system can be filtered out, filtrate enters secondary filtration and sets
Standby, secondary filtration equipment is smaller using filtration media pore diameters, can filter out the smaller final products 3 of granularity, 4- methylene-dioxy
Mandelic acid, Product recycling are more abundant.
Illustrative description has been done to the utility model above, it should explanation, in the core for not departing from the utility model
In the case where the heart, it is any it is simple deformation, modification or other skilled in the art can not spend creative work etc.
The protection scope of the utility model is each fallen with replacement.
Claims (10)
1. a kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid, which is characterized in that be distributed including jacket type
Device stirred tank, sulfuric acid gauge tank, jacket type distributor emulsifying kettle, jacket type distributor product stirred tank have venturi injection
The loop reactor of device, cyclic suspension bed reactor, piperonyl cyclonene measuring tank, thermostat, filter plant, charge pump, air accumulator, filter
Liquid bath, the sulfuric acid gauge tank outlet are connected with jacket type distributor stirred tank pipeline, thermostat circulation fluid outlet difference
The jacket inlet of the jacket type distributor stirred tank is connected using pipeline, the jacket inlet of jacket type distributor emulsifying kettle, is changed
The heat transferring medium entrance of hot device and the jacket inlet of jacket type distributor product stirred tank, the thermostat circulation fluid entrance difference
The jacket outlet of the jacket type distributor stirred tank is connected using pipeline, the jacket outlet of jacket type distributor emulsifying kettle, is changed
The jacket outlet of the heat transferring medium outlet and jacket type distributor product stirred tank of hot device, the jacket type distributor stirred tank
Outlet is connected with the inlet duct of charge pump, outlet and the jacket type distributor emulsifying kettle pipeline phase of the piperonyl cyclonene measuring tank
Even, the liquid phase inlet duct of jacket type distributor the emulsifying kettle outlet and the loop reactor with venturi-type eductors
It is connected, the inlet duct phase of the loop reactor outlet and the cyclic suspension bed reactor with venturi-type eductors
Even, the outlet of the cyclic suspension bed reactor is connected with the jacket type distributor product stirred tank inlet duct, the folder
The outlet of shell type distributor product stirred tank is connect with the feed inlet pipeline of the filter plant, and the outlet of the air accumulator is adopted respectively
The gas distribution tube entrance of the jacket type distributor stirred tank, the gas of the jacket type distributor emulsifying kettle are connected with pipeline
Tube inlet and jacket type distributor product stirred tank gas distribution tube entrance are distributed, described in the filter plant liquid-phase outlet connection
Filtrate receiver entrance.
2. a kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
Be, the loop reactor with venturi-type eductors include venturi-type eductors, autoclave, loop circulator pump and
Heat exchanger, wherein the top in the autoclave is arranged in the venturi-type eductors, autoclave lower part is provided with
Material outlet and loop exit, the loop exit are connect with the entrance of the loop circulator pump, and the loop circulator pump goes out
Mouth connects the material inlet of the heat exchanger, and the material that the material outlet of the heat exchanger connects at the top of the autoclave enters
Mouthful.
3. a kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, the sulfuric acid gauge tank and piperonyl cyclonene measuring tank outlet are provided with flowmeter.
4. a kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, the top of the jacket type distributor stirred tank is arranged in the sulfuric acid gauge tank, and the piperonyl cyclonene measuring tank setting exists
Above the jacket type distributor emulsifying kettle.
5. a kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, jacket inlet pipe, the heat exchanger of the jacket inlet pipe of the jacket type distributor stirred tank, jacket type distributor emulsifying kettle
Heat transferring medium inlet tube and jacket type distributor product stirred tank jacket inlet pipe on be provided with fluid flowmeter.
6. a kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, the gas distribution tube of the gas distribution tube inlet tube of the jacket type distributor stirred tank, jacket type distributor emulsifying kettle
Inlet tube, in the gas inlet pipe and jacket type distributor product stirred tank gas distribution tube inlet tube of the venturi-type eductors
It is provided with gas flowmeter.
7. a kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, emulsifier unit is provided on the jacket type distributor emulsifying kettle and scrapes wall agitating device.
8. a kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, 2 sets of emulsifier units are provided on the jacket type distributor emulsifying kettle and scrapes wall agitating device.
9. a kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, the filter plant can be multiple stage filter units.
10. a kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, is mounted on temperature instrument on the jacket type distributor stirred tank and jacket type distributor emulsifying kettle.
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|---|---|---|---|
| CN201821391924.9U CN208776619U (en) | 2018-08-28 | 2018-08-28 | A kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821391924.9U CN208776619U (en) | 2018-08-28 | 2018-08-28 | A kind of device of enhancing emulsification synthesis 3,4- methylene-dioxy mandelic acid |
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2018
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