Double still intermittent reaction devices on probation in one
Technical field
The present invention relates to the synthesis device field of chemical products, specifically one and be applicable to colleges and universities, chemical industry enterprise of scientific research institutions
Industry carries out double still intermittent reaction devices on probation in the middle tester kind of chemical products intermittent reaction.
Background technology
At present, universities, R&D institution, relevant enterprise carry out correlational study and pilot scale used time, reactant at home
In system, many use organic solvents also exist gas odorous discharge.Middle tester in chemical industry synthesis often needs to carry out solid-liquid
Separate, and more in domestic like product be not provided with equipment for separating liquid from solid.Volatile components can be generated in chemical industry building-up process,
Therefore need reactant liquor is carried out rectification or distillation, but current same device is not arranged.Domestic like product is being carried out
During layout, only consider completing of technique, do not consider industrialized zoning.And public work system is the most complete, suitable
Less by scope, layout is the most chaotic.
Summary of the invention
The purpose of the present invention is based on above-mentioned prior art situation and tries out double stills interval in custom-designed one instead
Answering device, this device has the batch reactor that two sets are independent, with Oxytarch etc. as reaction system;It is equipped with independent use
The heating system of different temperatures scope, the cooling recirculation system of imitative industrial equipment is, and independent separation system device and complete
Whole raw materials storage system, is particularly well-suited to colleges and universities, Research Center chemical enterprise in one's power and carries out testing or the chemical industry synthesis of pilot scale is anti-
Should.
It is an object of the invention to be achieved through the following technical solutions:
Still intermittent reaction devices on probation double in one, including raw material system, response system, piece-rate system, finished product system and public
Engineering system,
Described raw material system is by two set Lower tanks, raw material pump, head tank, adjuvant tank and static mixer, feed preheater structure
Becoming, two set Lower tank, raw material pump, head tank, adjuvant tanks are in being arranged in parallel;
Described response system is made up of the batch reactor of two and the heat exchanger of correspondence, circulating pump, and one of them reactor is
Neutralizing still, another is distillating still, two reactors or used in parallel to expand respond, or is used in series that to carry out two steps anti-
Should;
Described piece-rate system is made up of distillation column, centrifuge, and the distillating still in response system is with the distillation column in piece-rate system even
Connect, the solvent used in the light component produced in separating reaction or recovery course of reaction;Centrifuge respectively with reaction
The circulating pump that two reactors in system are corresponding is connected, for separating the solid phase components in any reactor;
Described finished product system is made up of mother liquor tank, finished pot, light phase tank, mother liquor tank and the centrifuge in piece-rate system, reaction system
Circulating pump in system is connected, and is used for collecting isolated mother solution, and by circulating pump, mother solution is got in response system
Row recycles, and finished pot is connected with two reactors in response system respectively, is used for collecting the finished product reflected;Light phase tank
It is connected with the distillation column in piece-rate system, is used for collecting light component finished product;
Described public engineer system is made up of circulating cooling water unit, steam heating unit, heat-conducting oil heating unit, main basis
The maintenance of process requirements and control the temperature of whole device, wherein circulating cooling water unit and the reactor in response system, change
In hot device and piece-rate system, distillation column is connected;Steam heating unit and reactor, heat exchanger and the raw material system in response system
Middle feed preheater is connected;Heat-conducting oil heating unit is connected with the reactor in response system.
In the present invention, the ratio of height to diameter of the reactor in described response system is 1: 1, and the ratio of height to diameter of distillating still is 1.2: 1,
To adapt to different reaction systems.
Described centrifuge is link-suspended basket centrifuge, it is achieved solid-liquid separation, and can carry out by changing the filter cloth of different meshes
The separation of different grain size reactant liquor.
Described circulating cooling water unit is by cooling down water storage tank and cooling water circulating pump forms.
By hotline heater, conduction oil emergency storage tank, (its effect is to prevent conduction oil to described heat-conducting oil heating cycling element
Expand the accident caused) and heat conduction oil circulating pump composition.
Described steam heating unit is made up of steamdrum, steam generator and water softener.
In two reactors, it is equipped with the general shaft with logical key, it can change difference according to process requirements
The stirring paddle of type.
This pair of still intermittent reaction device is applicable to Oxytarch reaction system.
More specific description of the present invention is as follows:
Raw material system is by two raw material pumps, two Lower tanks, two head tanks and two adjuvant tank preheaters and static mixer
Composition.Raw material is input to head tank A and head tank B by Lower tank A and B through raw material pump A and B and is jointly mixed into adjuvant tank A and B
Static mixer is sufficiently mixed and preheats at inflow feed preheater.
Response system is formed by neutralizing still, distillating still, neutralization still heat exchanger, distillating still heat exchanger and outer circulation pump.Instead
Answering process: material is entered reactor reaction by feed preheater, carries out heat exchange subsequently into heat exchanger, product enters and separates dress
Put.
Piece-rate system is made up of centrifuge, distillation column, overhead condenser, intermediate storage tank, condensed fluid booster pump.Via raw material
The material that system conveying comes enters centrifuge and realizes solid-liquid separation;Material is entered distillation by centrifuge, neutralization still and distillating still
Tower realizes gas-liquid separation, and distillation column gas out enters overhead condenser and is transported to intermediate storage tank, by condensed fluid booster pump
Carry out backflow and quantitative extraction.
Product systems are made up of mother liquor tank, finished pot, tower top finished pot.Material is entered mother liquor tank by centrifuge and stores standby
With, the material of masterbatch tank enters back into distillation column;Through overhead condenser material from intermediate storage tank enter tower top finished pot store.
Public engineer system is made up of cooling water circulation unit, heat-conducting oil heating unit, steam heating unit.Cooling water follows
Ring element by cooling down water storage tank, cooling water circulating pump forms, cooling water refluxes from the cooling cooled water-circulating pump of water storage tank;
Heat-conducting oil heating unit is made up of hotline heater, conduction oil emergency storage tank, heat conduction oil circulating pump.Emergency storage tank follows through conduction oil
Ring pump enters reactor.Conduction oil is back to hotline heater.Steam-heating system is by steamdrum and steam generator, soft water
Device is constituted.Tap water flows through water softener and flows into steam generator, and steam is assigned to response system and raw material after being transported to steamdrum
System.
The present invention has following functions and feature: package unit uses industrialization layout to be divided into raw material district, reaction zone, separation
District, product zone and public engineering area.There are two raw material Lower tanks and two head tanks and two storage tanks can carry out pre-
Mixed, it is also equipped with preheater and raw material can be preheated by low-pressure steam;And there is equipment for separating liquid from solid and gas-liquid separation device,
Stable separation and Extraction operation can be built;Two overlap independent batch reactor can carry out use in series or in parallel, two intervals
Stirring paddle in reactor can the current version agitator such as on-demand replacing anchor formula, frame, six straight leaf disc formulas;Course of reaction uses
With Oxytarch etc. as reaction system, safety operation can be carried out in the environment of not possessing ventilation condition;Tester in Tong Shi
Material heating in middle heat-conducting oil heating system and the applicable 0~300 DEG C of temperature range of steam-heating system, complete cooling follows
Loop systems can realize being carried out continuously of intermittent reaction.
Accompanying drawing explanation
Fig. 1 is double still intermittent reaction main material flow figures;
Fig. 2 is double still intermittent reaction device recirculating cooling water system figures;
Fig. 3 is double still intermittent reaction device heat-conducting oil heating system figures;
Fig. 4 is double still intermittent reaction device steam-heating system figures;
Fig. 5 always schemes for double still intermittent reaction device technique flow processs;
In Fig. 1-5: 1 head tank A, 2 adjuvant tank A, 3 adjuvant tank B, 4 head tank B, 5 static mixers, 6 raw materials
Preheater, 7 raw material pump A, 8 Lower tank A, 9 raw material pump B, 10 Lower tank B, 11 centrifugal pumps, in 12 and still,
13 centrifuges, with still heat exchanger in 14,15 outer circulation pump A, 16 distillating stills, 17 distillating still heat exchangers, outside 18
Circulating pump B, 19 distillation column, 20 overhead condensers, 21 intermediate storage tanks, 22 condensed fluid booster pumps, 23 mother liquor tanks,
24 finished pots, 25 tower top finished pots (the most light phase tank), 26 cooling water storage tanks, 27 cooling water circulating pump A, 28 coolings
Water-circulating pump B, 29 conduction oil emergency storage tanks, 30 hotline heaters, 31 heat conduction oil circulating pumps, 32 steamdrums, 33
Steam generator, 34 water softener.
Detailed description of the invention
The present invention is described in further detail below in conjunction with accompanying drawing:
As Figure 1-5: double still intermittent reaction devices on probation in one, including raw material system, response system, piece-rate system, one-tenth
Strain system and public engineer system,
Described raw material system is by two set Lower tanks, raw material pump, head tank, adjuvant tank and static mixer, feed preheater structure
Becoming, two sets Lower tank (8,10), raw material pump (7,9), head tank (1,4), adjuvant tank (2,3) are in being arranged in parallel;
Described response system is made up of, wherein the batch reactor of two and 14,17, two circulating pumps of two heat exchangers of correspondence
One reactor is for neutralizing still 12, and another is distillating still 16, two reactors or used in parallel to expand respond, or string
Connection use carries out two-step reaction;
Described piece-rate system is made up of distillation column 19, separator (i.e. centrifuge 13), the distillating still 16 in response system with separate
Distillation column 19 in system connects, the light component that produces in separating reaction or reclaim used in course of reaction molten
Agent;Separator is connected with two reactors in response system, two circulating pumps, the solid phase group in separating reaction system
Point;
Described finished product system is made up of mother liquor tank 23, finished pot 24, light phase tank 25, mother liquor tank 23 and the centrifuge in piece-rate system
13, the circulating pump in response system is connected, and is used for collecting isolated mother solution, and by circulating pump, mother solution is got to reaction
Being circulated use in system, finished pot 24 is connected with two reactors in response system, is used for collecting the finished product reflected;
Light phase tank 25 is connected with the distillation column 19 in piece-rate system, is used for collecting light component finished product;
Described public engineer system is made up of circulating cooling water unit, steam heating unit, heat-conducting oil heating unit, main basis
The maintenance of process requirements and control the temperature of whole device, wherein circulating cooling water unit and the reactor in response system, change
In hot device and piece-rate system, distillation column is connected;Steam heating unit and reactor, heat exchanger and the raw material system in response system
Middle feed preheater is connected;Heat-conducting oil heating unit is connected with the reactor in response system.
The present invention's is as follows from the generation process and material flow accompanying drawings feeding, reacting, be separated to finished product:
As shown in Figure 1: this flow process is universal interval class reaction system, two kinds of principal goods material participating in reaction are respectively added to low level
Groove A8, Lower tank B10, the adjuvant participating in reaction adds adjuvant tank A2, adjuvant tank B3, any two in principal goods material, auxiliary material to
Planting or two or more materials flows through static mixer 5 and sufficiently mixes, need not pre-if flowing through feed preheater 6(
Heat, can directly open bypass), flow through neutralization still 12, in neutralizing still, maintain certain pressure, temperature, time, feed liquid warp after reaction
Cross outer circulation pump A15, after neutralizing still heat exchanger 14, enter distillating still 16, in distillating still 16, (new raw material can be supplemented
Or adjuvant) maintaining certain pressure, temperature, time, after reaction, feed liquid is through outer circulation pump B18, after distillating still heat exchanger 17
Enter finished pot 24.According to technique needs, corresponding heat release or obvious reaction system of absorbing heat, neutralize in course of reaction still/
In distillating still reactant liquor respectively can through outer circulation pump, neutralize still distillating still ring heat exchanger return to neutralize still/distillating still, reach
Purpose to still external circulation heat exchanging.
If producing solid matter in neutralizing still or distillating still, the most outside circulating pump A directly feed liquid is squeezed into after B
Centrifuge 13, solid is stayed in the rotary drum of centrifuge, and liquid is as entering mother liquor tank 23, mother liquor tank after mother solution centrifugal pump 11 supercharging
Middle mother solution according to technique need to enter outer circulation pump A before B, neutralization still 12 can be arrived or distillating still 16 is circulated.
If distillating still reaction system producing gas-phase product or needing recycling design, distillating still 16 is heated to accordingly
Temperature, gaseous substance enters bottom distillation column 19, is flowed into overhead condenser 20 at tower top after tower inner transmission matter conducts heat, passes through
Becoming condensed fluid after condensation and enter into intermediate storage tank 21, the liquid of intermediate storage tank 21 divides two after subcooling condensate booster pump 22 supercharging
Road, wherein a road returns to distillation column 19 top and maintains the stable operation of distillation column, and an other road is directly entered tower top finished pot 25.
The circulating cooling water unit accompanying drawings of the present invention is as follows:
As shown in Figure 2: the recirculated cooling water in cooling water storage tank 26 through cooling water circulating pump A27 after B28 supercharging according to technique
Demand delivers to neutralize in the cooling coil in still 12, distillating still 16 or enter into neutralization still heat exchanger 14 respectively, distillating still changes
Hot device 17, overhead condenser 20 cool down, and then return to cool down water storage tank 26 by return main road.
The heat-conducting oil heating unit accompanying drawings of the present invention is as follows:
As shown in Figure 3: conduction oil is heated to uniform temperature, warp in conduction oil emergency storage tank 29 enters into hotline heater 30
Deliver to respectively neutralize in the conduction oil coil pipe in still 12, distillating still 16 according to process requirements after crossing conduction oil mixing pump 31 change
Heat, then returns to hotline heater 30 by conduction oil loop.
The steam-heating system accompanying drawings of the present invention is as follows:
As shown in Figure 4: water enters steam generator 33 after being exchanged by ion exchange column, and steam is divided into three by steamdrum 32
Road a: wherein road enters neutralization still heat exchanger 14 as required, distillating still heat exchanger 17 carries out heat exchange, after steam is condensed into liquid
Flow directly into trench;Wherein a road needs according to technique to enter in the chuck neutralized in still 12, distillating still 16, laggard through condensation
Enter to flow into trench;3rd tunnel is condensed into liquid after the shell side of feed preheater 6 and flows into trench.
The present invention on the basis of above-mentioned course of reaction and operation principle, each critical piece is further equipped with following metering, monitoring,
The functional accessory such as display, control:
Raw material district Lower tank 8,10 and head tank 1,4 are equipped with liquidometer can observe the change of raw material liquid level, at any time at head tank 1,4
And be provided with spinner flowmeter between Lower tank 8,10 material flow is accurately measured.By head tank 1,4, adjuvant tank 2,3 and
Raw material is premixed by static mixer 5, and then the raw material after premix can be preheated by feed preheater 6.
The equipment for separating liquid from solid of Disengagement zone, is main to be provided with filtrate tanks and can reclaim filtrate with centrifuge 13.Pass through
Centrifuge 13 is replaced the filter cloth of different meshes to realize the separation of different grain size reactant liquor.The separation of liquid phase is by steaming
Evaporate tower 19 to realize, distillation column 19 is provided with liquidometer and carries out liquid level monitoring.Distillate component and carry out cold by overhead condenser 20
Lime set is recycled to intermediate storage tank 21, and is provided with condensed fluid booster pump 22 on intermediate storage tank 21.Material flows to through intermediate storage tank 21
It is respectively equipped with spinner flowmeter between distillation column 19 and tower top finished pot 25 and pipeline, condensed fluid quantitatively can be refluxed or adopt
Go out.
Course of reaction can realize by neutralizing still 12, distillating still 16, and two stills can according to difference require to carry out series connection and
Used in parallel.Two stills are respectively equipped with temperature sensor can to reactor in liquid level carry out Automated condtrol.Also set on two stills
Internal pressure and thermometer carry out temperature test to have Pressure gauge to show.Two stills are designed with two jacket heating systems can realize conduction oil
And steam heating, it is adaptable to the temperature range of differential responses.After two stills, it is provided with heat exchanger 14,17 carries out heat exchange, heat exchanger 14,
17 import and export are designed with temperature indicator, measure variations in temperature before and after heat exchange.
Hotline heater 30 in heating system is provided with limit switch, and oil temperature in heater is carried out automatization's control
System.It is designed with temperature indicating device in the conveying and reflux course of conduction oil.Hotline heater is provided with emergency storage tank 29,
Emergency storage tank is provided with liquid level low-level alarm.Steam adds the steam generator 33 hankered and is provided with rotating speed control table, to liquid level
Carry out Automated condtrol, prevent liquid level too high or too low.Temperature is automatically controlled by temperature sensor.At steam generator 33
Before be provided with water softener, tap water is carried out sofening treatment, after be provided with the vapours that steamdrum 32 provides stable.Steamdrum sets
There are Pressure gauge and drain valve, the condensed fluid in steamdrum can be discharged.
Cooling water storage tank 26 in cooling is provided with rotating speed control table, and cooling water inlet is provided with temperature indicating device, cold
But water storage tank 26 is provided with cooling water circulating pump A, B, is provided with Pressure gauge, the using and the reserved after pump, uses turbine flowmeter to enter simultaneously
The consumption of row batching cycle water.