CN106000251B - Double kettle intermittent reaction devices are tried out in one kind - Google Patents
Double kettle intermittent reaction devices are tried out in one kind Download PDFInfo
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- CN106000251B CN106000251B CN201610449970.9A CN201610449970A CN106000251B CN 106000251 B CN106000251 B CN 106000251B CN 201610449970 A CN201610449970 A CN 201610449970A CN 106000251 B CN106000251 B CN 106000251B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00002—Chemical plants
- B01J2219/00004—Scale aspects
- B01J2219/00009—Pilot-scale plants
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Abstract
Double kettle intermittent reaction devices, including raw material system, reaction system, piece-rate system, finished product system and public engineer system are tried out in one kind.The method have the characteristics that：With two sets of independent batch reactors, the agitating paddle that can be changed on demand is equipped with, with oxidized starch etc. for reaction system；Two sets of heating systems for being applied to different temperatures scope, the cooling recirculation system of industrial equipment is imitated, using turbine flowmeter batching cycle water consumption, be equipped with independent separate system and complete raw materials storage system device.Batch reactor ratio of height to diameter is 1 in a device：1 and 1.2:1, the agitating paddle provisioned in per kettle can be changed on demand, and mixing speed can carry out stepless speed regulation in 0 ~ 120r/min.The circulatory system of imitative industrial equipment includes soft brush treatment device and circulating pump is applied to that water quality is harder, occasion without processing unit uses.Quantitative extraction and backflow can be carried out comprising independent gas-liquid separation device, is operated with the stable separation and Extraction of structure.
Description
Technical field
The present invention relates to the synthesis device field of chemical products, is specifically that one kind is applied to colleges and universities, chemical industry enterprise of scientific research institutions
Industry carries out the middle tester of chemical products intermittent reaction --- double kettle intermittent reaction devices are tried out in kind.
Background technology
At present, universities, R＆D institution, relevant enterprise carry out correlative study and pilot scale used time, reactant at home
It is more in system that using organic solvent, there is odorous gas to discharge.Often need to carry out solid-liquid in the middle tester of chemical industry synthesis
Separation, and more in domestic like product it is not provided with equipment for separating liquid from solid.Volatile components can be generated during chemical industry synthesis,
Therefore rectifying or distillation need to be carried out to reaction solution, but is not set in same device at present.Domestic like product is being carried out
During arrangement, only consider the completion of technique, do not consider industrialized zoning.And public work system is not complete enough, fit
Smaller with scope, layout is more chaotic.
The content of the invention
It is anti-that double kettle intervals are tried out in one kind that the purpose of the present invention is based on above-mentioned prior art situation and specially designed
Device is answered, the device has two sets of independent batch reactors, with oxidized starch etc. for reaction system；It is equipped with independent use
The heating system of different temperatures scope, imitate the cooling recirculation system of industrial equipment, and independent separation system device and complete
Whole raw materials storage system, especially suitable for colleges and universities, Research Center, chemical enterprise is tested in one's power or the chemical industry synthesis of pilot scale is anti-
Should.
The purpose of the present invention is achieved through the following technical solutions：
Try out double kettle intermittent reaction devices in one kind, including raw material system, reaction system, piece-rate system, finished product system and
Public engineer system,
The raw material system is by two sets of Lower tanks, raw material pump, head tank, auxiliary material tank and static mixer, raw material preheating
Device is formed, and two sets of Lower tanks, raw material pump, head tank, auxiliary material tank are in be arranged in parallel；
The reaction system is made up of the batch reactor and corresponding heat exchanger, circulating pump of two, one of reaction
For kettle to neutralize kettle, another is distillation still, two reactors or used in parallel to expand respond, or is used in series carry out two
Step reaction；
The piece-rate system is by destilling tower, centrifugal mechanism into the distillation in distillation still and piece-rate system in reaction system
Tower connects, for caused light component in separation reaction or the solvent used in recovery course of reaction；Centrifuge respectively with
Circulating pump corresponding to two reactors in reaction system is connected, for separating the solid phase components in any reactor；
The finished product system is made up of mother liquor tank, finished pot, light phase tank, centrifuge in mother liquor tank and piece-rate system, anti-
Answer the circulating pump in system to be connected, for collecting the mother liquor isolated, and mother liquor is got to by circulating pump by reaction system
In recycled, finished pot is connected with two reactors in reaction system respectively, for collecting the finished product reflected；Gently
Phase tank is connected with the destilling tower in piece-rate system, for collecting light component finished product；
The public engineer system is made up of circulating cooling water unit, steam heating unit, heat-conducting oil heating unit, mainly
According to the maintenance of process requirements and the temperature of control whole device, wherein circulating cooling water unit and the reaction in reaction system
Destilling tower is connected in kettle, heat exchanger and piece-rate system；Steam heating unit and reactor, heat exchanger and the raw material in reaction system
Feed preheater is connected in system；Heat-conducting oil heating unit is connected with the reactor in reaction system.
In the present invention, the ratio of height to diameter of the reactor in the reaction system is 1: 1, and the ratio of height to diameter of distillation still is 1.2: 1,
To adapt to different reaction systems.
The centrifuge is link-suspended basket centrifuge, realizes separation of solid and liquid, and can be carried out by changing the filter cloth of different meshes
The separation of different grain size reaction solution.
The circulating cooling water unit is made up of cooling water storage tank and cooling water circulating pump.
The heat-conducting oil heating cycling element is by hotline heater, conduction oil emergency storage tank（Its effect is to prevent conduction oil
Accident caused by expansion）And heat conduction oil circulating pump composition.
The steam heating unit is made up of steamdrum, steam generator and water softener.
The general agitating shaft with logical key is equipped with two reactors, can be changed thereon according to process requirements different
The agitating paddle of type.
This pair of kettle intermittent reaction device is applied to oxidized starch reaction system.
More specific description of the present invention is as follows：
Raw material system is mixed by two raw material pumps, two Lower tanks, two head tanks and two auxiliary material tank preheaters and static state
Clutch forms.It is common with auxiliary material tank A and B that raw material by Lower tank A and B is input to head tank A and head tank B by raw material pump A and B
It is mixed into static mixer to be sufficiently mixed and is preheated in inflow feed preheater.
Reaction system be by neutralization kettle, distillation still, neutralize kettle heat exchanger, distillation still heat exchanger and outer circulation pump group into.Instead
Answer process：Material is reacted by feed preheater into reactor, is exchanged heat subsequently into heat exchanger, and product enters separation and filled
Put.
Piece-rate system is made up of centrifuge, destilling tower, overhead condenser, intermediate storage tank, condensate liquid booster pump.Via raw material
The material that system conveying comes enters centrifuge to realize separation of solid and liquid；Material enters distillation by centrifuge, neutralization kettle and distillation still
Tower realizes gas-liquid separation, and the gas that destilling tower comes out is transported to intermediate storage tank into overhead condenser, passes through condensate liquid booster pump
Flowed back and quantitatively produced.
Product systems are made up of mother liquor tank, finished pot, tower top finished pot.Material is stored standby by centrifuge into mother liquor tank
With the material of masterbatch tank enters back into destilling tower；Material through overhead condenser stores from intermediate storage tank into tower top finished pot.
Public engineer system is made up of cooling water circulation unit, heat-conducting oil heating unit, steam heating unit.Cooling water follows
Ring element is made up of cooling water storage tank, cooling water circulating pump, and cooling water is flowed back from cooling water storage tank through cooling water circulating pump；
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 by 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 formed.Running water flows through water softener and flows into steam generator, and steam is assigned to reaction system and raw material after being transported to steamdrum
System.
The present invention has following functions and feature:Package unit is divided into raw material area, reaction zone, separation using industrialization layout
Area, product zone and public engineering area.It can be carried out with two raw material Lower tanks and two head tanks and two storage tanks pre-
It is 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 sets of independent batch reactors can carry out use in series or in parallel, two intervals
Agitating paddle in reactor can change the current version agitators such as anchor formula, frame, six straight leaf disc formulas on demand；Used in course of reaction
With oxidized starch etc. for reaction system, safety operation can be carried out in the environment of not possessing ventilation condition；Tester in simultaneously
Material heating in middle heat-conducting oil heating system and applicable 0~300 DEG C of temperature range of steam-heating system, complete cooling follow
Loop system can realize being carried out continuously for intermittent reaction.
Brief description of the drawings
Fig. 1 is the main material flow figure of double kettle intermittent reactions；
Fig. 2 is double kettle intermittent reaction device recirculating cooling water system figures；
Fig. 3 is double kettle intermittent reaction device heat-conducting oil heating system figures；
Fig. 4 is double kettle intermittent reaction device steam-heating system figures；
Fig. 5 is double kettle intermittent reaction device technique flow total figures；
In Fig. 1-5：1-head tank A, 2-auxiliary material tank A, 3-auxiliary material tank B, 4-head tank B, 5-static mixer, 6-
Feed preheater, 7-raw material pump A, 8-Lower tank A, 9-raw material pump B, 10-Lower tank B, 11-centrifugal pump, 12-neutralize
Kettle, 13-centrifuge, 14-neutralization kettle heat exchanger, 15-outer circulation pump A, 16-distillation still, 17-distillation still heat exchanger, 18-
Outer circulation pump B, 19-destilling tower, 20-overhead condenser, 21-intermediate storage tank, 22-condensate liquid booster pump, 23-mother liquor tank,
24-finished pot, 25-tower top finished pot（That is light phase tank）, 26-cooling water storage tank, 27-cooling water circulating pump A, 28-cooling
Water-circulating pump B, 29-conduction oil emergency storage tank, 30-hotline heater, 31-heat conduction oil circulating pump, 32-steamdrum, 33-
Steam generator, 34-water softener.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing：
As Figure 1-5：Double kettle intermittent reaction devices, including raw material system, reaction system, segregative line are tried out in one kind
System, finished product system and public engineer system,
The raw material system is by two sets of Lower tanks, raw material pump, head tank, auxiliary material tank and static mixer, raw material preheating
Device is formed, two sets of Lower tanks（8、10）, raw material pump（7、9）, head tank（1、4）, auxiliary material tank（2、3）In being arranged in parallel；
The reaction system is made up of the batch reactor of two and corresponding two heat exchangers 14,17, two circulating pumps,
One of reactor is neutralizes kettle 12, and another is distillation still 16, two reactors or used in parallel to expand respond,
Or it is used in series carry out two-step reaction；
The piece-rate system is by destilling tower 19, separator（That is centrifuge 13）Form, the distillation still 16 in reaction system with
Destilling tower 19 in piece-rate system connects, for separating caused light component in reaction or reclaiming used in course of reaction
Solvent；Separator is connected with two reactors in reaction system, two circulating pumps, for separating the solid phase in reaction system
Component；
The finished product system is made up of mother liquor tank 23, finished pot 24, light phase tank 25, in mother liquor tank 23 and piece-rate system from
Circulating pump in scheming 13, reaction system is connected, and for collecting the mother liquor isolated, and mother liquor is got to by circulating pump
Recycled in reaction system, finished pot 24 is connected with two reactors in reaction system, for collecting what is reflected
Finished product；Light phase tank 25 is connected with the destilling tower 19 in piece-rate system, for collecting light component finished product；
The public engineer system is made up of circulating cooling water unit, steam heating unit, heat-conducting oil heating unit, mainly
According to the maintenance of process requirements and the temperature of control whole device, wherein circulating cooling water unit and the reaction in reaction system
Destilling tower is connected in kettle, heat exchanger and piece-rate system；Steam heating unit and reactor, heat exchanger and the raw material in reaction system
Feed preheater is connected in system；Heat-conducting oil heating unit is connected with the reactor in reaction system.
The present invention from feed, react, be separated to the generating process of finished product and material flow be described with reference to the drawings it is as follows：
As shown in Figure 1：This flow is universal interval class reaction system, and two kinds of principal goods material for participating in reaction are respectively added to
Lower tank A8, Lower tank B10, the auxiliary material for participating in reaction are added to auxiliary material tank A2, auxiliary material tank B3, appointing in principal goods material, auxiliary material
Two or more material of anticipating flows through static mixer 5 and sufficiently mixed, and flows through feed preheater 6（If it is not required to
Preheat, can directly open bypass）, flow through and neutralize kettle 12, maintain certain pressure, temperature, time, after reaction to expect in and in kettle
Liquid passes through outer circulation pump A15, distillation still 16 is entered after neutralizing kettle heat exchanger 14, in distillation still 16（It can supplement new
Raw material or auxiliary material）Certain pressure, temperature, time are maintained, feed liquid passes through outer circulation pump B18 after reaction, by distillation still heat exchanger
Enter finished pot 24 after 17.According to technique needs, the obvious reaction system of corresponding heat release or heat absorption, neutralize during the course of the reaction
In kettle/distillation still reaction solution respectively can pass through outer circulation pump, neutralize kettle distillation still ring heat exchanger return to neutralization kettle/distillation still,
Reach the purpose of kettle external circulation heat exchanging.
If producing solid matter in and in kettle or distillation still, directly feed liquid is squeezed into after outer circulating pump A B
Centrifuge 13, solid is stayed in the rotary drum of centrifuge, and liquid enters mother liquor tank 23, mother liquor tank after being pressurized as mother liquor centrifugal pump 11
Middle mother liquor according to technique need to enter outer circulation pump A before B, can reach and neutralize kettle 12 or distillation still 16 is circulated.
If producing gas-phase product in distillation still reaction system or needing recycling design, distillation still 16 is heated to accordingly
Temperature, gaseous substance enter the bottom of destilling tower 19, are flowed into overhead condenser 20 in tower top after the heat transfer of tower inner transmission matter, pass through
It is changed into condensate liquid after condensation and enters intermediate storage tank 21, the liquid of intermediate storage tank 21 is divided to two after the supercharging of subcooling condensate booster pump 22
Road, wherein returning to the stable operation that the top of destilling tower 19 maintains destilling tower all the way, it is directly entered tower top finished pot 25 all the way in addition.
The circulating cooling water unit of the present invention is described with reference to the drawings as follows：
As shown in Figure 2：Cool down the basis after cooling water circulating pump A27 B28 superchargings of the recirculated cooling water in water storage tank 26
Process requirements are sent in the cooling coil neutralized in kettle 12, distillation still 16 or entered respectively neutralizes kettle heat exchanger 14, distillation
Kettle heat exchanger 17, overhead condenser 20 are cooled down, and then return to cooling water storage tank 26 by return main road.
The heat-conducting oil heating unit of the present invention is described with reference to the drawings as follows：
As shown in Figure 3：Conduction oil enters in hotline heater 30 by conduction oil emergency storage tank 29 and is heated to a constant temperature
Degree, it is sent to respectively according to process requirements after conduction oil mixing pump 31 in the conduction oil coil pipe neutralized in kettle 12, distillation still 16
Exchanged heat, hotline heater 30 is then returned to by heat conduction oil return line.
The steam-heating system of the present invention is described with reference to the drawings as follows：
As shown in Figure 4：Water enters steam generator 33 after being exchanged by ion exchange column, and steam is divided into by steamdrum 32
Three tunnels：Wherein exchanged heat as needed into neutralization kettle heat exchanger 14, distillation still heat exchanger 17 all the way, steam is condensed into liquid
After flow directly into trench；Wherein need to enter in the chuck in neutralization kettle 12, distillation still 16 according to technique all the way, after condensation
Into inflow 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, be further equipped with each critical piece it is following metering,
The functional accessories such as monitoring, display, control：
Raw material area Lower tank 8,10 and head tank 1,4, which are equipped with liquid level gauge, can observe the change of raw material liquid level at any time, in a high position
Material flow is accurately measured provided with spinner flowmeter between groove 1,4 and Lower tank 8,10.Pass through head tank 1,4, auxiliary material tank
2nd, 3 and static mixer 5 raw material is premixed, then feed preheater 6 can preheat to the raw material after premix.
The equipment for separating liquid from solid of Disengagement zone, filtrate can be reclaimed provided with filtrate tanks based on centrifuge 13.Pass through
To centrifuge 13 change the filter cloth of different meshes to realize the separation of different grain size reaction solution.The separation of liquid phase passes through steaming
Evaporate tower 19 to realize, liquid level gauge is provided with destilling tower 19 and carries out liquid level monitoring.Distillate component carried out by overhead condenser 20 it is cold
Lime set is recycled to intermediate storage tank 21, and condensate liquid booster pump 22 is provided with intermediate storage tank 21.Material flows to through intermediate storage tank 21
Spinner flowmeter is respectively equipped between destilling tower 19 and tower top finished pot 25 and pipeline, quantitative backflow can be carried out to condensate liquid or is adopted
Go out.
Course of reaction can by neutralizing kettle 12, distillation still 16 is realized, and two kettles can be carried out according to different requirements series connection and
It is used in parallel.Temperature sensor is respectively equipped with two kettles to carry out Automated condtrol to liquid level in reactor.Also set on two kettles
There is pressure gauge to show that internal pressure and thermometer carry out temperature test.Two kettles, which are designed with two jacket heating systems, can realize conduction oil
And steam heating, suitable for the temperature range of differential responses.Exchanged heat after two kettles provided with heat exchanger 14,17, heat exchanger 14,
17 inlet and outlet are designed with temperature indicator, temperature change before and after measurement heat exchange.
Hotline heater 30 in heating system is provided with limit switch, and automation control is carried out to oil temperature in heater
System.Temperature indicating device is designed with the conveying of conduction oil and reflux course.Emergency storage tank 29 is provided with hotline heater,
Liquid level low-level alarm is provided with emergency storage tank.Steam generator 33 in steam heating is provided with rotating speed control table, to liquid level
Automated condtrol is carried out, prevents that liquid level is too high or too low.Temperature sensor automatically controls to temperature.In steam generator 33
It is preceding to be provided with water softener, sofening treatment is carried out to running water, it is rear that stable vapours is provided provided with steamdrum 32.Set on steamdrum
There are pressure gauge and drain valve, the condensate liquid 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, pressure gauge, the using and the reserved is provided with after pump, while enter using turbine flowmeter
The dosage of row batching cycle water.
Claims (6)
1. double kettle intermittent reaction devices are tried out in one kind, it is characterised in that：Including raw material system, reaction system, piece-rate system, into
Strain is united and public engineer system,
The raw material system is by two sets of Lower tanks, raw material pump, head tank, auxiliary material tank and static mixer, feed preheater structure
Into two sets of Lower tanks, raw material pump, head tank, auxiliary material tank are in be arranged in parallel；
The reaction system is made up of two batch reactors and corresponding heat exchanger, circulating pump, during one of reactor is
And kettle, another is distillation still, and two reactors are in be used in series carry out two-step reaction；
The piece-rate system is by destilling tower, centrifugal mechanism into the destilling tower in the distillation still and piece-rate system in reaction system connects
Connect, for caused light component in separation reaction or the solvent used in recovery course of reaction；Centrifuge respectively with reaction
Circulating pump corresponding to two reactors is connected in system, for separating the solid phase components in any reactor；
The 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 for collecting the mother liquor isolated, and mother liquor is got in reaction system by circulating pump
Row recycles, and finished pot is connected with two reactors in reaction system respectively, for collecting the finished product reflected；Light phase tank
It is connected with the destilling tower in piece-rate system, for collecting light component finished product；
The public engineer system is made up of circulating cooling water unit, steam heating unit, heat-conducting oil heating unit, main basis
The maintenances of process requirements and the temperature for controlling whole device, wherein circulating cooling water unit and the reactor in reaction system, change
Destilling tower is connected in hot device and piece-rate system；Steam heating unit and reactor, heat exchanger and the raw material system in reaction system
Middle feed preheater is connected；Heat-conducting oil heating unit is connected with the reactor in reaction system.
2. double kettle intermittent reaction devices are tried out according to claim 1, it is characterised in that：It is anti-in the reaction system
The ratio of height to diameter for answering kettle is 1: 1, and the ratio of height to diameter of distillation still is 1.2: 1, to adapt to different reaction systems.
3. double kettle intermittent reaction devices are tried out according to claim 1, it is characterised in that：The circulating cooling water unit
It is made up of cooling water storage tank and cooling water circulating pump.
4. double kettle intermittent reaction devices are tried out according to claim 1, it is characterised in that：The heat-conducting oil heating unit
It is made up of hotline heater, conduction oil emergency storage tank and heat conduction oil circulating pump.
5. double kettle intermittent reaction devices are tried out according to claim 1, it is characterised in that：The steam heating unit by
Steamdrum, steam generator and water softener composition.
6. double kettle intermittent reaction devices are tried out according to claim 1, it is characterised in that：Match somebody with somebody in two reactors
The standby general agitating shaft with logical key, changes different types of agitating paddle according to process requirements thereon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610449970.9A CN106000251B (en) | 2016-06-21 | 2016-06-21 | Double kettle intermittent reaction devices are tried out in one kind |
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| CN201610449970.9A CN106000251B (en) | 2016-06-21 | 2016-06-21 | Double kettle intermittent reaction devices are tried out in one kind |
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| CN106000251B true CN106000251B (en) | 2017-11-28 |
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| US4968834A (en) * | 1990-05-07 | 1990-11-06 | Hoechst Celanese Corporation | Recovery of acrylic acid and/or ethyl acrylate from black acid |
| WO2013078391A1 (en) * | 2011-11-23 | 2013-05-30 | Segetis, Inc. | Process to prepare levulinic acid |
| CN203820667U (en) * | 2014-04-29 | 2014-09-10 | 浙江阿尔法化工科技有限公司 | Production system of tetrahydrophthalic anhydride |
| CN104803955B (en) * | 2015-04-24 | 2016-09-14 | 安徽华业香料股份有限公司 | The normal pressure process units of methyl decalactone synthetic perfume and production method |
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Inventor after: Zhao Yang Inventor after: Zhen Chaoying Inventor after: Zhu Mingyue Inventor after: Huang Shuangcheng Inventor after: Teng Wenrui Inventor after: Zhao Yuqi Inventor after: Yue Ruifeng Inventor after: He Sujiao Inventor after: Fu Yong Inventor after: Cai Zhuanghong Inventor before: Zhao Yang Inventor before: Zhen Chaoying Inventor before: Zhu Mingyue Inventor before: Huang Shuangcheng Inventor before: Teng Wenrui Inventor before: Zhao Yuqi Inventor before: Yue Ruifeng Inventor before: He Sujiao Inventor before: Fu Yong Inventor before: Cai Zhuanghong |
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Granted publication date: 20171128 Termination date: 20190621 |