CN208776620U - A kind of device improving emulsification synthesis 3,4- methylene-dioxy mandelic acid - Google Patents
A kind of device improving emulsification synthesis 3,4- methylene-dioxy mandelic acid Download PDFInfo
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- CN208776620U CN208776620U CN201821391966.2U CN201821391966U CN208776620U CN 208776620 U CN208776620 U CN 208776620U CN 201821391966 U CN201821391966 U CN 201821391966U CN 208776620 U CN208776620 U CN 208776620U
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Abstract
The utility model discloses the devices that a kind of improvement emulsifies 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, piperonyl cyclonene measuring tank, thermostat, feed measuring tank, filter plant, charge pump, air accumulator, filtrate receiver.It may be implemented all to be passed through gas into reaction system in preparing nitration mixture and emulsification synthesis process using the present apparatus, so that reaction-ure surface product be made to increase, increase the contact area between reactant, the conversion ratio and yield of reaction can be improved.Using product as emulsifier, both stable emulsion object system can be formed and did not introduced the substance outside reaction system, make product separation process is simpler to be easy, addition water-reducing agent may be implemented and the atent solvents such as methylene chloride, toluene, paraffin oil, naphthenic oil, white oil are added dropwise, the conversion ratio that reaction is improved on the basis of increasing the mobility of product, solves the problems, such as that product is sticky.
Description
Technical field
The utility model belongs to technical field of chemical engineering, and in particular to a kind of improvement 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 (silver nitrate technique study [J] of the medicinal jasminal synthesis of Zhang Kunshui, Huang Han, Chen Yisheng such as Zhang Kunshui
Contemporary Chinese medicinal application .2008,2:53-54.) when studying heliotropin synthetic method, and similar preparation 3 is used,
4- methylene-dioxy mandelic acid.Xi Hongjuan has investigated the factors such as reaction temperature, catalyst concn, raw material proportioning and reaction time
Influence, (the ocean Xi Hongjuan, Gao Zhixian, Wang Jianguo is inquired into sulfuric acid catalyst mechanism of action and the possible reaction mechanism mechanism of reaction
Jasminal 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 improvement 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 improvement emulsification synthesis 3,4- methylene-dioxy mandelic acid, follows the steps below:
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 water quality described in the 98wt% concentrated sulfuric acid total amount and step 1 is added dropwise is 98wt%
The 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, step 5 step is repeated as many times, every time between be spaced 3~10min, piperonyl cyclonene total amount and step is added
The ratio of water quality described in 1 is piperonyl cyclonene: water=10~15:1；
Step 7, to after step 6 solution carry out constant temperature stirring, 0 DEG C~10 DEG C of whipping temp, stirring rate
400rpm~600rpm, mixing time are 20min~40min, and atent solvent and/or water-reducing agent is added dropwise in whipping process；
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 the mixture
7~20 times of volume.
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 step 4 is added described in the amount and step 1 of 3,4- methylene-dioxy mandelic acid
The ratio of water quality is 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 water quality described in step 1,5~10min 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 water quality described in piperonyl cyclonene total amount and step 1 is added is piperonyl cyclonene: water=10~12:1；
In above-mentioned technical proposal, the step 7, the atent solvent is methylene chloride, toluene, paraffin oil, naphthenic oil, white
Oil one of is worked as or any a variety of combination, and dripping quantity per minute is 1.5~3 times of water quality described in step 1, and institute is added dropwise
The gross mass for stating atent solvent is 15~30 times of water quality described in step 1.
In above-mentioned technical proposal, the step 7, the water-reducing agent is polycarboxylate high performance water-reducing agent, is added described poly-
The ratio of water quality described in carboxylic acid series high-performance dehydragent total amount and step 1 is polycarboxylate high performance water-reducing agent: water=0.15
~0.3:1；
In above-mentioned technical proposal, the step 7, the dropwise addition mode of atent solvent is in whipping process, after step 7 beginning
After 10~20 minutes, starting that the atent solvent is added dropwise, dripping quantity per minute is 1.5~3 times of water quality described in step 1,
The gross mass that the atent solvent is added dropwise is 15~30 times of water quality described in step 1.
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.
A kind of device of improvement 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, piperonyl cyclonene measuring tank, thermostat, charging
Measuring tank, filter plant, charge pump, air accumulator, filtrate receiver, the sulfuric acid gauge tank outlet and jacket type distributor stirred tank pipe
Road is connected, thermostat circulation fluid outlet be respectively adopted pipeline connect the jacket type distributor stirred tank jacket inlet,
The jacket inlet of jacket type distributor emulsifying kettle and the jacket inlet of jacket type distributor product stirred tank, the thermostat circulation
The folder that pipeline connects the jacket outlet of the jacket type distributor stirred tank, jacket type distributor emulsifying kettle is respectively adopted in liquid entrance
The jacket outlet of set outlet and jacket type distributor product stirred tank, the outlet of the jacket type distributor stirred tank and charge pump
Inlet duct be connected, the outlet of the piperonyl cyclonene measuring tank is connected with jacket type distributor emulsifying kettle pipeline, and the charging is counted
The outlet of measuring tank is connected with the jacket type distributor product stirred tank pipeline, the jacket type distributor emulsifying kettle outlet and institute
It states jacket type distributor product stirred tank inlet duct to be connected, the jacket type distributor product stirred tank outlet and the filtering
The feed inlet pipeline of equipment connects, and the outlet of the air accumulator is respectively adopted pipeline and connects the jacket type distributor stirred tank
Gas distribution tube entrance, the gas distribution tube entrance of the jacket type distributor emulsifying kettle and jacket 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 sulfuric acid gauge tank, piperonyl cyclonene measuring tank and charging measuring tank outlet are provided with
Flowmeter.
In above-mentioned technical proposal, jacket inlet pipe, the jacket type distributor emulsifying kettle of the jacket type distributor stirred tank
Jacket inlet pipe and jacket type distributor product stirred tank jacket inlet pipe on be provided with fluid flowmeter.
In above-mentioned technical proposal, gas distribution tube inlet tube, the jacket type distributor of the jacket type distributor stirred tank
Gas is provided on the gas distribution tube inlet tube and jacket type distributor product stirred tank gas distribution tube inlet tube of emulsifying kettle
Flowmeter body.
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, 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 emulsion process is improved
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, for the utility model during the reaction with the method for addition water-reducing agent, water-reducing agent can be with oriented attachment in oil phase liquid
Surface is dripped, keeps its surface electrically charged, electrostatic repulsion is generated, plays the peptizaiton of water-reducing agent, makes oily mutually dispersion, increases flowing
Property.Water-reducing agent has lubricating action simultaneously, increases hydrophilic group, forms solvation moisture film, reduces frictional force, makes the product sticky stage
Piperonyl cyclonene mutually more disperse, lubricating action is played in the form of moisture film to be formed, the mass-and heat-transfer process of homogeneous reaction system improves
Product purity and yield.
5, the utility model is during the reaction with inertia such as dropwise addition methylene chloride, toluene, paraffin oil, naphthenic oil, white oils
The method of solvent improves the conversion ratio of reaction on the basis of increasing the mobility of product, solves the problems, such as that product is sticky.With dropwise addition
Mode, preventing methylene chloride or toluene from largely dissolving in reaction system piperonyl cyclonene influences reaction.
Detailed description of the invention
Fig. 1 is a kind of flow diagram for improving emulsification synthesis 3,4- methylene-dioxy mandelic acid.
Fig. 2 is the schematic diagram of the utility model embodiment 4.
Fig. 3 is the schematic diagram of the utility model embodiment 5.
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: charging measuring tank；
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 11-1: the first fluid flowmeter, 11-2: second liquid flowmeter, 11-3: third liquid
Flowmeter body.
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 one
A kind of method of improvement emulsification synthesis 3,4- methylene-dioxy mandelic acid, follows the steps below:
The mixture of water 10g, 50wt% glyoxalic acid solution 160g is carried out constant temperature stirring, the constant temperature stirring temperature by S1
Degree is -25 DEG C, stirring rate 400rpm；
After starting stirring, the 98wt% concentrated sulfuric acid is added dropwise in S2 in Xiang Suoshu mixture, dripping quantity 7g/min per minute is added dropwise
The 98wt% concentrated sulfuric acid total amount 140g, whipping temp are -25 DEG C, stirring rate 400rpm；
S3, after all 98wt% concentrated sulfuric acids are added dropwise to complete, continue stir 30min, -25 DEG C of whipping temp；
3,4- methylene-dioxy mandelic acid is added into the solution after the completion of S3 by S4, and 3,4- methylenedioxybenzenes is added
The amount 4g of glycolic；
S5 emulsifies the solution after the completion of S4, emulsifying rate 12Kr/min, piperonyl cyclonene is added dropwise simultaneously when emulsification, often
Minute dripping quantity is 5g, emulsification times 5min；
S6, the S5 step are repeated 4 times, every time between be spaced 3min, piperonyl cyclonene total amount 100g is added；
S7 carries out constant temperature stirring to the solution after S6, and 5 DEG C of whipping temp, stirring rate 500rpm, mixing time is
30min after stirring starts 15 minutes starts that toluene or methylene chloride is added dropwise, and dripping quantity per minute is 20g/min, and institute is added dropwise
The gross mass for stating toluene or methylene chloride is 200g.
200ml water is added into the solution after S7 by S8, terminates reaction, obtains product；
It further include the air-blowing process into solution during the S1~S7, air-blowing amount per minute is 2.5L/min, use
Air-blowing medium is nitrogen.
Through detecting purity 88.60%, total recovery 83.06%.
Embodiment two
A kind of method of improvement emulsification synthesis 3,4- methylene-dioxy mandelic acid, follows the steps below:
The mixture of water 10g, 50wt% glyoxalic acid solution 160g is carried out constant temperature stirring, the constant temperature stirring temperature by S1
Degree is -25 DEG C, stirring rate 400rpm；
After starting stirring, the 98wt% concentrated sulfuric acid is added dropwise in S2 in Xiang Suoshu mixture, dripping quantity 7g/min per minute is added dropwise
The 98wt% concentrated sulfuric acid total amount 140g, whipping temp are -25 DEG C, stirring rate 400rpm；
S3, after all 98wt% concentrated sulfuric acids are added dropwise to complete, continue stir 30min, -25 DEG C of whipping temp；
3,4- methylene-dioxy mandelic acid is added into the solution after the completion of S3 by S4, and 3,4- methylenedioxybenzenes is added
The amount 4g of glycolic；
S5 emulsifies the solution after the completion of S4, emulsifying rate 12Kr/min, piperonyl cyclonene is added dropwise simultaneously when emulsification, often
Minute dripping quantity is 5g, emulsification times 5min；
S6, the S5 step are repeated 4 times, every time between be spaced 3min, piperonyl cyclonene total amount 100g is added；
S7 carries out constant temperature stirring to the solution after S6, and 5 DEG C of whipping temp, stirring rate 500rpm, mixing time is
Liquid anti-freeze type polycarboxylate high performance water-reducing agent PCE--AF-L-JG/T223-2017, drop are added dropwise when stirring and starting by 30min
The gross mass for adding the water-reducing agent is 3g；
200ml water is added into the solution after S7 by S8, terminates reaction, obtains product；
It further include the air-blowing process into solution during the S1~S7, air-blowing amount per minute is 2.5L/min, use
Air-blowing medium is nitrogen.
Through detecting purity 91.50%, total recovery 85.78%.
Embodiment three
A kind of method of improvement emulsification synthesis 3,4- methylene-dioxy mandelic acid, follows the steps below:
The mixture of water 10g, 50wt% glyoxalic acid solution 160g is carried out constant temperature stirring, the constant temperature stirring temperature by S1
Degree is -25 DEG C, stirring rate 400rpm；
After starting stirring, the 98wt% concentrated sulfuric acid is added dropwise in S2 in Xiang Suoshu mixture, dripping quantity 7g/min per minute is added dropwise
The 98wt% concentrated sulfuric acid total amount 140g, whipping temp are -25 DEG C, stirring rate 400rpm；
S3, after all 98wt% concentrated sulfuric acids are added dropwise to complete, continue stir 30min, -25 DEG C of whipping temp；
3,4- methylene-dioxy mandelic acid is added into the solution after the completion of S3 by S4, and 3,4- methylenedioxybenzenes is added
The amount 4g of glycolic；
S5 emulsifies the solution after the completion of S4, emulsifying rate 12Kr/min, piperonyl cyclonene is added dropwise simultaneously when emulsification, often
Minute dripping quantity is 5g, emulsification times 5min；
S6, the S5 step are repeated 4 times, every time between be spaced 3min, piperonyl cyclonene total amount 100g is added；
S7 carries out constant temperature stirring to the solution after S6, and 5 DEG C of whipping temp, stirring rate 500rpm, mixing time is
Liquid anti-freeze type polycarboxylate high performance water-reducing agent PCE--AF-L-JG/T223-2017, drop are added dropwise when stirring and starting by 30min
The gross mass for adding the water-reducing agent is 3g, after stirring starts 15 minutes, starts that toluene or methylene chloride is added dropwise, is added dropwise per minute
Amount is 20g/min, and the gross mass that the toluene or methylene chloride is added dropwise is 200g；
200ml water is added into the solution after S7 by S8, terminates reaction, obtains product；
It further include the air-blowing process into solution during the S1~S7, air-blowing amount per minute is 2.5L/min, use
Air-blowing medium is nitrogen.
Through detecting purity 97.60%, total recovery 91.50%.
Example IV
A kind of device of improvement 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, piperonyl cyclonene measuring tank, thermostat, charging
Measuring tank, filter plant, charge pump, air accumulator, filtrate receiver, the sulfuric acid gauge tank outlet and jacket type distributor stirred tank pipe
Road is connected, and sulfuric acid gauge tank outlet is provided with flowmeter, and the thermostat circulation fluid outlet is respectively adopted described in pipeline connection
The jacket inlet of jacket type distributor stirred tank, the jacket inlet of jacket type distributor emulsifying kettle 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
Cover the jacket outlet of outlet, the jacket outlet of jacket type distributor emulsifying kettle and jacket type distributor product stirred tank, the folder
The outlet of shell type distributor stirred tank is connected with the inlet duct of charge pump, the outlet of the piperonyl cyclonene measuring tank and jacket type point
Cloth device emulsifying kettle pipeline is connected, and the outlet of the charging measuring tank is connected with the jacket type distributor product stirred tank pipeline,
The outlet and piperonyl cyclonene measuring tank outlet of charging measuring tank are provided with flowmeter, and the jacket type distributor emulsifying kettle goes out
Mouth is connected with the jacket type distributor product stirred tank inlet duct, the jacket type distributor product stirred tank outlet and institute
The feed inlet pipeline connection of filter plant is stated, the outlet of the air accumulator is respectively adopted the pipeline connection jacket type distributor and stirs
Mix the gas distribution tube entrance of kettle, the gas distribution tube entrance of the jacket type distributor emulsifying kettle and jacket type distributor product
Stirred tank gas distribution tube entrance, the filter plant liquid-phase outlet connect the filtrate receiver entrance.The jacket type distributor
The folder of the jacket inlet pipe of stirred tank, the jacket inlet pipe of jacket type distributor emulsifying kettle and jacket type distributor product stirred tank
Fluid flowmeter is provided on set inlet tube.Gas distribution tube inlet tube, the jacket type of the jacket type distributor stirred tank
It is all provided on the gas distribution tube inlet tube and jacket type distributor product stirred tank gas distribution tube inlet tube of distributor emulsifying kettle
It is equipped with gas flowmeter.It is provided with 2 sets of emulsifier units on the jacket type distributor emulsifying kettle and scrapes wall agitating device.The folder
Temperature instrument is mounted on shell type distributor stirred tank and jacket type distributor emulsifying kettle.
Embodiment five
A kind of device of improvement 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, piperonyl cyclonene measuring tank, thermostat, charging
Measuring tank, double-filtration equipment, charge pump, air accumulator, filtrate receiver, the sulfuric acid gauge tank outlet are stirred with jacket type distributor
Kettle pipeline is connected, and sulfuric acid gauge tank outlet is provided with flowmeter, and pipeline connection is respectively adopted in the thermostat circulation fluid outlet
The jacket inlet of the jacket type distributor stirred tank, the jacket inlet of jacket type distributor emulsifying kettle and jacket type distributor produce
The jacket inlet of product stirred tank, the thermostat circulation fluid entrance are respectively adopted pipeline and connect the jacket type distributor stirred tank
Jacket outlet, the jacket outlet of the jacket outlet of jacket type distributor emulsifying kettle and jacket type distributor product stirred tank, institute
The outlet for stating jacket type distributor stirred tank is connected with the inlet duct of charge pump, the outlet of the piperonyl cyclonene measuring tank and collet
Formula distributor emulsifying kettle pipeline is connected, the outlet and the jacket type distributor product stirred tank pipeline phase of the charging measuring tank
Even, the outlet and piperonyl cyclonene measuring tank outlet for the measuring tank that feeds are provided with flowmeter, the jacket type distributor emulsification
Kettle outlet is connected with the jacket type distributor product stirred tank inlet duct, the jacket type distributor product stirred tank outlet
It is connect with the feed inlet pipeline of the by-pass filtration equipment, the discharge port of the by-pass filtration equipment and the secondary filtration equipment
Feed inlet pipeline connection, the gas that pipeline connects the jacket type distributor stirred tank is respectively adopted in the outlet of the air accumulator
It is distributed the gas distribution tube entrance and jacket type distributor product stirred tank gas of tube inlet, the jacket type distributor emulsifying kettle
It is distributed tube inlet, the secondary filtration equipment liquid-phase outlet connects the filtrate receiver entrance.The jacket type distributor stirred tank
Jacket inlet pipe, the jacket inlet pipe of jacket type distributor emulsifying kettle and the jacket inlet of jacket type distributor product stirred tank
Fluid flowmeter is provided on pipe.Gas distribution tube inlet tube, the jacket type distributor of the jacket type distributor stirred tank
Gas is provided on the gas distribution tube inlet tube and jacket type distributor product stirred tank gas distribution tube inlet tube of emulsifying kettle
Flowmeter body.It is provided with 2 sets of emulsifier units on the jacket type distributor emulsifying kettle and scrapes wall agitating device.The jacket type point
Temperature instrument is mounted on cloth device stirred tank and jacket type distributor emulsifying kettle.
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 improvement 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, piperonyl cyclonene measuring tank are permanent
Warm slot, feed measuring tank, filter plant, charge pump, air accumulator, filtrate receiver, and the sulfuric acid gauge tank outlet is distributed with jacket type
Device stirred tank pipeline is connected, and the thermostat circulation fluid outlet is respectively adopted pipeline and connects the jacket type distributor stirred tank
The jacket inlet of jacket inlet, the jacket inlet of jacket type distributor emulsifying kettle and jacket type distributor product stirred tank, it is described
Thermostat circulation fluid entrance is respectively adopted pipeline and connects the jacket outlet of the jacket type distributor stirred tank, jacket type distributor
The jacket outlet of emulsifying kettle and the jacket outlet of jacket type distributor product stirred tank, the jacket type distributor stirred tank go out
Mouth is connected with the inlet duct of charge pump, and the outlet of the piperonyl cyclonene measuring tank is connected with jacket type distributor emulsifying kettle pipeline,
The outlet of the charging measuring tank is connected with the jacket type distributor product stirred tank pipeline, the jacket type distributor emulsification
Kettle outlet is connected with the jacket type distributor product stirred tank inlet duct, the jacket type distributor product stirred tank outlet
It is connect with the feed inlet pipeline of the filter plant, the outlet of the air accumulator is respectively adopted pipeline and connects the jacket type distribution
The gas distribution tube entrance and jacket type distributor of the gas distribution tube entrance of device stirred tank, the jacket type distributor emulsifying kettle
Product stirred tank gas distribution tube entrance, the filter plant liquid-phase outlet connect the filtrate receiver entrance.
2. a kind of device of improvement emulsification synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, the sulfuric acid gauge tank, piperonyl cyclonene measuring tank and charging measuring tank outlet are provided with flowmeter.
3. a kind of device of improvement emulsification synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, the jacket inlet pipe and collet of the jacket inlet pipe of the jacket type distributor stirred tank, jacket type distributor emulsifying kettle
Fluid flowmeter is provided on the jacket inlet pipe of formula distributor product stirred tank.
4. a kind of device of improvement 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
Gas flowmeter is provided on inlet tube and jacket type distributor product stirred tank gas distribution tube inlet tube.
5. a kind of device of improvement 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.
6. a kind of device of improvement 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.
7. a kind of device of improvement emulsification synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, the filter plant can be multiple stage filter units.
8. a kind of device of improvement emulsification synthesis 3,4- methylene-dioxy mandelic acid according to claim 1, feature
It is, the filter plant can be 2 grades of filter plants.
9. a kind of device of improvement 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.
10. a kind of device of improvement 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.
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| CN201821391966.2U CN208776620U (en) | 2018-08-28 | 2018-08-28 | A kind of device improving emulsification synthesis 3,4- methylene-dioxy mandelic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821391966.2U CN208776620U (en) | 2018-08-28 | 2018-08-28 | A kind of device improving emulsification synthesis 3,4- methylene-dioxy mandelic acid |
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| CN201821391966.2U Active CN208776620U (en) | 2018-08-28 | 2018-08-28 | A kind of device improving emulsification synthesis 3,4- methylene-dioxy mandelic acid |
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| CN (1) | CN208776620U (en) |
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2018
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Effective date of registration: 20200819 Address after: Room 2307, block B, polymer materials Industrial Innovation Park, No.51 Lutai Avenue, hi tech Zone, Zibo City, Shandong Province Patentee after: Shandong Tianda Taize Environmental Protection Technology Co., Ltd Address before: 255086 Polymer Material Industry Innovation Park B403, No. 51 Lutai Avenue, Zibo High-tech Zone, Shandong Province Patentee before: ZIBO TAIDIAN NEW MATERIAL Co.,Ltd. |