CN109925989A - A kind of liquid-phase reaction system - Google Patents
A kind of liquid-phase reaction system Download PDFInfo
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- CN109925989A CN109925989A CN201910249509.2A CN201910249509A CN109925989A CN 109925989 A CN109925989 A CN 109925989A CN 201910249509 A CN201910249509 A CN 201910249509A CN 109925989 A CN109925989 A CN 109925989A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 80
- 239000007791 liquid phase Substances 0.000 title claims abstract description 35
- 239000002994 raw material Substances 0.000 claims abstract description 31
- 238000012544 monitoring process Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims description 19
- 238000004804 winding Methods 0.000 claims description 2
- 230000008676 import Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 16
- 238000010924 continuous production Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000011344 liquid material Substances 0.000 description 28
- 239000000047 product Substances 0.000 description 16
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 15
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 11
- 238000002156 mixing Methods 0.000 description 11
- 230000008569 process Effects 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- XQXMBCRAZQYYPS-UHFFFAOYSA-N [Na].C(N)(O)=O Chemical compound [Na].C(N)(O)=O XQXMBCRAZQYYPS-UHFFFAOYSA-N 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- GSFSVEDCYBDIGW-UHFFFAOYSA-N 2-(1,3-benzothiazol-2-yl)-6-chlorophenol Chemical compound OC1=C(Cl)C=CC=C1C1=NC2=CC=CC=C2S1 GSFSVEDCYBDIGW-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 206010024769 Local reaction Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012806 monitoring device Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 210000000664 rectum Anatomy 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Physical Or Chemical Processes And Apparatus (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of liquid-phase reaction systems, it include: raw material feeding assembly, it includes at least two sets, raw material feeding assembly described in every set includes passing through the sequentially connected head tank of pipeline, dosing pump, measuring tank and feeding engine, the wherein measuring tank at least two, mutually and it is connected between the dosing pump and feeding engine, and the inlet port and outlet port of each measuring tank are equipped with control valve；Micro passage reaction connects the feeding engine and finished pot；And monitoring system comprising control machine and the finished product sensor set on the micro passage reaction downstream, the finished product sensor couple with the control machine signal, and the control machine controls the opening and closing of aforementioned all control valves and all dosing pumps, feeding engine.The beneficial effect comprise that using micro passage reaction for reacting environment, continuous production is realized, the magnitude of each reaction is small, highly-safe；Liquid phase feed rapid reaction and abundant, reaction accuracy height, and realize the automation of production.
Description
Technical field
The present invention relates to a kind of liquid-phase reaction systems.
Background technique
Existing liquid phase reactor is usually that liquid phase feed is all poured into reaction kettle in proportion, under certain condition (such as
Temperature adjustment, pressure regulation etc.) reaction certain time, during which it is aided with the mixing that the modes such as stirring help raw material, is obtained in final reaction kettle whole
A final product.Have the disadvantage that 1, reaction process is intermittent, it is necessary to which the reaction to present lot in reaction kettle carries out
It is complete, it just can be carried out the reaction of next batch, cannot achieve continuous production；2, the magnitude of each reaction is big, once operation thing occurs
Therefore danger coefficient is big, wastage of material is big；3, reaction mass distributing precision is low, and reaction mass homogeneous speed is slow, causes reaction raw materials
Insufficient or excessive, part generates side reaction object and local reaction is insufficient；It 4, is the reacting dose for adapting to different batches variation, every time
Reaction needs pointedly to adjust corresponding process parameters, this process is played can only be according to the experience adjustments of operator, it is difficult to realize
Automated production.
Summary of the invention
It is an object of the invention to overcome above-mentioned technical deficiency, a kind of liquid-phase reaction system is proposed, solve in the prior art
It cannot achieve the technical issues of continuous production, the magnitude of each reaction are big, reaction precision is low and are difficult to realize automated production.
To reach above-mentioned technical purpose, technical solution of the present invention provides a kind of liquid-phase reaction system, comprising:
Raw material feeding assembly comprising at least two sets, raw material feeding assembly described in every set includes being sequentially connected by pipeline
Head tank, dosing pump, measuring tank and feeding engine mutually and be connected in the dosing pump wherein the measuring tank at least two
Between feeding engine, and the inlet port and outlet port of each measuring tank are equipped with control valve；
Micro passage reaction connects the feeding engine and finished pot；And monitoring system comprising control machine and be set to institute
The finished product sensor in micro passage reaction downstream is stated, the finished product sensor couples with the control machine signal, the control machine
Control the opening and closing of aforementioned all control valves and all dosing pumps, feeding engine.
Compared with prior art, the beneficial effect comprise that using micro passage reaction for reacting environment, the company of realization
Continuous production substantially increases production efficiency, and because being that microchannel plate is answered, the magnitude of each reaction is small, highly-safe；Liquid phase
Raw material mixed in micro passage reaction sufficiently, rapid reaction and sufficiently, greatly reduce the generation of side reaction object；Every set raw material
Feeding assembly is equipped at least two measuring tanks, and the continuous feeding system of alternately metering, blowing is formed with the help of each control valve,
And it feeds back, is adjusted in real time by control machine micro- logical in conjunction with real-time monitoring of the finished product sensor in micro passage reaction downstream to finished product
The raw material supply amount of road reactor upstream to ensure that the accuracy of reaction, and realizes the automation of production.
Detailed description of the invention
Fig. 1 is the schematic illustration of liquid-phase reaction system of the present invention；
Fig. 2 is the structural schematic diagram of micro passage reaction microchannel of the present invention；
Fig. 3 is one structural schematic diagram of embodiment of micro passage reaction cutoff board of the present invention；
Fig. 4 is Section A-A figure in Fig. 3；
Fig. 5 is two structural schematic diagram of embodiment of micro passage reaction cutoff board of the present invention；
Fig. 6 is section B-B figure in Fig. 5；
Fig. 7 is three structural schematic diagram of embodiment of micro passage reaction cutoff board of the present invention；
Fig. 8 is C-C sectional view in Fig. 7；
Fig. 9 is Fig. 7 another kind status diagram.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
As shown in Figure 1, the present invention provides a kind of liquid-phase reaction systems, comprising: raw material feeding assembly 100, microchannel plate
Answer device 200 and monitoring system 300.
Raw material feeding assembly 100 includes at least two sets, and raw material feeding assembly 100 described in every set includes successively being connected by pipeline
Head tank 110, dosing pump 120, measuring tank 130 and the feeding engine 140 connect, wherein the measuring tank 130 at least two, mutually
And it is connected between the dosing pump 120 and feeding engine 140, and the inlet port and outlet port of each measuring tank 130 are equipped with
Control valve 150.
Micro passage reaction 200 connects the feeding engine 140 and finished pot 400.
Monitoring system 300 includes control machine 310 and the finished product sensor 320 set on 200 downstream of micro passage reaction,
The finished product sensor 320 couples with 310 signal of control machine, the control machine 310 control aforementioned all control valves 150 and
The opening and closing of all dosing pumps 120, feeding engine 140.
It is illustrated so that synthesization of dimethyl disulfide is for carbamic acid sodium as an example below.Sodium dimethyl dithiocarbamate
Production is that liquid alkaline, dimethylamine and carbon disulfide these three liquid phase feeds are put into reaction kettle to be thoroughly mixed, certain time
After obtain.
The reacting environment of existing production technology is reaction kettle, and production technology is compartment operation mode, unavoidably two
When these effumability raw material measuring tanks of methylamine, carbon disulfide are fed, uncontrollable discharge can be generated when reaction kettle loading and unloading.And
And when feedstock, it will cause since this metering method is measured using range estimation compared with the matter of fundamental importance using measuring tank metering feeding
Error is measured, to influence quality of finished, or even also needs to carry out polishing purification technique, unavoidably causes the increase of discharge of wastewater.
In addition, in order to improve output, domestic production enterprise is all but dimethylamine, curing using 2000L or more autoclave produced
Carbon raw material is all low boiling point, volatile, inflammable and explosive chemicals, and there is great security risks for this, once safe thing occurs
Therefore a large amount of raw material stores and brings acid test to safety in production in workshop.In addition, being operated using autoclave, need a large amount of
Operator, high labor cost.
When in use using this liquid-phase reaction system, every set raw material feeding assembly 100 is directed to a kind of reaction raw materials, by matching
Raw material is sent into measuring tank 130 by head tank 110 respectively and measured by material pump 120, measuring tank 130 and feeding engine 140, is re-fed into micro- logical
Road reactor 200 is sufficiently mixed reaction, finally sends out finished product, either raw material or finished product, and whole process is all in sealed environment
In, the leakage point can not be discharged, uncontrollable discharge greatly reduces.The above various pumps can use the pump of JYS series, such as
JYSZZ-100/4.0, JYSZZ-58/7.2, JYSZZ-110/9 etc..Measuring tank can use the Weighing module of plum Teller, such as
MT1041-20KG。
In the metering process to liquid phase feed, at least two are set side by side measuring tank 130, such as double measuring tanks, to original
While material realizes precise and tiny metering, alternately metering, blowing can be achieved with the help of each control valve 150, it can accomplish not stop
Machine continuous production.Each control valve can use pneumatic ball valve.Also, in conjunction with the finished product sensor in 200 downstream of micro passage reaction
To the real-time monitoring feedback of finished product, the raw material supply amount of 200 upstream of micro passage reaction is adjusted in real time by control machine, to guarantee
The accuracy of reaction, and realize the automation of production.Wherein finished product sensor can be gas chromatograph or liquid phase color
Spectrometer etc., to infer the distributing precision of reaction raw materials, can specifically select peace prompt by the residual quantity of certain raw material in detection finished product
The 7890A model gas chromatograph of human relations measures the content of dimethylamine in raw material.For example, when single material metering has deviation, control
Machine processed automatically adjusts dosing pump, it is ensured that deviation is no more than 100 grams, and (this precision is in existing compartment industrialized production can not be real
Existing), when deviation is greater than 100 grams or when other control machines can not be corrected, controls chance autostop and alarm, manually
It searches analysis reason and excludes post-fault system and could restore, it is ensured that product quality and raw material do not waste.Using this liquid phase
The disposable sintetics of reaction unit reduces process procedure, greatly reduces production cost even without disposing again through purification.
Since the reacting environment of this liquid-phase reaction system is micro passage reaction 200, the reactor internal procedure material total amount
It is typically not greater than 5kg, material summation is generally also no more than 80kg in raw material feeding assembly 100, and reactor latus rectum can be 20nm,
Pressure-bearing is more than 20MPa, and safety in production has obtained great guarantee.In addition monitoring system 300 and feed sump carry out chain control,
Further cooperate dimethylamine, Carbon Disulfide monitoring device, an amount system leak, 300 on-line checking concentration of monitoring system
System can be closed in first time after exceeded, once the chain accident prevention that is cut to of accident provides guarantee；It is automatic by control machine
Control automatic deviation correction adjustment avoids the maloperation factor of people.
This liquid-phase reaction system realizes automation control, and per tour only needs two patrol officers when production, operates without process,
Labor wage cost declines to a great extent.It, will be in the real-time production information of this liquid-phase reaction system if further cooperating technology of Internet of things
Cloud is passed to, it can be achieved that administrator is checked and controlled by portable hand-held terminal.
In order to optimize the structure of micro passage reaction 200, propose following concrete scheme: the micro passage reaction 200 is wrapped
The shell equipped with material inlet and product outlet is included, and is disposed in the housing and connects the material inlet and product outlet
The quantity of microchannel, the quantity of the material inlet and the raw material feeding assembly 100 is adapted.So that a variety of liquid phase feeds are equal
It can smoothly enter into and be reacted in micro passage reaction 200.
As shown in Fig. 2, the microchannel includes a series of heart-shaped knots of head and the tail series winding as a kind of specific embodiment
Structure unit 221, each heart-shaped structure unit is interior to be equipped with flow-stopping plate 222,222 several through-holes 223 of arrangement on the flow-stopping plate.In figure
Arrow direction is the flow direction of liquid phase feed, it is seen then that after liquid phase feed is pumped into micro passage reaction, is mixed in microchannel
It closes, the heart-shaped structure unit 221 of microchannel is disturbed liquid material is mixed, and stimulates being mutually mixed for liquid material, and flow-stopping plate 222 changes
The flow direction for mixing liquid material, sufficiently disturbs liquid material.Wherein, the shape of flow-stopping plate 222 can be and heart-shaped structure unit 221
Adaptable arc can cook up disturbance runner to make full use of the inner space of heart-shaped structure unit 221.It is distributed in gear
Through-hole 223 in flowing plate 222 is that mixing liquid material increases the access stopped by flow-stopping plate 222, by the liquid material structure of the access
At the liquid material lateral impact to flow-stopping plate 222 is bypassed, to further improve the disturbance of liquid material, further improve mixing
Adequacy.Advanced optimize mixing scheme, propose following scheme: the through-hole edge is with the entrance of the heart-shaped structure unit
The directions of rays arrangement that starting point is radiated around.Such arrangement can reduce kinetic energy of the liquid material by the through-hole 223 when
Loss guarantees to form enough impact forces to around the liquid material of flow-stopping plate 222, and the through-hole 223 is with radial arrangement side
Formula can make flow-disturbing uniform.
In view of many chemical reactions there are certain requirements mixing sequence, following scheme: the microchannel plate is proposed to this
To answer device 200 further include the passage 240 for connecting the material inlet 230 and microchannel, and if in the passage 240
Dry cutoff board 250, if the cutoff board 250 passage 240 is separated into it is corresponding with 230 quantity of material inlet
Mainstream road, and the cutoff board 250 can sliding axially along the passage 240, as shown in Fig. 2~Fig. 9.By sliding flow blocking
Plate 250 to change the opportunity that the adjacent liquid material that it is separated is met, that is, is realized with changing its length in passage 240
The control of feeding sequence when to liquid phase feed mixing.Or by taking synthesization of dimethyl disulfide is for carbamic acid sodium as an example, raw material is liquid
Alkali, dimethylamine and carbon disulfide these three, the material inlet 230 is correspondingly arranged 3 (respectively 230a, 230b, 230c), needle
To the cutoff board 250, following three kinds of specific embodiments are proposed.
Embodiment 1: as shown in Figure 3 and Figure 4, the two sides of the cutoff board 250 inner wall with the passage 240 respectively
It is slidably connected.Specifically, the inner wall of the passage 240 can axially arrangement guide rail 260, the cutoff board 250 be two pieces along it
Passage 240 is separated into 3 runners (240a, 240b, 240c) by (250a, 250b), with the aforementioned liquid alkaline of correspondence, dimethylamine and
Three kinds of liquid phase feeds of carbon disulfide.At this point, purposefully making side by the length for adjusting cutoff board 250a and cutoff board 250b
Liquid material in runner 240a or 240b is contacted with the liquid material in intermediate flow channel 240b first, then again with another side runner 240b or
Liquid material mixing in 240a, to realize the technique purpose for launching liquid material in a designated order.
Embodiment 2: as shown in Figure 5 and Figure 6, a side of all cutoff boards 250 is mutually slidably connected, another side
Inner wall with the passage 240 is slidably connected.A side of one of them cutoff board 250 is equipped with guide rail, other
The respective side of one cutoff board 250 is slidably connected with the guide rail.Difference from Example 1 is, flow blocking in the present embodiment
Any two in three runners that plate 250 is separated out are adjacent, i.e., liquid material there are three types of in the case where, adjust any cutoff board
250, which can be realized the two kind liquid materials adjacent with the cutoff board 250, preferentially mixes, i.e., any two kinds of liquid materials, which may be implemented in, first mixes
It closes, is then mixed again with the third liquid material.
Embodiment 3: as shown in fig. 7~fig. 9, the cutoff board 250 is the tubular plate being mutually arranged, each cutoff board 250
Outer wall be slidably connected with 250 inner wall of cutoff board being sheathed on outside it, the outer wall of outermost layer cutoff board 250 and the passage
240 inner wall is slidably connected；Gap, outermost layer cutoff board 250 between each cutoff board 250 cutoff board 250 adjacent thereto
The inner cavity in gap and innermost layer cutoff board 250 between the passage 240 forms the runner.It is different from embodiment 2 it
Be in, not only may be implemented liquid material be three kinds in the case where any two kinds of liquid materials first mixing, the present embodiment can be real
The mixing of the random order of incumbent meaning liquid material kind number, the scope of application are wider.In the state of Fig. 7, liquid material in runner 240a with
Liquid material in runner 240b formerly mixes, and then mixes with the liquid material in runner 240c；In the state of Fig. 9, in runner 240b
Liquid material formerly mixed with the liquid material in runner 240c, then mixed with the liquid material in runner 240a.
In order to guarantee the adequacy of reaction, it is further proposed that following scheme on the basis of above-mentioned all schemes: please again
Refering to fig. 1, the micro passage reaction 200 further includes the circulating pump 210 for connecting its product outlet and material inlet 230, this is followed
Ring pump 210, which is also controlled by the control machine 310, to be opened and closed.Certain reactions for not needing longer response path are made to return to microchannel plate
It answers device 200 to undergo mixing again, has elongated reaction tube side.
The above described specific embodiments of the present invention are not intended to limit the scope of the present invention..Any basis
Any other various changes and modifications that technical concept of the invention is made should be included in the guarantor of the claims in the present invention
It protects in range.
Claims (10)
1. a kind of liquid-phase reaction system, characterized by comprising:
Raw material feeding assembly comprising at least two sets, raw material feeding assembly described in every set includes passing through the sequentially connected original of pipeline
Batch can, dosing pump, measuring tank and feeding engine, wherein the measuring tank at least two, mutually and is connected in the dosing pump and send
Between material pump, and the inlet port and outlet port of each measuring tank are equipped with control valve；
Micro passage reaction connects the feeding engine and finished pot；And monitoring system comprising control machine and be set to described micro-
The finished product sensor in channel reactor downstream, the finished product sensor couple with the control machine signal, the control machine control
The opening and closing of aforementioned all control valves and all dosing pumps, feeding engine.
2. liquid-phase reaction system according to claim 1, it is characterised in that: the micro passage reaction includes being equipped with raw material
The shell of import and product outlet, and it is disposed in the housing and connects the microchannel of the material inlet and product outlet, institute
The quantity of the quantity and the raw material feeding assembly of stating material inlet is adapted.
3. liquid-phase reaction system according to claim 2, it is characterised in that: the microchannel includes a system of head and the tail series winding
Column heart-shaped structure unit, each heart-shaped structure unit is interior to be equipped with flow-stopping plate, arranges several through-holes on the flow-stopping plate.
4. liquid-phase reaction system according to claim 3, it is characterised in that: the through-hole is along with the heart-shaped structure unit
Entrance be starting point radiate around directions of rays arrangement.
5. liquid-phase reaction system according to claim 2, it is characterised in that: the micro passage reaction further includes connection institute
The passage of material inlet and microchannel is stated, and several cutoff boards in the passage, the cutoff board are led described
Expects pipe is separated into several runners corresponding with the material inlet quantity, and the cutoff board can be along the axial direction of the passage
Sliding.
6. liquid-phase reaction system according to claim 5, it is characterised in that: the two sides of the cutoff board respectively with it is described
The inner wall of passage is slidably connected.
7. liquid-phase reaction system according to claim 5, it is characterised in that: a side of all cutoff boards is mutually sliding
Dynamic connection, inner wall of another side with the passage are slidably connected.
8. liquid-phase reaction system according to claim 7, it is characterised in that: a side of one of them cutoff board is set
There is guide rail, the respective side of other any cutoff boards is slidably connected with the guide rail.
9. liquid-phase reaction system according to claim 5, it is characterised in that: the cutoff board is the tubular being mutually arranged
Plate, the outer wall of each cutoff board are slidably connected with the cutoff board inner wall being sheathed on outside it, the outer wall of outermost layer cutoff board with it is described
The inner wall of passage is slidably connected；Gap, outermost layer cutoff board between each cutoff board cutoff board adjacent thereto with it is described
The inner cavity in gap and innermost layer cutoff board between passage forms the runner.
10. according to any liquid-phase reaction system of claim 2~9, it is characterised in that: the micro passage reaction also wraps
The circulating pump of connection its product outlet and material inlet is included, which is also controlled by the control machine and be opened and closed.
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