CN107930565A - A kind of reaction kettle prepared for ethyltriphenylphosphonium bromide - Google Patents
A kind of reaction kettle prepared for ethyltriphenylphosphonium bromide Download PDFInfo
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- CN107930565A CN107930565A CN201711445952.4A CN201711445952A CN107930565A CN 107930565 A CN107930565 A CN 107930565A CN 201711445952 A CN201711445952 A CN 201711445952A CN 107930565 A CN107930565 A CN 107930565A
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- reaction kettle
- valve
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- steam
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 101
- JHYNXXDQQHTCHJ-UHFFFAOYSA-M ethyl(triphenyl)phosphanium;bromide Chemical compound [Br-].C=1C=CC=CC=1[P+](C=1C=CC=CC=1)(CC)C1=CC=CC=C1 JHYNXXDQQHTCHJ-UHFFFAOYSA-M 0.000 title claims abstract description 29
- 239000000498 cooling water Substances 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 238000011084 recovery Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 27
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 9
- 230000008676 import Effects 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 5
- RDHPKYGYEGBMSE-UHFFFAOYSA-N bromoethane Chemical compound CCBr RDHPKYGYEGBMSE-UHFFFAOYSA-N 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000012423 maintenance Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 6
- 238000004064 recycling Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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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
-
- 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
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- 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
- B01J19/0053—Details of the reactor
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/54—Quaternary phosphonium compounds
- C07F9/5456—Arylalkanephosphonium compounds
-
- 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
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00054—Controlling or regulating the heat exchange system
- B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
- B01J2219/00058—Temperature measurement
- B01J2219/00063—Temperature measurement of the reactants
-
- 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
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00094—Jackets
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a kind of reaction kettle prepared for ethyltriphenylphosphonium bromide, including reaction kettle housing, double-jacket, agitating shaft and motor, reaction kettle housing upper end is equipped with manhole and temperature measuring equipment, and lower end is equipped with discharge port, and reaction kettle housing lower end periphery is cased with double-jacket；Double-jacket is the double jacket being sequentially overlapped, and is equipped with two passages in it, is respectively first passage and second channel；First passage is arranged between reaction kettle housing and second channel, and first passage upper end is equipped with steam inlet, exhaust outlet and cooling water outlet, and lower end is equipped with steam (vapor) outlet and cooling water inlet, and steam (vapor) outlet is connected with condenser；Second channel lower end is equipped with cooling water inlet, and upper end is equipped with corresponding hot water outlet.The advantage of the invention is that：(1) without being modified to reaction kettle enclosure interior, not only facilitated and made, but also be beneficial to later period maintenance；(2) by the improvement to reacting kettle jacketing, it is made to integrate reaction kettle heating, heat recovery and cooling function.
Description
Technical field
The present invention relates to technical field of chemical, more particularly to a kind of reaction prepared for ethyltriphenylphosphonium bromide
Kettle.
Background technology
Reaction kettle is a kind of common consersion unit in chemical plant, and it is anti-to stir that it mainly drives agitating shaft by motor
Thing is answered it is fully reacted to obtain required material.
With the continuous development of chemical field, production finished product and required precision of the people to chemical products are higher and higher, phase
Ying Di, people it is also proposed the important equipment " reaction kettle " in chemical reaction the requirement of higher.
At present, common reaction kettle realizes that long-time constant temperature is kept the temperature by steam-heated mode, however, when reaction kettle is anti-
Should after, can also there are larger temperature in reaction kettle and chuck；Directly allowed in this regard, existing processing mode generally uses
Its mode for cooling down and not being used carries out, but it will necessarily cause certain energy waste.
For above-mentioned problem, Authorization Notice No. provides a kind of reaction kettle for the patent of CN 204307626U, it is being reacted
Separation layer is set in still shell body, makes the water stream channel that cooling water inflow is formed between separation layer and reaction kettle housing, by cold
Flowing of the water in passage reaches the after-heat recycling to reaction kettle.However, the reaction kettle of the patent but there are it is following some
Deficiency：(1) need to be improved reaction kettle inside, transformation process and later period maintenance are cumbersome；(2) can only recycle anti-
The heat in still shell body is answered, for steam-heated reaction kettle structure, the heat recovery (heat in chuck being unfavorable in chuck
It is remaining more).
Therefore, it is badly in need of a kind of transformation, easy to maintenance, the efficient reaction kettle of heat recovery and utilization at present.
The content of the invention
It is an object of the invention to overcome deficiency of the prior art, there is provided one kind transformation, easy to maintenance, heat recovery
The high reaction kettle for being used for ethyltriphenylphosphonium bromide and preparing of utilization ratio.
The present invention is achieved by the following technical solutions：A kind of reaction kettle prepared for ethyltriphenylphosphonium bromide,
Including reaction kettle housing, double-jacket, agitating shaft and it is arranged at reaction kettle housing upper end and the electricity being connected with one end of the mixing shaft
Machine, the upper end of reaction kettle housing are equipped with manhole and temperature measuring equipment, and lower end is equipped with discharge port, and the lower end periphery of reaction kettle housing is arranged
There is the double-jacket；The double-jacket is the double fastener nested structure being sequentially overlapped, and two passages are equipped with double-jacket,
Respectively first passage and second channel；The first passage is arranged between reaction kettle housing and second channel, first passage
Upper end is equipped with steam inlet, exhaust outlet and cooling water outlet, and lower end is equipped with steam (vapor) outlet and cooling water inlet, steam (vapor) outlet with it is cold
Condenser is connected；The second channel lower end is equipped with cooling water inlet, and upper end is equipped with corresponding hot water outlet.
One of preferred embodiment as the present invention, the lower end of the agitating shaft is stretched into reaction kettle housing, and other end is stretched
Go out reaction kettle housing with motor to be connected.
One of preferred embodiment as the present invention, the agitating shaft are used for the first in ethyltriphenylphosphonium bromide preparation process
Benzene, triphenylphosphine and bromoethane mixed liquor are stirred.
One of preferred embodiment as the present invention, the motor is arranged at the centre position of reaction kettle housing, motor side
Reaction kettle housing be equipped with manhole, the reaction kettle housing of motor opposite side is equipped with temperature measuring equipment, the extension of temperature measuring equipment lower end
To reaction kettle enclosure interior lower end.
One of preferred embodiment as the present invention, the manhole are used for the triphen in ethyltriphenylphosphonium bromide preparation process
The input of base phosphine.
One of preferred embodiment as the present invention, the steam inlet, exhaust outlet, cooling water outlet, steam (vapor) outlet, cooling
Valve member is further respectively had on water inlet, cooling water inlet and hot water outlet.
One of preferred embodiment as the present invention, the steam inlet is equipped with the first valve, steam (vapor) outlet and condenser
Between be equipped with the second valve, condenser ends are equipped with the 3rd valve, the first valve, the second valve and the 3rd valve collectively form plus
Thermal control component；The computer heating control component control steam enters first passage from steam inlet, then condensed device is condensed to cold
Channel switch and closure during condensate outflow.
As one of preferred embodiment of the present invention, the cooling water inlet is equipped with the 4th valve, and hot water outlet is equipped with the
Five valves, exhaust outlet are equipped with the 6th valve, and the 4th valve, the 5th valve and the 6th valve collectively form heat recovery control group
Part；The heat recovery control assembly control cold water enters second channel from cooling water inlet, then through hot water outlet in the form of hot water
Channel switch and closure during outflow.
One of preferred embodiment as the present invention, the cooling water inlet is equipped with the 7th valve, is set on cooling water outlet
There is the 8th valve, the 7th valve and the 8th valve collectively form cooling control assembly；The cooling control assembly control cooling water
Enter first passage from cooling water inlet, then channel switch and closure during being flowed out through cooling water outlet.
One of preferred embodiment as the present invention, the reaction kettle housing is specially stainless steel cauldron housing.
The present invention compared with prior art the advantages of be：
(1) in terms of existing technologies, the present invention both facilitates system without being modified to the inside of reaction kettle housing
Make, and be beneficial to later period maintenance；In addition, the present invention realizes heat recovery by being improved to the chuck of reaction kettle, moreover it is possible to high
Heat in the most chuck of effect recycling after-heat；
(2) of the invention the first valve, the second valve and the 3rd valve collectively form computer heating control component, control steam from
Steam inlet enters first passage, then condensed device condenses to condensed water the channel switch and closure during flowing out, realization pair
The control of reaction kettle heating；
(3) the 4th valve, the 5th valve and the 6th valve of the invention collectively form heat recovery control assembly, and control is cold
Water enters second channel from cooling water inlet, then channel switch and closure during being flowed out through hot water outlet in the form of hot water, real
Now the recycling to after-heat in double-jacket after reaction controls；
(4) the 7th valve and the 8th valve of the invention collectively form cooling control assembly, control cooling water from cooling water
Import enters first passage, then channel switch and closure during being flowed out through cooling water outlet, realizes to anti-after reaction
Answer the rapid cooling control of kettle.
Brief description of the drawings
Fig. 1 is the overall structure diagram for being used for reaction kettle prepared by ethyltriphenylphosphonium bromide in embodiment 1.
In figure：1 is reaction kettle housing, and 11 be manhole, and 12 be discharge port, and 13 be temperature measuring equipment, and 2 be double-jacket, and 21 are
First passage, 211 be steam inlet, and 212 be exhaust outlet, and 213 be steam (vapor) outlet, and 214 be cooling water outlet, and 215 be cooling water
Import, 22 be second channel, and 221 be cooling water inlet, and 222 be hot water outlet, and 3 be agitating shaft, and 4 be motor, and 5 be condenser, and 6 are
Valve member, 61 be the first valve, and 62 be the second valve, and 63 be the 3rd valve, and 64 be the 4th valve, and 65 be the 5th valve, 66
It is the 7th valve for the 6th valve, 67,68 be the 8th valve.
Embodiment
Elaborate below to the embodiment of the present invention, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
As shown in Figure 1, a kind of reaction kettle prepared for ethyltriphenylphosphonium bromide of the present embodiment, simple in structure, make
With convenient, beneficial to effective recycling of heat after reaction in reaction kettle, including reaction kettle housing 1, reaction kettle housing 1 is sheathed on
Double-jacket 2, agitating shaft 3 and the motor 4 for being arranged at 1 upper end centre position of reaction kettle housing of lower end periphery.Wherein, stir
The lower end of axis 3 is stretched into reaction kettle housing 1, to the toluene in ethyltriphenylphosphonium bromide preparation process, triphenylphosphine and bromine second
Alkane mixed liquor is stirred mixing；The other end of agitating shaft 3 then stretches out reaction kettle housing 1 and is connected with motor 4, makes the motor 4 be
It provides power source.
Reaction kettle housing 1 is stainless steel cauldron housing, and 1 upper end of reaction kettle housing deviates middle position and is equipped with manhole
11, which is used for the input of the triphenylphosphine in ethyltriphenylphosphonium bromide preparation process；1 upper end of reaction kettle housing and people
The opposite opposite side in hole 11 is equipped with temperature measuring equipment 13, and 13 lower end of temperature measuring equipment extends to 1 interior lower end of reaction kettle housing, the thermometric
Device 13 is used to measure the temperature in reaction kettle；In addition, 1 lower end of reaction kettle housing is additionally provided with discharge port 12, which uses
Terminate the discharge of material in reaction.
Double-jacket 2 is the double fastener nested structure being sequentially overlapped, and is equipped with two passages in double-jacket 2, respectively uses
First passage 21 in steam flowing and the second channel 22 for current flowing.Wherein, first passage 21 is arranged at reaction kettle
Between housing 1 and second channel 22, the upper end is equipped with steam inlet 211, exhaust outlet 212 and cooling water outlet 214, and lower end is equipped with
Steam (vapor) outlet 213 and cooling water inlet 215, steam (vapor) outlet 213 are further connected with condenser 5；22 lower end of second channel is equipped with
Cooling water inlet 221, upper end are equipped with corresponding hot water outlet 222.Wherein, steam inlet 211, exhaust outlet 212, cooling water outlet,
Valve member 6 is further respectively had on steam (vapor) outlet 213, cooling water inlet, cooling water inlet 221 and hot water outlet 222.
Further, steam inlet 211 is equipped with the first valve 61, and second is equipped between steam (vapor) outlet 213 and condenser 5
Valve 62,5 end of condenser are equipped with the 3rd valve 63, and the first valve 61, the second valve 62 and the 3rd valve 63, which collectively form, to be added
Thermal control component；The computer heating control component controls steam to enter first passage 21 from steam inlet 211, then condensed device 5 condenses
Channel switch and closure during being flowed out to condensed water, so as to fulfill the control heated to reaction kettle.
Further, cooling water inlet 221 is equipped with the 4th valve 64, and hot water outlet 222 is equipped with the 5th valve 65, exhaust
Mouth 212 is equipped with the 6th valve 66, and the 4th valve 64, the 5th valve 65 and the 6th valve 66 collectively form heat recovery control group
Part；The heat recovery control assembly controls cold water to enter second channel 22 from cooling water inlet 221, then through hot water outlet 222 with heat
Channel switch and closure during the outflow of water form, are returned so as to fulfill to after-heat in double-jacket 2 after reaction
Receive control.
Further, cooling water inlet 215 is equipped with the 7th valve 67, and cooling water outlet 214 is equipped with the 8th valve 68,
7th valve 67 and the 8th valve 68 collectively form cooling control assembly；The cooling control assembly controls cooling water from cooling water
Import 215 enters first passage 21, then through the channel switch and closure during the outflow of cooling water outlet 214, realizes to reaction
After reaction kettle rapid cooling control.
Wherein, the detailed process that prepared by ethyltriphenylphosphonium bromide is as follows：
(1) 1600kg toluene is added by head tank with pump in 3000L stainless steel cauldrons；
(2) 433kg triphenylphosphines are added by manhole, mixed liquor is stirred with 65rpm/min mixing speeds；Heating
183kg bromoethanes are slowly added dropwise to 110 DEG C of reflux, then by head tank, are then refluxed for reaction 8.0h；
(3) using the mixed liquor after HPLC sampling detection back flow reactions, treat that the testing result of sample shows as raw material residual
During less than 0.5%, it is considered as qualification；After detection is qualified, stops heating, be cooled to 25 DEG C of room temperature, centrifuge；
(4) filter cake that above-mentioned centrifugation obtains is washed with 200kg toluene in centrifuge, toluene is washed using vacuum desiccator
Filter cake after washing is dried, and obtains ethyltriphenylphosphonium bromide；
(5) filtrate is distilled to recover toluene, for lower batch reaction；Wherein, the specific method of filtrate distillation recovery toluene is：Return
Receive kettle chuck and lead to steam heat temperature raising, treat that temperature in the kettle rises to 110 DEG C, begin to boil off, then be received back after being condensed by condenser
Receive toluene.
The present embodiment reaction kettle is specially the reaction used in above-mentioned ethyltriphenylphosphonium bromide preparation process (1)-(3)
Kettle, the specifically used method and principle of the reaction kettle are as follows：
(1) toluene is added in reaction kettle；
(2) triphenylphosphine is put into by manhole 11, then mixing is stirred it by agitating shaft 3；Meanwhile to steam into
Mouth 211, which is passed through hot steam, makes its flowing in first passage 21, and opens the first valve 61, the second valve 62 and the 3rd valve 63
(closing of other valves) carries out reaction kettle to be heated to target temperature (observing temperature by temperature measuring equipment 13)；When steam flows to
21 bottom of first passage, it continues through steam (vapor) outlet 213 and flows out, then is condensed by condenser 5 to condensed water and discharge (condensed water
Recycling)；
(3) bromoethane, back flow reaction are added in reaction kettle；
(4) reacted in question response kettle and terminate (reaction kettle in double-jacket 2 with there remains many heats), first close the first valve
The 61, second valve 62 of door and the 3rd valve 63, then cold water is passed through to cooling water inlet 221, and open the 4th valve 64, the 5th valve
65 and the 6th valve 66；On the one hand, remaining steam is discharged by exhaust outlet 212, on the other hand, cold water absorbing reaction kettle with it is double
Remaining heat is converted into hot water in layer chuck 2, and flow out that (it is hot that hot water is used for other in the form of hot water by hot water outlet 222
Measure source recycling to use)；
(5) reactor temperature is measured using temperature measuring equipment 13, treats that temperature no longer declines, close the 4th valve the 64, the 5th
65 and the 6th valve 66 of valve；
(6) if temperature is also not up in ethyltriphenylphosphonium bromide preparation process at this time " after detection is qualified, stop heating,
Be cooled to 25 DEG C of room temperature " in temperature requirement, then open the 7th valve 67 and the 8th valve 68, control cooling water from cooling water into
Mouth 215 enters first passage 21, then is flowed out through cooling water outlet 214, realizes the rapid cooling to reaction kettle.
(7) to the end of all processes, all valves are closed.
The aforesaid reaction vessel of the present embodiment and ethyltriphenylphosphonium bromide preparation process are fully mated, it can not only be realized instead
Answer the rapid heating of kettle, moreover it is possible to when necessary to its rapid cooling, moreover it is possible to recycle reaction kettle after reaction and folder in time
After-heat in set, for secondary use, avoids wasting.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of reaction kettle prepared for ethyltriphenylphosphonium bromide, it is characterised in that including reaction kettle housing, Double-layer clamp
Set, agitating shaft and be arranged at reaction kettle housing upper end and the motor being connected with one end of the mixing shaft, and the upper end of reaction kettle housing is set
There are manhole and temperature measuring equipment, lower end is equipped with discharge port, and the lower end periphery of reaction kettle housing is arranged with the double-jacket；It is described double
Layer chuck is the double fastener nested structure being sequentially overlapped, and two passages are equipped with double-jacket, is respectively first passage and second
Passage；The first passage is arranged between reaction kettle housing and second channel, and first passage upper end is equipped with steam inlet, exhaust
Mouth and cooling water outlet, lower end are equipped with steam (vapor) outlet and cooling water inlet, and steam (vapor) outlet is connected with condenser；The second channel
Lower end is equipped with cooling water inlet, and upper end is equipped with corresponding hot water outlet.
2. the reaction kettle according to claim 1 prepared for ethyltriphenylphosphonium bromide, it is characterised in that the stirring
The lower end of axis is stretched into reaction kettle housing, and other end stretches out reaction kettle housing and is connected with motor.
3. the reaction kettle according to claim 1 prepared for ethyltriphenylphosphonium bromide, it is characterised in that the stirring
Toluene, triphenylphosphine and the bromoethane mixed liquor that axis is used in ethyltriphenylphosphonium bromide preparation process are stirred.
4. the reaction kettle according to claim 1 prepared for ethyltriphenylphosphonium bromide, it is characterised in that the motor
The centre position of reaction kettle housing is arranged at, the reaction kettle housing of motor side is equipped with manhole, the reaction kettle of motor opposite side
Housing is equipped with temperature measuring equipment, and temperature measuring equipment lower end extends to reaction kettle enclosure interior lower end.
5. the reaction kettle according to claim 1 prepared for ethyltriphenylphosphonium bromide, it is characterised in that the manhole
Input for the triphenylphosphine in ethyltriphenylphosphonium bromide preparation process.
6. the reaction kettle according to claim 1 prepared for ethyltriphenylphosphonium bromide, it is characterised in that the steam
Valve is further respectively had on import, exhaust outlet, cooling water outlet, steam (vapor) outlet, cooling water inlet, cooling water inlet and hot water outlet
Component.
7. the reaction kettle according to claim 6 prepared for ethyltriphenylphosphonium bromide, it is characterised in that the steam
Import is equipped with the first valve, and the second valve is equipped between steam (vapor) outlet and condenser, and condenser ends are equipped with the 3rd valve, the
One valve, the second valve and the 3rd valve collectively form computer heating control component；The computer heating control component controls steam from steam
Import enters first passage, then condensed device condenses to condensed water the channel switch and closure during flowing out.
8. the reaction kettle according to claim 6 prepared for ethyltriphenylphosphonium bromide, it is characterised in that the cold water
Import is equipped with the 4th valve, and hot water outlet is equipped with the 5th valve, and exhaust outlet is equipped with the 6th valve, the 4th valve, the 5th
Valve and the 6th valve collectively form heat recovery control assembly；The heat recovery control assembly controls cold water from cooling water inlet
Into second channel, then channel switch and closure during being flowed out through hot water outlet in the form of hot water.
9. the reaction kettle according to claim 6 prepared for ethyltriphenylphosphonium bromide, it is characterised in that the cooling
Water inlet is equipped with the 7th valve, and cooling water outlet is equipped with the 8th valve, and the 7th valve and the 8th valve collectively form cooling
Control assembly；The cooling control assembly control cooling water enters first passage from cooling water inlet, then through cooling water outlet stream
Channel switch and closure during going out.
10. according to any reaction kettles for being used for ethyltriphenylphosphonium bromide and preparing of claim 1-9, it is characterised in that
The reaction kettle housing is specially stainless steel cauldron housing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711445952.4A CN107930565A (en) | 2017-12-27 | 2017-12-27 | A kind of reaction kettle prepared for ethyltriphenylphosphonium bromide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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