CN206902053U - Device for producing 2, 3, 5, 6-4-methoxymethyl-tetrafluorobenzyl alcohol - Google Patents
Device for producing 2, 3, 5, 6-4-methoxymethyl-tetrafluorobenzyl alcohol Download PDFInfo
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- CN206902053U CN206902053U CN201720736838.6U CN201720736838U CN206902053U CN 206902053 U CN206902053 U CN 206902053U CN 201720736838 U CN201720736838 U CN 201720736838U CN 206902053 U CN206902053 U CN 206902053U
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 55
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 190
- 238000006243 chemical reaction Methods 0.000 claims abstract description 152
- 238000005406 washing Methods 0.000 claims abstract description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 claims abstract description 28
- 239000003513 alkali Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000011084 recovery Methods 0.000 claims abstract description 8
- 230000008676 import Effects 0.000 claims description 45
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 29
- 238000007599 discharging Methods 0.000 claims description 29
- 238000004064 recycling Methods 0.000 claims description 23
- 238000007600 charging Methods 0.000 claims description 21
- 239000002351 wastewater Substances 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 14
- 238000001704 evaporation Methods 0.000 claims description 7
- 230000008020 evaporation Effects 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 4
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 206010062575 Muscle contracture Diseases 0.000 claims description 2
- 208000006111 contracture Diseases 0.000 claims description 2
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 abstract description 30
- 238000000034 method Methods 0.000 abstract description 13
- 239000000047 product Substances 0.000 abstract description 11
- 235000019445 benzyl alcohol Nutrition 0.000 abstract description 10
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 230000006872 improvement Effects 0.000 abstract description 5
- 238000010924 continuous production Methods 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 5
- 239000007864 aqueous solution Substances 0.000 abstract 3
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N dimethyl sulfate Chemical compound COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 abstract 3
- 238000002360 preparation method Methods 0.000 abstract 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 16
- 229960004217 benzyl alcohol Drugs 0.000 description 9
- 230000008569 process Effects 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 238000009834 vaporization Methods 0.000 description 7
- 230000008016 vaporization Effects 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 238000012546 transfer Methods 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000004702 methyl esters Chemical class 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000002175 menstrual effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model relates to a device of production 2, 3, 5, 6-4-methoxymethyl-tetrafluorobenzyl alcohol, including toluene raw materials basin, dimethyl sulfate raw materials basin, dihydric alkali aqueous solution basin, first heat exchanger, blender, microchannel reactor, first order layering jar group, second level layering jar group, washing blender, washing back reaction solution receiving tank, second heat exchanger, take off the dissolver in succession, toluene recovery jar and finished product jar, include in the preparation process: preparing a water solution of the dihydroxyl alkali for later use; heating the aqueous solution of the double-alcohol alkali, mixing dimethyl sulfate and toluene, heating, simultaneously feeding the aqueous solution of the double-alcohol alkali and the toluene solution of the dimethyl sulfate into a reactor for mixing reaction, carrying out layering and washing treatment on the reaction solution, and distilling the washed reaction solution to recover toluene to obtain crude benzyl alcohol. The method has the advantages of continuous production, higher reaction rate than the traditional method, shorter reaction time, high production efficiency, reduction of the generation of by-product diether, improvement of production yield and reduction of production consumption.
Description
Technical field
A kind of production 2 is the utility model is related to, the device of 3,5,6-4- methoxyl methyls-tetrafluorobenzyl alcohol, specifically, is related to
One kind can efficiently and safely continuous production 2, the device of 3,5,6-4- methoxyl methyls-tetrafluorobenzyl alcohol.
Background technology
2,3,5,6-4- methoxyl methyls-tetrafluorobenzyl alcohol（Herein referred to as：Benzylalcohol）Production process in, main reaction is 2,
3,5,6- tetrafluoro terephthalyl alcohols（Referred to as double alcohol herein）Methylated with sodium methoxide, another method is by double alcohol and sulfuric acid two
Methyl esters methylates, but with these methods in traditional autoclave building-up process, because the heat and mass effect of reactor is poor, easily
There is superfluous product to produce, that is, a part easily continues reaction generation bis ether by-product with the dimethyl suflfate of surplus in the principal product generated
Thing.Key reaction equation is as follows：
Therefore, traditional reactor has that hybrid reaction is uneven, energy consumption consumption is high, equipment volume is big, and installation, cleaning are difficult
The shortcomings of.
The process of production benzylalcohol typically all uses autoclave Batch Process at present, and time-consuming for this method production, production effect
Rate is low, and accessory substance bis ether content is higher in production process, general bis ether content 10~20%, crude product benzylalcohol content 80~90%, sternly
Ghost image rings the content yield of principal product benzylalcohol, and cost of material consumption is larger.Separately because reactor material stock volume is larger, have in production
Larger safety in production hidden danger is present.
The content of the invention
In order to solve the problems, such as that the above method prepares that benzylalcohol crude product purity is low, accessory substance is high, the utility model provides a kind of
Production 2,3, the device of 5,6-4- methoxyl methyls-tetrafluorobenzyl alcohol.In this process units, micro passage reaction can make double alcohol exist
In micro passage reaction with the quick hybrid reaction of dimethyl suflfate, the timely outflow reactor of product of reaction, avoid principal product with
Dimethyl suflfate continues reaction generation accessory substance bis ether.
Technical scheme is used by the utility model solves its technical problem：
One kind production 2, the device of 3,5,6-4- methoxyl methyls-tetrafluorobenzyl alcohol, including methylbenzene raw material basin V01, sulfuric acid two
Methyl ester feedstocks basin V02, double alcohol aqueous alkali basin V03, First Heat Exchanger E01, blender MR01, micro passage reaction
The first receiving tank of reaction solution V11 after MR02, the first stage layered tank group, substratification tank group, washing blender MR03, washing,
The second receiving tank of reaction solution V12, the second heat exchanger E02, continuous desolventizing device D01, the 3rd heat exchanger E03, toluene first after washing
Recycling can V14, the second recycling can of toluene V15, finished pot V13 and measuring pump；Described measuring pump include toluene feed pump P01,
Dimethyl suflfate feed pump P02, double alcohol buck feed pump P03, washing water feed pump P04, handle well reaction solution feed pump P05,
Reclaim toluene discharging pump P06；The first stage layered tank group includes two first receptions layering tank V04, V05 being used alternatingly,
The reaction flow containers of first waste water tank V06 and first V07；The substratification tank group includes two second receptions point being used alternatingly
Layer tank V08, V09, the second waste water tank V10, the receiving tank of reaction solution second after reaction solution the first receiving tank V11 and washing after washing
V12；The outlet of the methylbenzene raw material basin V01 is connected with toluene feed pump P01 imports, and toluene feed pump P01 is exported with mixing
Device MR01 import connection；Described dimethyl suflfate material storaging tank V02 outlet connects with dimethyl suflfate feed pump P02 imports
Connect, dimethyl suflfate feed pump P02 outlets are connected with blender MR01 import；In double alcohol aqueous alkali basin V03
Outlet is connected with double alcohol buck feed pump P03 imports, and double alcohol buck feed pump P03 outlets are connected with First Heat Exchanger E01 imports；
The outlet of the blender MR01 and First Heat Exchanger E01 outlet are all connected to micro passage reaction MR02 entrance；Should
The import that micro passage reaction MR02 outlet receives layering tank V04, V05 with two first of the first stage layered tank group simultaneously connects
Connect；Two first of first stage layered tank group receive the outlet for being layered tank V04, V05 while first with the first stage layered tank group
The reaction flow containers of waste water tank V06 and first V07 import connection；The outlet of the first reaction flow container V07 and the washing blender
MR03 import connection；Water inlet, water inlet and washing water feed pump P04 phases are additionally provided with the washing blender MR03
Even；The outlet of the washing blender MR03 receives layering tank V08, V09 with two second of substratification tank group simultaneously
Import connects；Two second of the substratification tank group outlets for receiving layering tank V08, V09 simultaneously with the second waste water tank V10 and
The first receiving tank of reaction solution V11 import connection after washing, reaction solution the after reaction solution the first receiving tank V11 and washing after washing
Two receiving tank V12 are connected；The second receiving tank of reaction solution V12 outlet is passed through with handling reaction solution feed pump P05 well after the washing
Import is connected, and reaction solution feed pump P05 outlets are connected with the second heat exchanger E02 charging apertures, the second heat exchanger E02 discharging openings and company
Continuous desolventizing device D01 import connection；The gas outlet on continuous desolventizing device D01 tops is connected with the 3rd heat exchanger E03 imports, and the 3rd
Heat exchanger E03 outlets are connected with toluene the first recycling can V14 and toluene the second recycling can V14 imports, the first recycling can of toluene V14
It is connected with the second recycling can of toluene V14 discharging opening with recovery toluene discharging pump P06, the discharging opening of continuous desolventizing device D01 bottoms
It is connected with finished pot V13.
To above-mentioned production 2, in the improvement project of the device of 3,5,6-4- methoxyl methyls-tetrafluorobenzyl alcohol, described is micro- anti-
Answer channel reactor MR02 connected by two charging apertures, a hybrid reaction passage, a straight-through reaction channel with discharging opening and
Into；The hybrid reaction passage has the reaction structure that inwall is in multistage arc.
To above-mentioned production 2, in the improvement project of the device of 3,5,6-4- methoxyl methyls-tetrafluorobenzyl alcohol, the washing is mixed
Clutch MR03 is the combination of conical funnel shape microchannel.
It is described continuous de- in the improvement project of the device of 3,5,6-4- methoxyl methyls-tetrafluorobenzyl alcohol to above-mentioned production 2
Molten device D01 is the stainless steel negative-pressure cup of sealing, is internally provided with flat board of at least four pieces of bands to descending slope, in upper and lower point of tank body
There are not the outlet of solvent and the outlet of product.
To above-mentioned production 2, in the improvement project of the device of 3,5,6-4- methoxyl methyls-tetrafluorobenzyl alcohol, described is micro- logical
Reactor specification preferred passage inside dimension in road is 1~8mm.
The utility model produces the technical process of benzylalcohol using above-mentioned device：First stock up, prepare double alcohol aqueous alkalis, it is standby
With；Make double alcohol aqueous alkali heatings, dimethyl suflfate mixes heating, double alcohol aqueous alkalis and dimethyl suflfate toluene liquid with toluene
Enter reactor hybrid reaction simultaneously, reaction solution is layered, washing process, and the reaction solution after washing obtains through being distilled to recover toluene
Thick benzylalcohol, benzylalcohol content 94~96%, accessory substance bis ether 3~5%, yield 94~96%.
The beneficial effects of the utility model：Pass through the reaction of effective connection of device, wherein the use enhancing of microreactor
Mass transfer and heat transfer course of reaction, two layering tank group uses, reacted waste water energy is discharged in time by waste water tank, instead
Liquid is answered to obtain reaction product into the continuous recycling design of continuous desolventizing device；So achieve that continuous production, reaction rate ratio
Traditional height, the reaction time is shorter, improves production efficiency；Its efficient mass transfer, heat-transfer character, reduce accessory substance bis ether
Generation, improves product yield, reduces production consuming cost；Reaction unit small volume, easy to operate, production security is high.
Brief description of the drawings：
The utility model is further illustrated with implementation example below in conjunction with the accompanying drawings
Fig. 1 is the utility model process units schematic diagram；
The double alcohol alkali water tanks of V01 toluene basin, V02 dimethyl suflfates basin, V03, V04 first receive layering tank, V05 first
Receive layering tank, the waste water tanks of V06 first, V07 first react flow container, V08 second receive layering tank, V09 second receive layering tank,
The waste water tanks of V10 second, V11 washing after the receiving tank of reaction solution first, V12 washing after the receiving tank of reaction solution second, V13 finished pots,
The double alcohol of the recycling can of V14 toluene first, the recycling can of V15 toluene second, P01 toluene feeds pump, P02 dimethyl suflfates feed pump, P03
Buck feed pump, P04 washing waters feed pump, P05 handle reaction solution feed pump, P06 recovery toluene discharging pump, MR01 mixing well
Device, MR02 micro passage reactions, MR03 washing blender, E01 First Heat Exchangers, the heat exchangers of E02 second, the heat exchangers of E03 the 3rd,
The counterbalance valves of BPV01 first, the counterbalance valves of BPV02 second, D01 continuous desolventizings device, 101 times conduction oils, 102 water sides, 103 water inlets
End, 104 heat conductive oil inlets, 105 wastewater outlets.
Fig. 2 is the utility model micro passage reaction internal microstructure figure；
1 first reactor charging aperture, 2 second reactor charging apertures, 3 hybrid reaction passages, 4 sealed grooves, 5 screw holes, 6
Discharging opening, 7 straight-through reaction channels
Fig. 3 is Fig. 2 A-A to sectional view；
8 passage arcwall face structures
Fig. 4 is the top view of washing blender of the present utility model；
9 first blender charging apertures, 10 second blender charging apertures
Fig. 5 is Fig. 4 B-B direction sectional view；
11 blender discharging openings
Fig. 6 is the top view of continuous desolventizing device of the present utility model；
Fig. 7 is Fig. 6 C-C to sectional view.
12 rise vaporization mouth, 13 desolventizing device charging apertures, 14 evaporation plates, 15 desolventizing device discharging openings, 16 heat-transferring jackets
Embodiment：
The following unrestricted implementation examples of the utility model can be more fully understood using one of ordinary skill in the art
The utility model, but the utility model is not limited in any way.
Test method described in following examples, it is conventional method unless otherwise specified；The raw material and material, such as nothing
Specified otherwise, commercially obtain.
One kind production 2, the device of 3,5,6-4- methoxyl methyls-tetrafluorobenzyl alcohol, as shown in figure 1, including methylbenzene raw material basin
V01, dimethyl suflfate material storaging tank V02, double alcohol aqueous alkali basin V03, First Heat Exchanger E01, blender MR01, microchannel
Reaction solution first receives after reactor MR02, the first stage layered tank group, substratification tank group, washing blender MR03, washing
The second receiving tank of reaction solution V12, the second heat exchanger E02, continuous desolventizing device D01, the 3rd heat exchanger E03, first after tank V11, washing
The first recycling can of benzene V14, the second recycling can of toluene V15, finished pot V13 and measuring pump；Described measuring pump includes toluene feed
Pump P01, dimethyl suflfate feed pump P02, double alcohol buck feed pump P03, washing water feed pump P04, handle well reaction solution charging
Pump P05, recovery toluene discharging pump P06；The first stage layered tank group includes two first reception layering tanks being used alternatingly
V04, V05, the reaction flow containers of the first waste water tank V06 and first V07；The substratification tank group include being used alternatingly two the
Two receive layering tank V08, V09, the second waste water tank V10, reaction solution second after reaction solution the first receiving tank V11 and washing after washing
Receiving tank V12；The outlet of the methylbenzene raw material basin V01 is connected with toluene feed pump P01 imports, toluene feed pump P01 outlets
Import with blender MR01 is connected；Described dimethyl suflfate material storaging tank V02 outlet and dimethyl suflfate feed pump P02
Import is connected, and dimethyl suflfate feed pump P02 outlets are connected with blender MR01 import；Double alcohol aqueous alkali basins
Outlet in V03 is connected with double alcohol buck feed pump P03 imports, and double alcohol buck feed pump P03 outlets are entered with First Heat Exchanger E01
Mouth connection；The outlet of the blender MR01 and First Heat Exchanger E01 outlet are all connected to micro passage reaction MR02's
Entrance；Micro passage reaction MR02 outlet receives layering tank V04, V05 with two first of the first stage layered tank group simultaneously
Import connection；Two first of the first stage layered tank group outlets for receiving layering tank V04, V05 simultaneously with the first stage layered tank
The reaction flow containers of first waste water tank V06 of group and first V07 import connection；The outlet of the first reaction flow container V07 and the water
Wash blender MR03 import connection；Water inlet is additionally provided with the washing blender MR03, water inlet is fed with washing water
Pump P04 is connected；The outlet of the washing blender MR03 receives layering tank with two second of substratification tank group simultaneously
V08, V09 import connection；The outlet that two second of substratification tank group receive layering tank V08, V09 is simultaneously useless with second
Water pot V10 and the first receiving tank of reaction solution V11 after washing import connect, reaction solution the first receiving tank V11 and washing after washing
The second receiving tank of reaction solution V12 is connected afterwards；The second receiving tank of reaction solution V12 outlet is passed through with handling reaction solution well after the washing
Feed pump P05 imports are connected, and reaction solution feed pump P05 outlets are connected with the second heat exchanger E02 charging apertures, the second heat exchanger E02
Discharging opening is connected with continuous desolventizing device D01 import；The gas outlet on continuous desolventizing device D01 tops is entered with the 3rd heat exchanger E03
Mouthful connection, the 3rd heat exchanger E03 outlets are connected with toluene the first recycling can V14 and toluene the second recycling can V14 imports, toluene the
One recycling can V14 and the second recycling can of toluene V14 discharging opening are connected with recovery toluene discharging pump P06, under continuous desolventizing device D01
The discharging opening in portion is connected with finished pot V13.In connection, above-mentioned each tank, container or device are respectively by pipeline with being connected
Equipment connection.At work, the raw material in described methylbenzene raw material basin V01, dimethyl suflfate basin V02 enters the present apparatus
Into blender MR01, after making both raw material mixed heat transfers, with coming out from double alcohol aqueous alkali basin V03 and being changed through first
In micro passage reaction MR02 hybrid reactions, reaction solution first connects double alcohol aqueous alkalis of hot device E01 heat exchange into one of them
Contracture layer tank V04, another the first reception layering tank V05 are then closed, at this moment in that first reception layering tank V05 of closing
Reaction solution after layering, first open the first waste water tank V06, allow the waste water of bottom to enter in the first waste water tank V06, Ran Houzai
Close the first waste water tank V06 and open the first reaction flow container V07, the reaction solution on upper strata is flowed into the first reaction flow container V07；Connect down
Come, the reaction solution in the first reaction flow container V07 enters washing blender MR03, makes reaction solution and is added to washing blender MR03
In water mixing, through the mixed mixed liquor of water enter back into substratification tank group carry out layered shaping, this is with the first stage layered
Processing is the same, and the first receiving tank of reaction solution V11 is collected after reaction solution enters washing, and reaction solution second connects after entering washing after collection
Closed cans V12, the second receiving tank of reaction solution V12 enters through desolventizing device charging aperture 13 again after coming out through the second heat exchanger E02 after washing
Enter continuous desolventizing device D01, continuous desolventizing device chuck is passed through conduction oil, preheats evaporation plate 14, reaction solution is through the evaporation plate in molten device
14 heating, the toluene after vaporization is set to enter after flowing through the 3rd heat exchanger E03 condensations from continuous desolventizing device D01 rising vaporization mouth 12
Into toluene the first recycling can V14 and the first recycling can of toluene V15, while by toluene recovery, product component is in Action of Gravity Field
Under enter from desolventizing device discharging opening 15 in finished pot V13, thick benzylalcohol is made.
In the present embodiment, as shown in Figure 2,3, described micro- reaction channel reactor MR02 is by first reactor charging aperture
1st, 3, one, the hybrid reaction passage of second reactor charging aperture 2, one straight-through reaction channel 7 and discharging opening 6 are formed by connecting；It is described
Hybrid reaction passage 3 have inwall be in multistage arc reaction structure, when fluid is entered in feeding-passage, constantly warp up and down and
The flowing collision of vias inner walls arc, enter in straight-through reaction channel after upper and lower both sides collisional mixing, so through multiple impacts,
Can reaction is abundant after mixing；In use, circulation is anti-from the first reactor charging aperture 1, second of micro- reaction channel device respectively
Device charging aperture 2 is answered to feed, two plumes stimulate the menstrual flow the hybrid reaction of hybrid reaction passage 3, then through straight-through reaction channel 7 to continue mixing anti-
Should, reaction is completed to come out from discharging opening 6；The preferred passage inside dimension of described micro passage reaction specification is 1~8mm.
As shown in Figure 4,5, the washing blender MR03 is the combination of conical funnel shape microchannel, and reaction material liquid is being revolved with water
Rotating disk is fed to tangential direction, bumpy flow is formed, from bottom discharge, in use, reaction solution and water enter from the first blender respectively
Material mouth 9, the second blender charging aperture 10 are entered in washing blender MR03, and reaction solution discharges from blender after blended washing
Mouth 11 flows out.
As shown in Figure 6,7, the continuous desolventizing device D01 is the stainless steel negative-pressure cup of sealing, is internally provided with least four pieces
Band vaporizes the desolventizing device discharging opening of mouth 12 and product to the evaporation plate 14 of descending slope in the upper and lower rising for having solvent respectively of tank body
15.In use, first preheating conduction oil enters continuous desolventizing device D01, preheat heat-transferring jacket 16 and evaporation plate 14 arrives temperature in use, instead
Answer liquid to enter from desolventizing device charging aperture 13, flow into evaporation plate 14 and evaporate, the solvent of vaporization changes from vaporization mouth 12 is risen into the 3rd
Hot device E03, product do not vaporize, and are flowed out from desolventizing device discharging opening 15.
Embodiment 1
It is in molar ratio double alcohol as shown in figure 1, preparing double alcohol aqueous alkalis：Piece alkali：Reaction water=1:1.5:8 dispensings, match somebody with somebody
Make be placed on it is standby in its couple of alcohol aqueous alkali basin V03；Toluene, dimethyl suflfate be added separately to methylbenzene raw material basin V01,
In dimethyl suflfate material storaging tank V02, the mol ratio of material is double alcohol：Dimethyl suflfate：Toluene=1:1.5:3；Toluene pump
P01 and dimethyl suflfate pump P02 sets 60 degree with 1.31 liters/min of flow velocity, 0.86 liter/min of charging, heat exchange respectively, into mixing
After clutch MR01, converge with double alcohol aqueous alkalis after First Heat Exchanger E01 heat exchange in micro passage reaction MR02 imports, its
Middle double 1.78 liters/min of the alcohol buck pump P03 flows of control, heat exchange set 60 degree, the BPV01 system back pressure 0.4Mpa of counterbalance valve I, led to
Cross and after sufficient hybrid reaction, obtain reaction solution in micro passage reaction MR02；Reaction solution is respectively in the first stage layered tank group
Two first receive collection layering in layering tank V04, V05, obtain reaction solution and react liquid temperature into the first reaction flow container V07, control
For degree at 50 degree, reaction solution enters washing blender MR03, the second counterbalance valve BPV02 system back pressures from the first reaction flow container V07
0.4Mpa, washing is mixed with a certain amount of water of addition, and water inlet is washed with water water feed pump P04, come out from washed reaction device MR03
Reaction solution be again introduced into two second of substratification tank group and receive layering tank V08, V09, be subdivided layer processing, handle well
Reaction solution enter washing after reaction solution the first receiving tank V11 and washing after the second receiving tank of reaction solution V12.Reaction solution is from turning one's coat
Wash rear the second receiving tank of reaction solution V12 out to convey into the second heat exchanger E02 preheatings through discharging pump P05, enter after preheating continuous
Desolventizing device D01, toluene is reclaimed by vaporization process, and obtain thick benzylalcohol, thick benzylalcohol content 95.3%, accessory substance bis ether 3%, received
Rate 95.5%.
Embodiment 2
It is in molar ratio double alcohol as shown in figure 1, preparing double alcohol aqueous alkalis：Piece alkali：Reaction water=1:1.8:5 dispensings, match somebody with somebody
Make be placed on it is standby in its couple of alcohol aqueous alkali basin V03；Toluene, dimethyl suflfate be added separately to methylbenzene raw material basin V01,
In dimethyl suflfate material storaging tank V02, the mol ratio of material is double alcohol：Dimethyl suflfate：Toluene=1:1.2:5；Toluene pump
P01 and dimethyl suflfate pump P02 sets 70 degree with 4.38 liters/min of flow velocity, 1.38 liters/min of chargings, heat exchange respectively, into mixing
After clutch MR01, converge with double alcohol aqueous alkalis after First Heat Exchanger E01 heat exchange in micro passage reaction MR02 imports, its
Middle double 3.54 liters/min of the alcohol buck pump P03 flows of control, heat exchange set 70 degree, the first counterbalance valve BPV01 system back pressures
0.8Mpa, after the sufficient hybrid reaction in micro passage reaction MR02, obtain reaction solution；Reaction solution is in the first stage layered tank
Two first of group receive in layering tank V04, V05 and collect layering, obtain reaction solution into the first reaction flow container V07, control reaction
For liquid temperature degree at 60 degree, reaction solution enters washing blender MR03, the second counterbalance valve BPV02 systems from the first reaction flow container V07
Back pressure 0.8Mpa, washing is mixed with a certain amount of water of addition, water feed pump P04 is washed with water in water inlet, from washed reaction device MR03
Reaction solution out is again introduced into two second receptions layering tank V08, V09 of substratification tank group, is subdivided layer processing, place
The reaction solution managed enters reaction solution the first receiving tank V11 and the second receiving tank of reaction solution V12 after washing after washing.Reaction solution from
The second receiving tank of reaction solution V12 is out conveyed into the second heat exchanger E02 through discharging pump P05 and preheated after washing, is entered after preheating and is connected
Continuous desolventizing device D01, toluene is reclaimed by vaporization process, and obtains thick benzylalcohol, thick benzylalcohol content 94.5%, accessory substance bis ether 4%,
Yield 95.2%.
Described above, only example is preferably embodied in the utility model, but the scope of protection of the utility model is not
Limitation and this, any one skilled in the art is in technical scope of the present utility model, according to the utility model
Technical scheme and design are subject to equivalent substitution or change, should all be included within the scope of protection of the utility model.
Claims (5)
1. one kind production 2, the device of 3,5,6-4- methoxyl methyls-tetrafluorobenzyl alcohol, it is characterised in that including methylbenzene raw material basin
（V01）, dimethyl suflfate material storaging tank（V02）, double alcohol aqueous alkali basins（V03）, First Heat Exchanger（E01）, blender
（MR01）, micro passage reaction（MR02）, the first stage layered tank group, substratification tank group, washing blender（MR03）, washing
The receiving tank of reaction solution first afterwards（V11）, the receiving tank of reaction solution second after washing（V12）, the second heat exchanger（E02）, continuous desolventizing
Device（D01）, the 3rd heat exchanger（E03）, the recycling can of toluene first（V14）, the recycling can of toluene second（V15）, finished pot（V13）And
Measuring pump；Described measuring pump includes toluene feed pump（P01）, dimethyl suflfate feed pump（P02）, double alcohol buck feed pumps
（P03）, washing water feed pump（P04）, handle reaction solution feed pump well（P05）, recovery toluene discharging pump（P06）；Described first
Stage layered tank group includes two first reception layering tanks being used alternatingly（V04、V05）, the first waste water tank（V06）With the first reaction
Flow container（V07）；The substratification tank group includes two second reception layering tanks being used alternatingly（V08、V09）, second is useless
Water pot（V10）, the receiving tank of reaction solution first after washing（V11）With the receiving tank of reaction solution after washing second（V12）；The toluene is former
Expect basin（V01）Outlet and toluene feed pump（P01）Import connects, toluene feed pump（P01）Outlet and blender（MR01）
Import connection；Described dimethyl suflfate material storaging tank（V02）Outlet and dimethyl suflfate feed pump（P02）Import connects
Connect, dimethyl suflfate feed pump（P02）Outlet and blender（MR01）Import connection；Double alcohol aqueous alkali basins
（V03）In outlet and double alcohol buck feed pumps（P03）Import connects, double alcohol buck feed pumps（P03）Outlet and the first heat exchange
Device（E01）Import connects；The blender（MR01）Outlet and First Heat Exchanger（E01）Outlet be all connected to the microchannel
Reactor（MR02）Entrance；The micro passage reaction（MR02）Outlet connect simultaneously with two first of the first stage layered tank group
Contracture layer tank（V04、V05）Import connection；Two first of first stage layered tank group receive layering tank（V04、V05）Outlet
The first waste water tank with the first stage layered tank group simultaneously（V06）With the first reaction flow container（V07）Import connection；Described first is anti-
Answer flow container（V07）Outlet and the washing blender（MR03）Import connection；In the washing blender（MR03）On also set
There are water inlet, water inlet and washing water feed pump（P04）It is connected；The washing blender（MR03）Outlet simultaneously and the second level
Be layered tank group two second receive layering tank（V08、V09）Import connection；Two second receptions of substratification tank group
It is layered tank（V08、V09）Outlet simultaneously with the second waste water tank（V10）With the receiving tank of reaction solution after washing first（V11）Import
Connection, the receiving tank of reaction solution first after washing（V11）With the receiving tank of reaction solution after washing second（V12）It is connected；After the washing
The receiving tank of reaction solution second（V12）Outlet pass through with handling reaction solution feed pump well（P05）Import connects, reaction solution feed pump
（P05）Outlet and the second heat exchanger（E02）Charging aperture connects, the second heat exchanger（E02）Discharging opening and continuous desolventizing device（D01）'s
Import connects；The continuous desolventizing device（D01）The gas outlet on top and the 3rd heat exchanger（E03）Import connects, the 3rd heat exchanger
（E03）Outlet and the recycling can of toluene first（V14）With the recycling can of toluene second（V14）Import connects, the recycling can of toluene first
（V14）With the recycling can of toluene second（V14）Discharging opening with recovery toluene discharging pump（P06）Connection, continuous desolventizing device（D01）Under
The discharging opening and finished pot in portion（V13）Connection.
2. production 2 according to claim 1, the device of 3,5,6-4- methoxyl methyls-tetrafluorobenzyl alcohol, it is characterised in that：Institute
The micro passage reaction stated（MR02）By first reactor charging aperture（1）, second reactor charging aperture（2）, a hybrid reaction
Passage（3）, a straight-through reaction channel（7）And discharging opening（6）It is formed by connecting；The hybrid reaction passage（3）It is in inwall
The reaction structure of multistage arc.
3. production 2 according to claim 1, the device of 3,5,6-4- methoxyl methyls-tetrafluorobenzyl alcohol, it is characterised in that：Institute
State washing blender（MR03）It is the combination of conical funnel shape microchannel.
4. production 2 according to claim 1, the device of 3,5,6-4- methoxyl methyls-tetrafluorobenzyl alcohol, it is characterised in that：Institute
State continuous desolventizing device（D01）For the stainless steel negative-pressure cup of sealing, at least four pieces of bands are internally provided with to the evaporation plate of descending slope
（14）, mouth is vaporized in the upper and lower rising for having solvent respectively of tank body（12）With the desolventizing device discharging opening of product（15）.
5. production 2 according to claim 2, the device of 3,5,6-4- methoxyl methyls-tetrafluorobenzyl alcohol, it is characterised in that：Institute
The passage inside dimension for the micro passage reaction stated is 1~8mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720736838.6U CN206902053U (en) | 2017-06-22 | 2017-06-22 | Device for producing 2, 3, 5, 6-4-methoxymethyl-tetrafluorobenzyl alcohol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720736838.6U CN206902053U (en) | 2017-06-22 | 2017-06-22 | Device for producing 2, 3, 5, 6-4-methoxymethyl-tetrafluorobenzyl alcohol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN206902053U true CN206902053U (en) | 2018-01-19 |
Family
ID=61283997
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201720736838.6U Active CN206902053U (en) | 2017-06-22 | 2017-06-22 | Device for producing 2, 3, 5, 6-4-methoxymethyl-tetrafluorobenzyl alcohol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN206902053U (en) |
-
2017
- 2017-06-22 CN CN201720736838.6U patent/CN206902053U/en active Active
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