CN208632423U - A kind of device of emulsifying process synthesis 3,4- methylene-dioxy mandelic acid - Google Patents
A kind of device of emulsifying process synthesis 3,4- methylene-dioxy mandelic acid Download PDFInfo
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Abstract
The utility model discloses a kind of emulsifying process synthesis 3, the device of 4- methylene-dioxy mandelic acid, the device includes jacket type distributor stirred tank, sulfuric acid gauge tank, jacket type distributor emulsifying kettle, piperonyl cyclonene measuring tank, thermostat, filter plant, charge pump, air accumulator, filtrate receiver may be implemented all to be passed through gas into reaction system in preparing nitration mixture and emulsification synthesis process, make to generate a large amount of bubbles in reaction system, to make reaction-ure surface product increase, increases the contact area between reactant, the conversion ratio and yield of reaction can be improved.And during the reaction with addition sponge, multiple small reaction systems can be formed in emulsion reactor, it solves uneven because conducting heat, local reaction temperature is possible excessively high and piperonyl cyclonene is caused further to react the problem for generating by-product urheen acid with product, viscous product is dispersed into bulk simultaneously, increases mobility by carrier of sponge, thus the selectivity and yield of the reaction improved, the technical process of emulsifying process synthesis 3,4- methylene-dioxy mandelic acid can be efficiently completed.
Description
Technical field
The utility model belongs to technical field of chemical engineering, and in particular to a kind of emulsifying process 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 emulsifying process synthesis 3,4- methylene two
Two-phase object mixing efficiency in reaction system can be improved in the device of oxygroup mandelic acid, the utility model, improves reaction speed, shortens
Reaction time improves reaction yield, and reduces the wastewater flow rate generated in reaction process.
The utility model is achieved through the following technical solutions:
A kind of method of emulsifying process 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 the quality of water 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 the quality of water 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, transferring film sponge is added into the solution after step 6, and carries out constant temperature stirring, 0 DEG C of whipping temp~
10 DEG C, stirring rate 400rpm~600rpm, mixing time is 20min~40min；
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 7, 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=0.4~1:1.
In above-mentioned technical proposal, piperonyl cyclonene is added dropwise simultaneously when emulsification, often in the step 5,12~15Kr/min of emulsifying rate
Minute dripping quantity is 0.5~1 times of the water quality, 5~10min of emulsification times.
In above-mentioned technical proposal, the step 6, step 5 step is repeated 3~8 times, every time between interval 3~
10min, the ratio that piperonyl cyclonene total amount and the water quality is added is piperonyl cyclonene: water=10~12:1.
In above-mentioned technical proposal, the step 7, the addition transferring film sponge is 0.8~1.2cm of volume3Particle, be added
Total amount be step 6 step at the end of obtain 0.5~1.2 times of solution body accumulated amount.
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 -25 DEG C~-23 DEG C, 400~420rpm of stirring rate；
Step 2, after starting stirring, the 98wt% concentrated sulfuric acid is added dropwise in Xiang Suoshu mixture, dripping quantity per minute is described mixed
0.03~0.05 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 -25 DEG C~-23 DEG C；
Step 3, after all 98wt% concentrated sulfuric acids are added dropwise to complete, continue 20~30min of stirring, whipping temp -25
DEG C~-23 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=0.1~0.4:
1；
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 0.3~0.5 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=10~12:1；
Step 7, transferring film sponge is added into the solution after step 6, and carries out constant temperature stirring, 0 DEG C of whipping temp~
10 DEG C, stirring rate 400rpm~600rpm, mixing time is 20min~40min；
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=20~25:1, terminates reaction, obtains product；
It further include the process of the air-blowing into solution during the step 1~step 7, air-blowing amount per minute is the mixing
7~15 times of object product.
In above-mentioned technical proposal, the air-blowing medium that the air-blowing process uses is nitrogen.
A kind of device of emulsifying process synthesis 3,4- methylene-dioxy mandelic acid, including jacket type distributor stirred tank,
Sulfuric acid gauge tank, jacket type distributor emulsifying kettle, piperonyl cyclonene measuring tank, thermostat, filter plant, charge pump, air accumulator, filtrate
Slot, the sulfuric acid gauge tank outlet are connected with jacket type distributor stirred tank pipeline, and the thermostat circulation fluid outlet is adopted respectively
The jacket inlet of the jacket type distributor stirred tank and the jacket inlet of jacket type distributor emulsifying kettle are connected with pipeline, it is described
The jacket outlet and jacket type distribution that pipeline connects the jacket type distributor stirred tank is respectively adopted in thermostat circulation fluid entrance
The outlet of the jacket outlet of device emulsifying kettle, the jacket type distributor stirred tank is connected with the inlet duct of charge pump, the Hu
The outlet of green pepper ring measuring tank is connected with jacket type distributor emulsifying kettle pipeline, jacket type distributor emulsifying kettle outlet with it is described
The feed inlet pipeline of filter plant connects, and the outlet of the air accumulator is respectively adopted pipeline and connects the jacket type distributor stirring
The gas distribution tube entrance of the gas distribution tube entrance of kettle and the jacket type distributor emulsifying kettle, the filter plant liquid phase go out
Mouth connects the filtrate receiver entrance.
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 jacket inlet pipe and jacket type distributor emulsifying kettle of the jacket type distributor stirred tank
Jacket inlet pipe on be provided with fluid flowmeter.
In above-mentioned technical proposal, the gas distribution tube inlet tube and jacket type distributor of the jacket type distributor stirred tank
Gas flowmeter is provided on the gas distribution tube inlet tube of emulsifying kettle.
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 is multiple stage filter units.
In above-mentioned technical proposal, the filter plant is 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 emulsification 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 can form multiple small reactions during the reaction with addition sponge in emulsion reactor
System, solution is uneven because conducting heat, and local reaction temperature is possible excessively high and piperonyl cyclonene is caused further to react generation pair with product
The problem of product urheen acid, while viscous product is dispersed into bulk, increase mobility by carrier of sponge, so that improves is anti-
The selectivity and yield answered.
Detailed description of the invention
Fig. 1 is a kind of flow diagram of emulsifying process 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 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；
6-1: by-pass filtration equipment, 6-2: secondary filtration equipment, 10-1: first gas flowmeter, 10-2: second gas stream
Meter, the 11-1: the first fluid flowmeter, 11-2: second liquid flowmeter.
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 up to
Fluid temperature reaches 5 DEG C in collet.
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 emulsifying process 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 is added into the solution after the completion of step 3,3,4- methylene two is added
The amount 4g of oxygroup mandelic acid；
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 7,1cm × 1cm × 1cm transferring film sponge (brand western is added into the solution after step 6
Blot, product batch number G6002, article No.: 151837) totally 400 piece, and constant temperature stirring is carried out, and 5 DEG C of whipping temp, stirring rate
500rpm, mixing time 30min；
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 7, air-blowing amount per minute is 2.5L/min,
The air-blowing medium used is nitrogen.
Through detecting purity 98.48%, total recovery 92.32%.
Embodiment 2
A kind of method of emulsifying process 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 450rpm；
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 -30 DEG C, stirring rate 450rpm；
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 is added into the solution after the completion of step 3,3,4- methylene two is added
The amount 8g 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 4.7g, emulsification times 8min；
Step 6, the step 5 is repeated 4 times, every time between be spaced 3min, piperonyl cyclonene total amount 150g is added；
Step 7,1cm × 1cm × 1cm transferring film sponge (brand western is added into the solution after step 6
Blot, product batch number G6002, article No.: 151837) totally 600 piece, and constant temperature stirring is carried out, and 5 DEG C of whipping temp, stirring rate
500rpm, mixing time 30min；
Step 8,250ml 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 7, air-blowing amount per minute is 2.5L/min,
The air-blowing medium used is nitrogen.
Through detecting purity 98.37%, total recovery 92.23%.
Embodiment 3
A kind of device of emulsifying process synthesis 3,4- methylene-dioxy mandelic acid, including jacket type distributor stirred tank,
Sulfuric acid gauge tank, jacket type distributor emulsifying kettle, piperonyl cyclonene measuring tank, thermostat, filter plant, charge pump, air accumulator, filtrate
Slot, the sulfuric acid gauge tank outlet are connected with jacket type distributor stirred tank pipeline, and the thermostat circulation fluid outlet is adopted respectively
The jacket inlet of the jacket type distributor stirred tank and the jacket inlet of jacket type distributor emulsifying kettle are connected with pipeline, it is described
Liquid is provided on the jacket inlet pipe of jacket type distributor stirred tank and the jacket inlet pipe of jacket type distributor emulsifying kettle
Flowmeter.The thermostat circulation fluid entrance be respectively adopted pipeline connect the jacket type distributor stirred tank jacket outlet and
The jacket outlet of jacket type distributor emulsifying kettle, the outlet and the inlet duct phase of charge pump of the jacket type distributor stirred tank
Even, the outlet of the piperonyl cyclonene measuring tank is connected with jacket type distributor emulsifying kettle pipeline, the jacket type distributor emulsifying kettle
Outlet is connect with the feed inlet pipeline of the filter plant, and the outlet of the air accumulator is respectively adopted pipeline and connects the jacket type
The gas distribution tube entrance of the gas distribution tube entrance of distributor stirred tank and the jacket type distributor emulsifying kettle, the collet
It is all provided on the gas distribution tube inlet tube of formula distributor stirred tank and the gas distribution tube inlet tube of jacket type distributor emulsifying kettle
It is equipped with gas flowmeter, the filter plant liquid-phase outlet connects the filtrate receiver entrance.The sulfuric acid gauge tank and piperonyl cyclonene
Measuring tank outlet is provided with flowmeter, is respectively mounted on the jacket type distributor stirred tank and jacket type distributor emulsifying kettle
There is temperature instrument, 2 sets of emulsifier units are provided on the jacket type distributor emulsifying kettle and scrape wall agitating device.
When implementing a kind of method of emulsifying process synthesis 3,4- methylene-dioxy mandelic acid of the utility model, in step
5 and step 6 open 2 sets of emulsifier units on the jacket type distributor emulsifying kettle and scrape wall agitating device.It is closed in step 7
2 sets of emulsifier units on the jacket type distributor emulsifying kettle, it is in the open state that wall agitating device is scraped in holding.
Embodiment 4
A kind of device of emulsifying process synthesis 3,4- methylene-dioxy mandelic acid, including jacket type distributor stirred tank,
Sulfuric acid gauge tank, jacket type distributor emulsifying kettle, piperonyl cyclonene measuring tank, thermostat, filter plant, charge pump, air accumulator, filtrate
Slot, the sulfuric acid gauge tank outlet are connected with jacket type distributor stirred tank pipeline, and the thermostat circulation fluid outlet is adopted respectively
The jacket inlet of the jacket type distributor stirred tank and the jacket inlet of jacket type distributor emulsifying kettle are connected with pipeline, it is described
Liquid is provided on the jacket inlet pipe of jacket type distributor stirred tank and the jacket inlet pipe of jacket type distributor emulsifying kettle
Flowmeter.The thermostat circulation fluid entrance be respectively adopted pipeline connect the jacket type distributor stirred tank jacket outlet and
The jacket outlet of jacket type distributor emulsifying kettle, the outlet and the inlet duct phase of charge pump of the jacket type distributor stirred tank
Even, the outlet of the piperonyl cyclonene measuring tank is connected with jacket type distributor emulsifying kettle pipeline, the jacket type distributor emulsifying kettle
Outlet is connect with the feed inlet pipeline of by-pass filtration equipment, the discharge port of the by-pass filtration equipment and secondary filtration equipment into
Material mouth pipeline is connected, and the gas distribution that pipeline connects the jacket type distributor stirred tank is respectively adopted in the outlet of the air accumulator
The gas distribution tube entrance of tube inlet and the jacket type distributor emulsifying kettle, the gas point of the jacket type distributor stirred tank
Gas flowmeter, the second level are provided on the gas distribution tube inlet tube of stringing inlet tube and jacket type distributor emulsifying kettle
Filter plant liquid-phase outlet connects the filtrate receiver entrance.The sulfuric acid gauge tank and piperonyl cyclonene measuring tank outlet are provided with
Temperature instrument is mounted on flowmeter, the jacket type distributor stirred tank and jacket type distributor emulsifying kettle.It is described
It is provided with 2 sets of emulsifier units on jacket type distributor emulsifying kettle and scrapes wall agitating device.
When implementing a kind of method of emulsifying process synthesis 3,4- methylene-dioxy mandelic acid of the utility model, in step
5 and step 6 open 2 sets of emulsifier units on the jacket type distributor emulsifying kettle and scrape wall agitating device.It is closed in step 7
2 sets of emulsifier units on the jacket type distributor emulsifying kettle, it is in the open state that wall agitating device is scraped in holding.
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 transferring film sponge of granularity larger in product system can be filtered out, filtrate enters second level mistake
Equipment is filtered, secondary filtration equipment is smaller using filtration media pore diameters, can filter out final products 3,4- methylenedioxybenzenes second
Alkyd.
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 emulsifying process 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, piperonyl cyclonene measuring tank, thermostat, filter plant, charge pump, storage
Gas tank, filtrate receiver, the sulfuric acid gauge tank outlet are connected with jacket type distributor stirred tank pipeline, and the thermostat circulation fluid goes out
Mouth is respectively adopted pipeline and connects the jacket inlet of the jacket type distributor stirred tank and the collet of jacket type distributor emulsifying kettle
The jacket outlet and folder that pipeline connects the jacket type distributor stirred tank is respectively adopted in entrance, the thermostat circulation fluid entrance
The jacket outlet of shell type distributor emulsifying kettle, the outlet and the inlet duct phase of charge pump of the jacket type distributor stirred tank
Even, the outlet of the piperonyl cyclonene measuring tank is connected with jacket type distributor emulsifying kettle pipeline, the jacket type distributor emulsifying kettle
Outlet is connect with the feed inlet pipeline of the filter plant, and the outlet of the air accumulator is respectively adopted pipeline and connects the jacket type
The gas distribution tube entrance of the gas distribution tube entrance of distributor stirred tank and the jacket type distributor emulsifying kettle, the filtering
Equipment liquid-phase outlet connects the filtrate receiver entrance.
2. a kind of device of emulsifying process 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.
3. a kind of device of emulsifying process synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, the sulfuric acid gauge tank is arranged above the jacket type distributor stirred tank, and the piperonyl cyclonene measuring tank is arranged in institute
State the top of jacket type distributor emulsifying kettle.
4. a kind of device of emulsifying process synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, is all provided on the jacket inlet pipe of the jacket type distributor stirred tank and the jacket inlet pipe of jacket type distributor emulsifying kettle
It is equipped with fluid flowmeter.
5. a kind of device of emulsifying process synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, the gas distribution tube inlet tube of the jacket type distributor stirred tank and the gas distribution tube of jacket type distributor emulsifying kettle
Gas flowmeter is provided on inlet tube.
6. a kind of device of emulsifying process 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.
7. a kind of device of emulsifying process 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.
8. a kind of device of emulsifying process synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, the filter plant is multiple stage filter units.
9. a kind of device of emulsifying process synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, the filter plant is 2 grades of filter plants.
10. a kind of device of emulsifying process 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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