CN104436731B - A kind of automatic division box of ethyl acetate backflow reaction - Google Patents
A kind of automatic division box of ethyl acetate backflow reaction Download PDFInfo
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- CN104436731B CN104436731B CN201410692011.0A CN201410692011A CN104436731B CN 104436731 B CN104436731 B CN 104436731B CN 201410692011 A CN201410692011 A CN 201410692011A CN 104436731 B CN104436731 B CN 104436731B
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Abstract
The present invention relates to a kind of automatic division box of ethyl acetate backflow reaction, comprise distillation still, condenser, water knockout drum and point water receiving tank; It also comprises conductivity meter and air-operated solenoid valve, and air-operated solenoid valve is connected on the distributive pipe road between water knockout drum and point water receiving tank, and the probe of conductivity meter is positioned at water knockout drum, and conductivity meter and air-operated solenoid valve are interlocked by DCS control system; When the conductivity values that conductivity meter is measured is greater than after setting value S, DCS system program carries out timing, when arrival set after the time, and conductivity values is greater than setting value S, air-powered electromagnetic unlatching all the time, moisture goes out, in the time that conductivity values is less than setting value S, air-operated solenoid valve is closed, and program recovery is to initial state, with this cycling, until point not water outlet in water knockout drum. Device in the present invention divides water by the water in reactant liquor automatically by conductivity meter, air-operated solenoid valve and DCS control system, thereby alleviates personnel labor intensity and maloperation.
Description
Technical field
The present invention relates to a kind of division box automatically, be specifically related to a kind of taking back flow reaction as main, by reactant liquorIn water by conductivity meter and DCS automatic control system, automatically divide the ethyl acetate backflow of water to reactAutomatic division box.
Background technology
In chemical products are produced, there is the technique of many generation water to relate to back flow reaction, by solvent and waterAzeotropic form and reflux, then layering in water knockout drum, then relies on and manually divide water, but general backflowThe time of reaction is long, and therefore dividing water is a veryer long and meticulous operation, is easy to occur solventMistake point or water divides and put in place and get back in distillation still, in the increase reaction time, waste resource.
Summary of the invention
For the problems referred to above, it is a kind of taking back flow reaction as main that main purpose of the present invention is to provide, and will reactWater in liquid, by conductivity meter and DCS automatic control system, divides the ethyl acetate backflow of water anti-automaticallyThe automatic division box of answering.
The present invention solves above-mentioned technical problem by following technical proposals:
An automatic division box for ethyl acetate backflow reaction, described automatic division box comprise distillation still,Condenser, water knockout drum and point water receiving tank; Wherein distillation still is connected with condenser by gas phase pipe, condenserAnd between water knockout drum, be connected by input duct, between water knockout drum and point water receiving tank, connect by distributive pipe road;It is characterized in that, also comprise a conductivity meter and an air-operated solenoid valve, described in described air-operated solenoid valve is connected onOn distributive pipe road between water knockout drum and point water receiving tank, the probe of described conductivity meter is positioned at described water knockout drumIn, described conductivity meter and air-operated solenoid valve are interlocked by DCS control system; When the electricity of conductivity meter mensurationConductance numerical value is greater than after setting value S, and DCS system program carries out timing, when arrival set after the time, and electricityConductance numerical value is greater than setting value S all the time, and air-powered electromagnetic is opened, and moisture goes out, and treats that conductivity values is less than setting valueWhen S, air-operated solenoid valve is closed, and program recovery is to initial state, with this cycling, until divide in water knockout drumTill not water outlet; Each point water yield ⊿ T is exactly the water amount ⊿ M that described distillation still is taken out of.
In a preferred embodiment of the invention, described point of water receiving tank disposes weighing device, described titleDCS system and described conductivity meter and air-operated solenoid valve interlocking described in same work are put in refitting, when dividing in water receiving tankWater weight be greater than theoretically while generating the water yield, described air-operated solenoid valve is in closed condition.
In a preferred embodiment of the invention, in described water knockout drum, be provided with water fender and at water knockout drumOn dispose overfall, described overfall is by overflow pipe and be serially connected in the backflow on described overflow pipeValve is connected with described distillation still; The probe of described overfall and described conductivity meter divides and is located at described water fenderBoth sides.
In a preferred embodiment of the invention, the probe of described conductivity meter is installed the end higher than water knockout drumMore than the 50mm of portion.
In a preferred embodiment of the invention, dispose bleeder in the bottom of described water knockout drum, described inBleeder is connected with described point of water receiving tank by distributive pipe road; The spy of described bleeder and described conductivity meterHead is positioned at the same side of described water fender.
In a preferred embodiment of the invention, dispose inlet and Fen Shui at the top of described water knockout drumDevice drain, described inlet is connected with condenser by described input duct, at described water knockout drum drainOn dispose balance blow-down pipe; Described inlet and water knockout drum drain divide be located at described water fender both sides alsoAnd the probe of described water knockout drum drain and described conductivity meter is positioned at the same side of described water fender.
In a preferred embodiment of the invention, described distillation still is that volume is the stainless steel of 2500-3500LReactor; Described condenser is that surface area is 15-25M2Stainless steel condenser; Described water knockout drum is that volume isThe glass trap of 40-60L; The described point of rustless steel container that water dump tank is 150-250L.
In a preferred embodiment of the invention, described conductivity meter adopts screw thread to be arranged on water knockout drum bottom.
Positive progressive effect of the present invention is: the device in the present invention is taking back flow reaction as main, by reactant liquorIn water by conductivity meter, air-operated solenoid valve and DCS control system, automatically divide water, therebyAlleviate personnel labor intensity and maloperation.
Brief description of the drawings
Fig. 1 is overall structure schematic diagram of the present invention.
Detailed description of the invention
Provide preferred embodiment of the present invention below in conjunction with accompanying drawing, to describe technical scheme of the present invention in detail.
Fig. 1 is overall structure schematic diagram of the present invention, as Fig. 1 shows: ethyl acetate backflow provided by the inventionThe automatic division box of reaction, comprises distillation still 1, condenser 2, water knockout drum 3 and point water receiving tank 4.
Steam is installed in distillation still 1 and enters pipeline 101, cooling water outlet pipe road 102, cooling water inlet pipeRoad 103, steam exhaust pipe 104, still internal pressure table 105, pressure transmitter 106, temperature transmitter 107,Temperature of charge meter 108, refuse discharge line 109 and raw material inlet 110.
Steam enters pipeline 101, cooling water outlet pipe road 102, cooling water inlet pipe road 103 and steam exhaust-gasPipe 104 is for reacting front cleaning distillation still 1.
Raw material inlet 110 is inlet ports of distillation still 1 interior raw material, and raw material is in the present invention moistureEthyl acetate mother liquor.
Still internal pressure table 105 measures the pressure of distillation still 1 interior water, will be surveyed by pressure transmitter 106The data transaction measuring becomes the signal of telecommunication to output to DCS control system.
Temperature of charge meter 108 measures the temperature of distillation still 1 interior water, will be surveyed by temperature transmitter 107The data transaction measuring becomes the signal of telecommunication to output to DCS control system.
On condenser 2, have material steam import 201, cooling water inlet 202, cooling water inlet 203, coldSolidifying water out 204 and condenser drain 205, material steam import 201 connects by gas phase pipe 5 and distillation stillConnect, top temperature thermometer 501 and temperature transmitter 502 are installed on gas phase pipe 5; Thermometer is temperature surveyUtensil, temperature transmitter is to become the signal of telecommunication to output to DCS control system the data transaction measuring. ColdOn condenser drain 205, dispose balance blow-down pipe 7.
Water knockout drum 3 bottoms have bleeder 301, and top disposes inlet 302 and water knockout drum drain 303,The sidepiece of water knockout drum 3 disposes overfall 304, and inlet 302 is cold by input duct 6 and condenser 2Solidifying water out 204 connects, and disposes balance blow-down pipe 8 on water knockout drum drain 303. Overfall 304 passes throughOne overflow pipe 12 and return valve 13 are connected with distillation still 1, bleeder 301 by distributive pipe road 11 withDivide water receiving tank 4 to connect.
Have a liquid barrier 305 in the internal configurations of water knockout drum 3, conductivity meter 306 adopts screw thread to be arranged on a point waterDevice 3 bottoms, the probe of conductivity meter 306 stretches into the inside of water knockout drum 3 and installation site higher than water knockout drum 3Bottom 50mm more than.
The bleeder 301 of water knockout drum 3 bottoms, the probe of conductivity meter 306 and water knockout drum drain 303 are positioned atOne side of water fender 305, inlet 302 and overfall 304 are positioned at an other side of water fender 305.
On distributive pipe road 11, be connected in series an air-operated solenoid valve 10, air-operated solenoid valve 10 and conductivity meter 306 are logicalCross a DCS control system interlocking.
DCS control system is the abbreviation of scattered control system (DistributedControlSystem),It is that a multi-level computer taking communication network as tie being made up of process control level and process monitoring level isSystem, combines the 4C technology such as computer, communication, demonstration and control, and its basic thought is decentralised control, collectionMiddle operation, differentiated control, flexible configuration, configuration are conveniently.
Point water receiving tank 4 be also connected with control electronic module transmitter 401, weighing device 402, remove waste waterPipeline 403 and point water receiving tank drain 404, weighing device 402 is weight measurement utensils, in native systemEffect be exactly that the weight of the water in point water receiving tank 4 is measured, electronic module transmitter 401 be byThe data transaction that weighing device 402 measures becomes the signal of telecommunication to output to DCS control system. Divide water receiving tank 4Bottom waste pipe 403 is installed. Divide water receiving tank drain 404 to be connected with balance blow-down pipe 9.
Balance blow-down pipe 7,8,9 is PA tube, and remaining all pipeline is the pipeline of stainless steel,All connected modes are steel flange and connect.
The stainless steel cauldron that distillation still 1 is 2500-3500L for volume. Condenser 2 for surface area is15-25M2Stainless steel condenser. The glass trap that water knockout drum 3 is 40-60L for volume. Divide water dump tank4 is the rustless steel container with Weighing module of 150-250L.
Be the automatic dividing method for water of a concrete ethyl acetate backflow reaction below, comprise:
(1), toward the moisture ethyl acetate mother liquor that adds needs distillation in distillation still 1, open cold condenser 2Cooling water valve, opens the valve on gas phase pipe 5 between distillation still 1 and condenser 2, continues distillation still 1Heat up, the interior temperature of still 1 to be distilled is elevated to after the azeotropic point of ethyl acetate and water, ethyl acetate and waterJointly steam, arrive condenser 2 carry out condensation by gas phase pipe 5, the condensed condensate liquid of condenser 2 is logicalCross input duct 6 and enter into water knockout drum 3 and carry out layering after interior, treat that the interior liquid level of water knockout drum 3 is higher than overfall 304Time, open return valve 13 and start point water program automatically in DCS control system, divide water, divide at every turnChu Shui Liang ⊿ T is exactly the Shui Liang ⊿ M that interior distillation still 1 is taken out of;
(2) conductivity meter 306, in water knockout drum 3 is interlocked with air-operated solenoid valve 10, and initial state is for when electricityThe conductivity values that electrical conductivity instrument 306 is measured is greater than after setting value S, and DCS system program carries out timing, works as arrivalSet after the time, and conductivity values be greater than all the time setting value S, operated pneumatic valve open, moisture goes out, and treats electricityWhen conductance numerical value is less than setting value S, operated pneumatic valve is closed, and program recovery is to initial state, with this behaviour of circulatingDo, until point not water outlet in reactor. (for preventing accident, when dividing, the water weight in water receiving tank 4 is largeIn the time that theory generates water yield M, point water stop, air-operated solenoid valve 10 is closed).
More than show and described general principle of the present invention and principal character and advantage of the present invention. The industryTechnical staff should understand, the present invention is not restricted to the described embodiments, in above-described embodiment and descriptionThat describes just illustrates principle of the present invention, without departing from the spirit and scope of the present invention, and the present inventionAlso have various changes and modifications, these changes and improvements all fall in the claimed scope of the invention, thisInventing claimed scope is defined by appending claims and equivalent thereof.
Claims (8)
1. an automatic division box for ethyl acetate backflow reaction, described automatic division box comprises distillationStill, condenser, water knockout drum and point water receiving tank; Wherein distillation still is connected with condenser by gas phase pipe,Between condenser and water knockout drum, be connected by input duct, between water knockout drum and point water receiving tank, pass through a point waterPipeline connects; On described gas phase pipe, temperature transmitter is installed, described temperature transmitter is to measureTo data transaction become the signal of telecommunication to output to DCS control system; It is characterized in that, also comprise an electrical conductivityInstrument and an air-operated solenoid valve, described air-operated solenoid valve is connected between described water knockout drum and point water receiving tankOn distributive pipe road, the probe of described conductivity meter is positioned at described water knockout drum, described conductivity meter and pneumaticMagnetic valve is interlocked by DCS control system; When the conductivity values that conductivity meter is measured is greater than after setting value S,DCS control system program is carried out timing, and when arrival set after the time, and conductivity values is greater than and establishes all the timeDefinite value S, air-operated solenoid valve is opened, and moisture goes out, in the time that conductivity values is less than setting value S, air-powered electromagneticValve cuts out, and program recovery is to initial state, with this cycling, until point not water outlet in water knockout drum;Each point water yield ⊿ T is exactly the water amount ⊿ M that described distillation still is taken out of.
2. the automatic division box of a kind of ethyl acetate backflow reaction as claimed in claim 1, its featureBe, described point of water receiving tank disposes weighing device, and described weighing device is by described DCS control systemWith described conductivity meter and air-operated solenoid valve interlocking, when the water weight in point water receiving tank is greater than theoretical generationWhen the water yield, described air-operated solenoid valve is in closed condition.
3. the automatic division box of a kind of ethyl acetate backflow reaction as claimed in claim 1, its feature existsIn, in described water knockout drum, be provided with water fender and on water knockout drum, dispose overfall, described overfallBe connected with described distillation still by overflow pipe and the return valve that is serially connected on described overflow pipe; InstituteThe probe of stating overfall and described conductivity meter divides the both sides that are located at described water fender.
4. the automatic division box of a kind of ethyl acetate backflow reaction as claimed in claim 3, its feature existsIn, more than the probe of described conductivity meter is installed the bottom 50mm higher than water knockout drum.
5. the automatic division box of a kind of ethyl acetate backflow reaction as claimed in claim 3, its feature existsIn, disposing bleeder in the bottom of described water knockout drum, described bleeder is by distributive pipe road and described pointWater receiving tank connects; The probe of described bleeder and described conductivity meter is positioned at the same side of described water fender.
6. the automatic division box of a kind of ethyl acetate backflow reaction as claimed in claim 5, its featureBe, dispose inlet and water knockout drum drain at the top of described water knockout drum, described inlet passes throughDescribed input duct is connected with condenser, on described water knockout drum drain, disposes balance blow-down pipe; InstituteState inlet and water knockout drum drain divide be located at the both sides of described water fender and described water knockout drum drain withThe probe of described conductivity meter is positioned at the same side of described water fender.
7. the automatic division box of a kind of ethyl acetate backflow reaction as claimed in claim 1, its featureBe, described distillation still is that volume is the stainless steel cauldron of 2500-3500L; Described condenser is surfaceAmass the stainless steel condenser for 15-25M2; Described water knockout drum is that volume is the glass trap of 40-60L;The described point of rustless steel container that water dump tank is 150-250L.
8. the automatic division box of a kind of ethyl acetate backflow reaction as claimed in claim 1, its featureBe, described conductivity meter adopts screw thread to be arranged on water knockout drum bottom.
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| CN201410692011.0A CN104436731B (en) | 2014-11-25 | 2014-11-25 | A kind of automatic division box of ethyl acetate backflow reaction |
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| CN201410692011.0A CN104436731B (en) | 2014-11-25 | 2014-11-25 | A kind of automatic division box of ethyl acetate backflow reaction |
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| CN114671786A (en) * | 2022-03-23 | 2022-06-28 | 浙江友联化学工业有限公司 | 2B acid high-yield production process and equipment |
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| JPS6291203A (en) * | 1985-06-22 | 1987-04-25 | Mitsui Petrochem Ind Ltd | Purification of water-soluble liquid |
| KR101666920B1 (en) * | 2009-02-06 | 2016-10-17 | 잇판자이단호진 조스이 소꾸신센타 | Operation management device for a vaporization device, fresh water generator provided with the operation management device, and operation management method and fresh water-generating method for vaporization devices |
| CN101890248B (en) * | 2010-07-09 | 2013-01-16 | 神华集团有限责任公司 | Distillation system and method for separating liquid product |
| CN202682819U (en) * | 2012-07-11 | 2013-01-23 | 宿迁科思化学有限公司 | Rectifying tower device with water distributor |
| CN203389358U (en) * | 2013-07-02 | 2014-01-15 | 浙江万邦药业股份有限公司 | Distillation reflux secondary water distribution device |
| CN203609901U (en) * | 2013-11-28 | 2014-05-28 | 山东方明药业集团股份有限公司 | Distilling dehydration device |
| CN204352576U (en) * | 2014-11-25 | 2015-05-27 | 上海试四化学品有限公司 | A kind of automatic division box of ethyl acetate backflow reaction |
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Address after: 200940 Baoshan District Taihe Road, Shanghai, No. 1004 Applicant after: Shanghai Shishi Hewei Chemical Industry Co., Ltd. Applicant after: SHANGHAI SHISI CHEMICAL PRODUCT CO., LTD. Address before: 201512 Shanghai City, Jinshan District Jinshan Zhen Hua Road No. 200 Applicant before: SHANGHAI SHISI CHEMICAL PRODUCT CO., LTD. Applicant before: Shanghai Shishi Hewei Chemical Industry Co., Ltd. |
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