CN208632422U - It is a kind of to emulsify the device for catalyzing and synthesizing 3,4- methylene-dioxy mandelic acid - Google Patents
It is a kind of to emulsify the device for catalyzing and synthesizing 3,4- methylene-dioxy mandelic acid Download PDFInfo
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Abstract
The utility model discloses the devices that a kind of emulsification catalyzes and synthesizes 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, filter plant, charge pump, air accumulator, filtrate receiver may be implemented to carry out synthesis 3, the method for 4- methylene-dioxy mandelic acid using emulsification catalytic process.Using can make to generate a large amount of bubbles in reaction system when the present apparatus, so that reaction-ure surface product be made to increase, increases the contact area between reactant, the conversion ratio and yield of reaction can be improved.
Description
Technical field
The utility model belongs to technical field of chemical engineering, and in particular to a kind of emulsification catalyzes and synthesizes 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 emulsify and catalyze and synthesize 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:
It is a kind of to emulsify the method for catalyzing and synthesizing 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 and benzyl triethyl ammonium chlorination are added into the solution after the completion of step 3
Ammonium, the ratio that water quality described in the amount and step 1 of 3,4- methylene-dioxy mandelic acid is added is 3,4- methylenedioxybenzenes second
Alkyd: water=0.1~1:1, the ratio that water quality described in the amount and step 1 of benzyltriethylammoinium chloride is added is benzyl triethyl ammonium
Ammonium chloride: water=0.5~1.5:1;
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, 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;
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 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, water quality described in the amount and step 1 of benzyltriethylammoinium chloride is added in the step 4
Ratio be benzyltriethylammoinium chloride: water=0.8~1.2:1.
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, 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 and benzyl triethyl ammonium chlorination are added into the solution after the completion of step 3
Ammonium, the mass ratio that water described in the amount and step 1 of 3,4- methylene-dioxy mandelic acid is added is 3,4- methylenedioxybenzenes second
Alkyd: water=0.3~0.4:1, the mass ratio that water described in the amount and step 1 of benzyltriethylammoinium chloride is added is three second of benzyl
Ammonium chloride: water=0.8~1:1;
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, 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;
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 7, air-blowing amount per minute is the mixing
12~20 times of object product.
In above-mentioned technical proposal, the air-blowing medium that the air-blowing process uses is nitrogen.
It is a kind of to emulsify the device for catalyzing and synthesizing 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, filtering
Equipment, charge pump, air accumulator, filtrate receiver, the sulfuric acid gauge tank outlet is connected with jacket type distributor stirred tank pipeline, described
The outlet of thermostat circulation fluid is respectively adopted pipeline and connects the jacket inlet of the jacket type distributor stirred tank, jacket type distributor
The jacket inlet of emulsifying kettle and the jacket inlet of jacket type distributor product stirred tank, the thermostat circulation fluid entrance are adopted respectively
The jacket outlet of the jacket type distributor stirred tank, the jacket outlet and collet of jacket type distributor emulsifying kettle are connected with pipeline
The jacket outlet of formula distributor product stirred tank, 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 connected with the jacket type distributor product stirred tank inlet duct, the jacket type distributor product stirred tank export and
The feed inlet pipeline of the filter plant 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 and jacket type distributor produce
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 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 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, 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 emulsification catalytic 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, for the utility model during the reaction with the method for addition phase transfer catalyst, raising water phase is affine with oily phase
Property, the effect of emulsification is further increased, thus the selectivity and yield of the reaction improved.
Detailed description of the invention
Fig. 1 is a kind of flow diagram for emulsifying and catalyzing and synthesizing 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;12: jacket type distributor product stirred 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 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
It is a kind of to emulsify the method for catalyzing and synthesizing 3,4- methylene-dioxy mandelic acid, it 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 9.3g 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, step 5 step is repeated 4 times, every time between be spaced 3min, piperonyl cyclonene total amount 100g is added;
Step 7, constant temperature stirring is carried out to the solution after step 6,5 DEG C of whipping temp, stirring rate 500rpm, stirred
Time is 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 97.60%, total recovery 91.50%.
Embodiment 2
It is a kind of to emulsify the method for catalyzing and synthesizing 3,4- methylene-dioxy mandelic acid, it 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 and benzyl triethyl ammonium chlorination are added into the solution after the completion of step 3
Ammonium is added the amount 9g of 3,4- methylene-dioxy mandelic acid, the amount 13g of benzyltriethylammoinium chloride is added;
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, constant temperature stirring is carried out to the solution after step 6,5 DEG C of whipping temp, stirring rate 600rpm, stirred
Time is 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 97.53%, total recovery 91.43%.
Embodiment 3
It is a kind of to emulsify the device for catalyzing and synthesizing 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, filtering
Equipment, charge pump, air accumulator, filtrate receiver, the sulfuric acid gauge tank outlet are connected with jacket type distributor stirred tank pipeline, sulfuric acid
Measuring tank outlet is provided with flowmeter, and the thermostat circulation fluid outlet is respectively adopted pipeline and connects the jacket type distributor
The collet of the jacket inlet of stirred tank, the jacket inlet of jacket type distributor emulsifying kettle and jacket type distributor product stirred tank enters
Mouthful, the thermostat circulation fluid entrance is respectively adopted pipeline and connects the jacket outlet of the jacket type distributor stirred tank, collet
The jacket outlet of formula distributor emulsifying kettle and the jacket outlet of jacket type distributor product stirred tank, the jacket type distributor stir
The outlet for mixing kettle is connected with the inlet duct of charge pump, the outlet of the piperonyl cyclonene measuring tank and jacket type distributor emulsifying kettle pipe
Road is connected, and piperonyl cyclonene measuring tank outlet is provided with flowmeter, the jacket type distributor emulsifying kettle outlet and the jacket type
Distributor product stirred tank inlet duct is connected, jacket type distributor product stirred tank outlet and the filter plant into
The gas distribution that pipeline connects the jacket type distributor stirred tank is respectively adopted in the connection of material mouth pipeline, the outlet of the air accumulator
Tube inlet, the gas distribution tube entrance of the jacket type distributor emulsifying kettle and the distribution of jacket type distributor product stirred tank gas
Tube inlet, the filter plant liquid-phase outlet connect the filtrate receiver entrance.The collet of the jacket type distributor stirred tank enters
It is all provided on the jacket inlet pipe of mouth pipe, the jacket inlet pipe of jacket type distributor emulsifying kettle and jacket type distributor product stirred tank
It is equipped with fluid flowmeter.The gas distribution tube inlet tube of the jacket type distributor stirred tank, jacket type distributor emulsifying kettle
Gas flowmeter is provided on gas distribution tube inlet tube and jacket type distributor product stirred tank gas distribution tube inlet tube.
It is provided with 2 sets of emulsifier units on the jacket type distributor emulsifying kettle and scrapes wall agitating device.The jacket type distributor stirring
Temperature instrument is mounted on kettle and jacket type distributor emulsifying kettle.
Embodiment 4
It is a kind of to emulsify the device for catalyzing and synthesizing 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, two-stage
Filter plant, charge pump, air accumulator, filtrate receiver, the sulfuric acid gauge tank outlet are connected with jacket type distributor stirred tank pipeline,
Sulfuric acid gauge tank outlet is provided with flowmeter, and the thermostat circulation fluid outlet is respectively adopted pipeline and connects the jacket type point
The folder of the jacket inlet of cloth device stirred tank, the jacket inlet of jacket type distributor emulsifying kettle and jacket type distributor product stirred tank
Cover entrance, the thermostat circulation fluid entrance be respectively adopted pipeline connect the jacket type distributor stirred tank jacket outlet,
The jacket outlet of jacket type distributor emulsifying kettle and the jacket outlet of jacket type distributor product stirred tank, the jacket type distribution
The outlet of device stirred tank is connected with the inlet duct of charge pump, and the outlet of the piperonyl cyclonene measuring tank and jacket type distributor emulsify
Kettle pipeline is connected, and piperonyl cyclonene measuring tank outlet is provided with flowmeter, the jacket type distributor emulsifying kettle outlet and the folder
Shell type distributor product stirred tank inlet duct is connected, the jacket type distributor product stirred tank outlet and the by-pass filtration
The feed inlet pipeline of equipment connects, and the feed inlet pipeline of the discharge port of the by-pass filtration equipment and the secondary filtration equipment connects
It connects, the outlet of the air accumulator is respectively adopted pipeline and connects the gas distribution tube entrance of the jacket type distributor stirred tank, institute
State the gas distribution tube entrance and jacket type distributor product stirred tank gas distribution tube entrance of jacket type distributor emulsifying kettle, institute
It states secondary filtration equipment liquid-phase outlet and connects the filtrate receiver entrance.The jacket inlet pipe of the jacket type distributor stirred tank,
It is provided on the jacket inlet pipe of jacket type distributor emulsifying kettle and the jacket inlet pipe of jacket type distributor product stirred tank
Fluid flowmeter.The gas of the gas distribution tube inlet tube of the jacket type distributor stirred tank, jacket type distributor emulsifying kettle
Gas flowmeter is provided on distributor pipe inlet tube and jacket type distributor product stirred tank gas distribution tube inlet tube.It is described
It is provided with 2 sets of emulsifier units on jacket type distributor emulsifying kettle and scrapes wall agitating device.The jacket type distributor stirred tank and
Temperature instrument is mounted on 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 emulsify the device for catalyzing and synthesizing 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, filter plant, charge pump, air accumulator, filtrate receiver, the sulfuric acid gauge tank outlet and jacket type distributor stirred tank pipeline
It is connected, the thermostat circulation fluid outlet is respectively adopted pipeline and connects the jacket inlet of the jacket type distributor stirred tank, folder
The jacket inlet of shell type distributor emulsifying kettle and the jacket inlet of jacket type distributor product stirred tank, the thermostat circulation fluid
The collet that pipeline connects the jacket outlet of the jacket type distributor stirred tank, jacket type distributor emulsifying kettle is respectively adopted in entrance
The jacket outlet of outlet and jacket type distributor product stirred tank, the outlet of the jacket type distributor stirred tank and charge pump
Inlet duct is connected, and the outlet of the piperonyl cyclonene measuring tank is connected with jacket type distributor emulsifying kettle pipeline, the jacket type point
The outlet of cloth device emulsifying kettle is connected with the jacket type distributor product stirred tank inlet duct, and the jacket type distributor product stirs
It mixes kettle outlet to connect with the feed inlet pipeline of the filter plant, the outlet of the air accumulator is respectively adopted pipeline and connects the folder
The gas distribution tube entrance and collet of the gas distribution tube entrance of shell type distributor stirred tank, the jacket type distributor emulsifying kettle
Formula distributor product stirred tank gas distribution tube entrance, the filter plant liquid-phase outlet connect the filtrate receiver entrance.
2. a kind of emulsification according to claim 1 catalyzes and synthesizes the device of 3,4- methylene-dioxy mandelic acid, feature
It is, the sulfuric acid gauge tank and piperonyl cyclonene measuring tank outlet are provided with flowmeter.
3. a kind of emulsification according to claim 1 catalyzes and synthesizes the device of 3,4- methylene-dioxy mandelic acid, 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.
4. a kind of emulsification according to claim 1 catalyzes and synthesizes the device of 3,4- methylene-dioxy mandelic acid, 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.
5. a kind of emulsification according to claim 1 catalyzes and synthesizes the device of 3,4- methylene-dioxy mandelic acid, 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.
6. a kind of emulsification according to claim 1 catalyzes and synthesizes the device of 3,4- methylene-dioxy mandelic acid, feature
It is, emulsifier unit is provided on the jacket type distributor emulsifying kettle and scrapes wall agitating device.
7. a kind of emulsification according to claim 1 catalyzes and synthesizes the device of 3,4- methylene-dioxy mandelic acid, feature
It is, 2 sets of emulsifier units are provided on every jacket type distributor emulsifying kettle and scrapes wall agitating device.
8. a kind of emulsification according to claim 1 catalyzes and synthesizes the device of 3,4- methylene-dioxy mandelic acid, feature
It is, the filter plant is multiple stage filter units.
9. a kind of emulsification according to claim 1 catalyzes and synthesizes the device of 3,4- methylene-dioxy mandelic acid, feature
It is, the filter plant is 2 grades of filter plants.
10. a kind of emulsification according to claim 1 catalyzes and synthesizes the device of 3,4- methylene-dioxy mandelic acid, 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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