CN109912395A - A kind of device and process of differential circulation continuous production dichloro pinacolone - Google Patents
A kind of device and process of differential circulation continuous production dichloro pinacolone Download PDFInfo
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- CN109912395A CN109912395A CN201910270578.1A CN201910270578A CN109912395A CN 109912395 A CN109912395 A CN 109912395A CN 201910270578 A CN201910270578 A CN 201910270578A CN 109912395 A CN109912395 A CN 109912395A
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- UDWZXMQIEHAAQT-UHFFFAOYSA-N 1,1-dichloro-3,3-dimethylbutan-2-one Chemical compound CC(C)(C)C(=O)C(Cl)Cl UDWZXMQIEHAAQT-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000010924 continuous production Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 16
- 230000008569 process Effects 0.000 title abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 89
- 239000007788 liquid Substances 0.000 claims abstract description 81
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 75
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 61
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 61
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000000460 chlorine Substances 0.000 claims abstract description 55
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 55
- 238000006243 chemical reaction Methods 0.000 claims abstract description 44
- 238000001816 cooling Methods 0.000 claims abstract description 18
- PJGSXYOJTGTZAV-UHFFFAOYSA-N pinacolone Chemical compound CC(=O)C(C)(C)C PJGSXYOJTGTZAV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000007599 discharging Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000007033 dehydrochlorination reaction Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 5
- -1 main reactor Chemical compound 0.000 claims abstract description 4
- 239000000498 cooling water Substances 0.000 claims description 25
- 238000000926 separation method Methods 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 19
- 238000012856 packing Methods 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 9
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 6
- 239000010962 carbon steel Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims 1
- 239000002699 waste material Substances 0.000 abstract description 5
- 238000010923 batch production Methods 0.000 abstract description 3
- 239000005708 Sodium hypochlorite Substances 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000007086 side reaction Methods 0.000 abstract description 2
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 1
- 239000003513 alkali Substances 0.000 abstract 1
- 238000006298 dechlorination reaction Methods 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- MBGXGIRUXKTQIN-UHFFFAOYSA-N CC(C(C)(C)C)=O.[Cl] Chemical compound CC(C(C)(C)C)=O.[Cl] MBGXGIRUXKTQIN-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The present invention provides a kind of device and process of differential circulation continuous production dichloro pinacolone, including main reactor, pre-reactor, separator, circulating pump, discharging pump, pipeline and automatic instrument(s), the main reactor and pre-reactor are that tubular type microchannel plate answers heat exchanger, all have multiple longitudinal tube sides and multiple lateral shell sides, shell side is for cooling down, tube side is for conveying material, the present invention reduces the generation of trichlorine pinacolone by differential circle flow process, improve the yield of product, with the pinacolone being newly added chemical reaction is occurred into for free chlorine in tail gas hydrogen chloride gas using pre-reactor and is removed, save the side reaction problem of the method bring sodium hypochlorite with alkali cleaning, chlorated liquid after reaction realizes efficiently separating for dichloro pinacolone and the hydrogen chloride that is dissolved in chlorated liquid using vacuum dechlorination hydrogen technology, replace traditional Environmental issue batch process plus that water dehydrochlorination brings waste hydrochloric acid to generate.
Description
Technical field
The present invention relates to field of fine chemical, and in particular to a kind of device of differential circulation continuous production dichloro pinacolone with
Technique.
Background technique
Dichloro pinacolone is the important source material and intermediate of organic synthesis.It can be widely used for pesticide, medicine intermediate, past
Also once to prepare triazolinones fungicide.
Dichloro pinacolone synthetic method is by pinacolone by chlorinated with chlorine, and is made.
Technological principle:
The chlorine pinacolone of metering is added in chlorinating container, and chlorine is warming up to 40 DEG C of chlorine, and through surge tank to be passed into chlorination anti-
It answers in kettle, at this temperature insulation reaction 70 hours.Device for absorbing tail gas is opened simultaneously, and the hydrogen chloride of association is absorbed through water into salt
Acid, excessive chlorine generate the waste liquid containing sodium hypochlorite and are focused on through absorbing by liquid caustic soda.After reaction, will add in kettle
Water cooling, washing to solution not chloride ion-containing.Waste liquid is filtered out, crystal cooling packing is at product
The production method is that batch production technique, simple process, flexible operation, but consumption of raw materials are high, and the production cycle is long,
Equipment investment is big (reaction kettle is more), at high cost, seriously polluted.
Currently, under the new demand of " efficiency multiplication, sustainable economic development ", need it is a kind of it is novel " energy conservation, consumption reduction,
The dichloro pinacolone production method of environmental protection ".
Summary of the invention
The purpose of the present invention is to provide a kind of device and process of differential circulation continuous production dichloro pinacolone, to solve
The problems mentioned above in the background art.
To achieve the above object, the invention provides the following technical scheme:
A kind of device of continuity method production pinacolone, including main reactor, pre-reactor, separator, circulating pump, discharging
Pump, demister and pipeline and automatic instrument(s), the main reactor is that tubular type microchannel plate answers heat exchanger, with multiple longitudinal directions
Main reactor tube side and multiple lateral main reactor shell sides, main reactor shell side both ends be separately connected set on main reactor two
The main reactor cooling water inlet and main reactor cooling water outlet of side, the main reactor bottom are provided with gas-liquid mixed room,
Gas-liquid mixed room bottom offers main reactor gas access, and side offers main reactor liquid inlet, the gas-liquid
Efficient mixed structure body is set in mixing chamber, gas distributor is equipped in the middle part of the main reactor, and gas distributor is equipped with master
Reactor chlorine inlet, the main reactor tube side upper and lower ends be separately connected main reactor discharge port at the top of main reactor and
Gas-liquid mixed room；
The pre-reactor is that tubular type microchannel plate answers heat exchanger, with multiple longitudinal pre-reactor tube sides and multiple
Lateral pre-reactor shell side, upper end is provided with packed tower section in the pre-reactor, and pre-reactor shell side both ends are separately connected
Pre-reactor cooling water inlet and pre-reactor cooling water outlet set on pre-reactor two sides, the pre-reactor bottom are equipped with
Pre-reactor mixing chamber, pre-reactor mixing chamber bottom are equipped with pre-reactor mixture export, and side is equipped with pre-reactor gas
Entrance, pre-reactor top are equipped with pre-reactor separation chamber, and pre-reactor separation chamber side is equipped with pinacolone feed opening, and top is set
There is pre-reactor discharge port；
Separator feeding inlet, separator gas outlet are equipped at the top of the separator, separator bottom is equipped with separator chlorine
Import and separator discharge port；
The main reactor gas access and main reactor gas access are passed through chlorine, the connection separation of main reactor discharge port
Device feeding inlet, the pre-reactor gas access connect separator gas outlet, and pre-reactor discharge port connects the entrance of demister,
The outlet liquid phase of demister connects and pump entry, and gas phase connects hydrogen chloride absorption equipment, and the outlet connection of circulating pump is main anti-
Device liquid inlet is answered, separator chlorine inlet is passed through chlorine, and separator discharge port connects the entrance of circulating pump and entering for discharging pump
Mouthful, the outlet device for separating connection of discharging pump.
Preferably, being filled with microchannel ceramic packing in the main reactor tube side and pre-reactor tube side, this is micro-
Channel ceramic packing diameter is 8~100mm, and the diameter of main reactor tube side is 10~110mm, and the diameter of pre-reactor tube side is
8~120mm.
Preferably, the microchannel ceramic packing diameter is 14~64mm, main reactor tube side diameter is 15~65mm,
Pre-reactor tube side diameter is 30~100mm.
Preferably, the main body of the main reactor and pre-reactor is by titanium alloy, impregnated graphite, carbon steel, carbonization
The one or more of silicon are made, and the shell of main reactor and pre-reactor is carbon steel.
Preferably, being equipped with separator refluxing opening at the top of the separator, it is mixed which connects pre-reactor
Close liquid outlet.
A kind of technique of differential circulation continuous production dichloro pinacolone based on above-mentioned apparatus, comprising the following steps:
Step 1: the chlorine that the chlorated liquid in separator is passed through with separator chlorine inlet chemically reacts, and by separating
Device discharge port is discharged and by entering gas-liquid mixed room from main reactor liquid inlet after circulating pump pressurization, with main reactor gas
The chlorine that entrance is passed through is sufficiently mixed under the action of efficient mixed structure body, and mixed mixed liquor enters main reactor tube side
Chemically reacted, all the way chlorine from main reactor chlorine inlet enter after gas distributor is uniformly dispersed with main reactor pipe
Mixed liquor in journey is chemically reacted, while cooling by the cooling water in main reactor shell side, the mixed liquor warp after reaction
It crosses main reactor discharge port and separator feeding inlet flows back into and carries out gas-liquid separation in separator；
Step 2: the hydrogen chloride gas after separation is entered after the discharge of separator gas outlet by pre-reactor gas access
Pre-reactor mixing chamber, chlorated liquid again through circulating pump enters main reactor the reaction was continued in separator；
When the dichloro pinacolone concentration of chlorated liquid in separator reaches 97% or more, then chlorated liquid is beaten by discharging pump
Out, it send to dehydrochlorination equipment, under vacuum removes the hydrogen chloride gas dissolved in chlorated liquid, solution is through crystallisation by cooling at two
Chlorine pinacolone, hydrogen chloride absorb hydrochloric acid with water；
Step 3: the free chlorine of hydrogen chloride gas entrainment reacts in pre-reactor and rises to pre-reactor separation chamber, with
After the pinacolone mixing that pinacolone feed opening is added, the liquid of entrainment is recycled herein, hydrogen chloride gas is from pre-reactor discharge port
It is discharged into demister, it is cooling by the cooling water in pre-reactor shell side when pre-reactor reacts；
Step 4: demister retains the hydrogen chloride drop carried secretly in hydrogen chloride gas, and hydrogen chloride gas enters hydrogen chloride suction
Receiving unit；
Step 5: the mixed liquor that the hydrogen chloride drop and separator discharge port separated in demister comes out passes through after converging to follow
Ring pump is squeezed into main reactor.
Preferably, the reaction temperature in the step 1 is 35~75 DEG C, reaction pressure is 80~250KPa.
Preferably, reaction temperature is 20~65 DEG C in the step 3, reaction pressure is 80~250KPa.
Compared with the prior art, the invention has the following advantages that
(1) low equipment investment:
Due to by differential circle flow process (by circulating pump come chlorated liquid and chlorine in the microchannel of main reactor, gas
Liquid comes into full contact with, and increases its residence time, while controlling the temperature of reaction process, is passed through at chlorination liquified chlorine gas and chlorated liquid point three
To evade depth chlorination generation, referred to as differential circulation reacts) generation that reduces trichlorine pinacolone in chlorated liquid, it improves anti-
Should be selective, therefore compared with traditional technology, set of device may replace tens reaction kettles, reduce integral device investment；
(2) high production efficiency:
Circulation continuous production is integrally formed, and uses microchannel mechanism in main reactor and pre-reactor, mentions significantly
High reaction efficiency, chlorine have effectively evaded the generation of side reaction trichlorine pinacolone, Jin Erti by being reacted at three with chlorated liquid
The high product quality of dichloro pinacolone；
(3) environmentally protective:
Chlorated liquid removes the hydrogen chloride gas of dissolution through rotary film evaporator under vacuum conditions, and avoidable batch process adds
The pollution of water washing hydrogen chloride bring waste hydrochloric acid；The hydrogen chloride that tail gas generates can retain 98% or more 1um through demister
Liquid, high-purity hydrogen chloride can be used for producing downstream hydrogen chloride product.Prior art is compared, entire production process no three wastes generates,
It is automatically cleaning chemical industry skill, reaches circular economy purpose.
Detailed description of the invention
Fig. 1 is the whole structure flow chart of the present invention；
Fig. 2 is the structural schematic diagram of main reactor in the present invention；
Fig. 3 is the structural schematic diagram of pre-reactor in the present invention；
Fig. 4 is the structural schematic diagram of separator in the present invention.
In figure: 1- main reactor, 2- pre-reactor, 3- separator, 101- gas distributor, 102- main reactor shell side,
103- main reactor cooling water outlet, 104- main reactor discharge port, 105- main reactor tube side, 106- main reactor cooling water
Import, 107- main reactor chlorine inlet, 108- gas-liquid mixed room, the efficient mixed structure body of 109-, 110- main reactor gas
Entrance, 111- main reactor liquid inlet, 201- pre-reactor shell side, 202- pinacolone feed opening, the discharging of 203- pre-reactor
Mouthful, 204- pre-reactor separation chamber, 205- pre-reactor cooling water outlet, 206- pre-reactor tube side, 207- packed tower section,
208- pre-reactor mixing chamber, 209- pre-reactor gas access, 210- pre-reactor mixture export, 211- pre-reactor are cold
But water inlet, 301- separator gas outlet, 302- separator discharge port, 303- separator feeding inlet, 304- separator refluxing opening,
305- separator chlorine inlet.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Please refer to Fig. 1-4, a kind of device of differential circulation continuous production dichloro pinacolone, including main reactor 1, pre-reaction
Device 2, separator 3, circulating pump, discharging pump, demister and pipeline and automatic instrument(s), the main reactor 1 are tubular type microchannel
Reacting replacing heat device, with multiple longitudinal main reactor tube sides 105 and multiple lateral main reactor shell sides 102, main reaction
102 both ends of device shell side are separately connected main reactor cooling water inlet 106 and main reactor cooling water set on 1 two sides of main reactor
Outlet 103,1 bottom of main reactor are provided with gas-liquid mixed room 108, and 108 bottom of gas-liquid mixed room offers main anti-
Device gas access 110 is answered, side offers main reactor liquid inlet 111, and efficiently mixing knot is set in the gas-liquid mixed room 108
Structure body 109, gas distributor 101 is equipped in the middle part of the main reactor 1, and gas distributor 101 is equipped with main reactor chlorine
Import 107,105 upper and lower ends of main reactor tube side are separately connected 104 He of main reactor discharge port at 1 top of main reactor
Gas-liquid mixed room 108；
The pre-reactor 2 is that tubular type microchannel plate answers heat exchanger, with multiple longitudinal 206 Hes of pre-reactor tube side
Multiple lateral pre-reactor shell sides 201, upper end is provided with packed tower section 207, pre-reactor shell side in the pre-reactor 2
201 both ends are separately connected pre-reactor cooling water inlet 211 and pre-reactor cooling water outlet set on 2 two sides of pre-reactor
205,2 bottom of pre-reactor is equipped with pre-reactor mixing chamber 208, and 208 bottom of pre-reactor mixing chamber is equipped with pre-reactor
Mixture export 210, side are equipped with pre-reactor gas access 209, are equipped with pre-reactor separation chamber 204 at the top of pre-reactor 2,
204 side of pre-reactor separation chamber is equipped with pinacolone feed opening 202, and top is equipped with pre-reactor discharge port 203；
Separator feeding inlet 303, separator gas outlet 301 are equipped at the top of the separator 3,3 bottom of separator, which is equipped with, to be divided
From device chlorine inlet 305 and separator discharge port 302；
The main reactor gas access 110 and main reactor chlorine inlet 107 are passed through chlorine, main reactor discharge port
104 connection separator feeding inlets 303, the pre-reactor gas access 209 connect separator gas outlet 301, and pre-reactor goes out
Material mouth 203 connects the entrance of demister, the outlet liquid phase connection of demister and pump entry, and gas phase connection hydrogen chloride absorption is set
Standby, the outlet of circulating pump connects main reactor liquid inlet 111, and separator chlorine inlet 305 is passed through chlorine, separator discharge port
The entrance of 302 connection circulating pumps and the entrance of discharging pump, the outlet device for separating connection of discharging pump.
Wherein, it is filled with microchannel ceramic packing in the main reactor tube side 105 and pre-reactor tube side 206, it should
Microchannel ceramic packing diameter is 8~100mm, and the diameter of main reactor tube side 105 is 10~110mm, pre-reactor tube side 206
Diameter be 8~120mm.
Preferably, the microchannel ceramic packing diameter be 14~64mm, 105 diameter of main reactor tube side be 15~
65mm, 206 diameter of pre-reactor tube side are 30~100mm.
Wherein, the main body of the main reactor 1 and pre-reactor 2 is by titanium alloy, impregnated graphite, carbon steel, silicon carbide
One or more be made, the shell of main reactor 1 and pre-reactor 2 is carbon steel.
Wherein, separator refluxing opening 304 is equipped at the top of the separator 3, which connects pre-reactor
Mixture export 210.
Embodiment one:
Step 1: the chlorine that the chlorated liquid in separator 3 is passed through with separator chlorine inlet 305 chemically reacts, and by
Separator discharge port 302 is discharged and by entering gas-liquid mixed room 108 from main reactor liquid inlet 111 after circulating pump pressurization,
The chlorine being passed through with main reactor gas access 110 is sufficiently mixed under the action of efficient mixed structure body 109, mixed mixed
Conjunction liquid enters main reactor tube side 105 and is chemically reacted, and chlorine enters from main reactor chlorine inlet 107 through gas point all the way
Cloth device 101 is chemically reacted after being uniformly dispersed with the mixed liquor in main reactor tube side 105, and (reaction temperature is 35 DEG C, reaction
Pressure is 80KPa), at the same it is cooling by the cooling water in main reactor shell side 102, and the mixed liquor after reaction passes through main reactor
Discharge port 104 and separator feeding inlet 303, which flow back into, carries out gas-liquid separation in separator 3；
Step 2: the hydrogen chloride gas after separation passes through pre-reactor gas access after being discharged from separator gas outlet 301
209 enter pre-reactor mixing chambers 208, and chlorated liquid again through circulating pump enters main reactor 1 the reaction was continued in separator 3；
When the dichloro pinacolone concentration of chlorated liquid in separator 3 reaches 97% or more, then pass through discharging pump for chlorated liquid
Get, send to dehydrochlorination equipment, under vacuum remove the hydrogen chloride gas dissolved in chlorated liquid, solution through crystallisation by cooling at
Dichloro pinacolone, hydrogen chloride absorb hydrochloric acid with water；
Step 3: hydrogen chloride gas entrainment free chlorine react in pre-reactor 2 (reaction temperature be 20 DEG C, reaction pressure
For 80KPa) and pre-reactor separation chamber 204 is risen to, after mixing with the pinacolone that pinacolone feed opening 202 is added, in this time
The liquid of entrainment is received, hydrogen chloride gas is discharged into demister from pre-reactor discharge port 203, and pre-reactor 2 passes through when reacting
Cooling water in pre-reactor shell side 201 is cooling；
Step 4: demister retains the hydrogen chloride drop carried secretly in hydrogen chloride gas, and hydrogen chloride gas enters hydrogen chloride suction
Receiving unit；
Step 5: the mixed liquor that the hydrogen chloride drop and separator discharge port 302 separated in demister comes out passes through after converging
Circulating pump is squeezed into main reactor 1.
Embodiment two:
Step 1: the chlorine that the chlorated liquid in separator 3 is passed through with separator chlorine inlet 305 chemically reacts, and by
Separator discharge port 302 is discharged and by entering gas-liquid mixed room 108 from main reactor liquid inlet 111 after circulating pump pressurization,
The chlorine being passed through with main reactor gas access 110 is sufficiently mixed under the action of efficient mixed structure body 109, mixed mixed
Conjunction liquid enters main reactor tube side 105 and is chemically reacted, and chlorine enters from main reactor chlorine inlet 107 through gas point all the way
Cloth device 101 is chemically reacted after being uniformly dispersed with the mixed liquor in main reactor tube side 105, and (reaction temperature is 75 DEG C, reaction
Pressure is 250KPa), at the same it is cooling by the cooling water in main reactor shell side 102, and the mixed liquor after reaction passes through main reaction
Device discharge port 104 and separator feeding inlet 303, which flow back into, carries out gas-liquid separation in separator 3；
Step 2: the hydrogen chloride gas after separation passes through pre-reactor gas access after being discharged from separator gas outlet 301
209 enter pre-reactor mixing chambers 208, and chlorated liquid again through circulating pump enters main reactor 1 the reaction was continued in separator 3；
When the dichloro pinacolone concentration of chlorated liquid in separator 3 reaches 97% or more, then pass through discharging pump for chlorated liquid
Get, send to dehydrochlorination equipment, under vacuum remove the hydrogen chloride gas dissolved in chlorated liquid, solution through crystallisation by cooling at
Dichloro pinacolone, hydrogen chloride absorb hydrochloric acid with water；
Step 3: hydrogen chloride gas entrainment free chlorine react in pre-reactor 2 (reaction temperature be 65 DEG C, reaction pressure
For 250KPa) and pre-reactor separation chamber 204 is risen to, after mixing with the pinacolone that pinacolone feed opening 202 is added, in this time
The liquid of entrainment is received, hydrogen chloride gas is discharged into demister from pre-reactor discharge port 203, and pre-reactor 2 passes through when reacting
Cooling water in pre-reactor shell side 201 is cooling；
Step 4: demister retains the hydrogen chloride drop carried secretly in hydrogen chloride gas, and hydrogen chloride gas enters hydrogen chloride suction
Receiving unit；
Step 5: the mixed liquor that the hydrogen chloride drop and separator discharge port 302 separated in demister comes out passes through after converging
Circulating pump is squeezed into main reactor 1.
Embodiment three:
Step 1: the chlorine that the chlorated liquid in separator 3 is passed through with separator chlorine inlet 305 chemically reacts, and by
Separator discharge port 302 is discharged and by entering gas-liquid mixed room 108 from main reactor liquid inlet 111 after circulating pump pressurization,
The chlorine being passed through with main reactor gas access 110 is sufficiently mixed under the action of efficient mixed structure body 109, mixed mixed
Conjunction liquid enters main reactor tube side 105 and is chemically reacted, and chlorine enters from main reactor chlorine inlet 107 through gas point all the way
Cloth device 101 is chemically reacted after being uniformly dispersed with the mixed liquor in main reactor tube side 105, and (reaction temperature is 55 DEG C, reaction
Pressure is 165KPa), at the same it is cooling by the cooling water in main reactor shell side 102, and the mixed liquor after reaction passes through main reaction
Device discharge port 104 and separator feeding inlet 303, which flow back into, carries out gas-liquid separation in separator 3；
Step 2: the hydrogen chloride gas after separation passes through pre-reactor gas access after being discharged from separator gas outlet 301
209 enter pre-reactor mixing chambers 208, and chlorated liquid again through circulating pump enters main reactor 1 the reaction was continued in separator 3；
When the dichloro pinacolone concentration of chlorated liquid in separator 3 reaches 97% or more, then pass through discharging pump for chlorated liquid
Get, send to dehydrochlorination equipment, under vacuum remove the hydrogen chloride gas dissolved in chlorated liquid, solution through crystallisation by cooling at
Dichloro pinacolone, hydrogen chloride absorb hydrochloric acid with water；
Step 3: the free chlorine of hydrogen chloride gas entrainment reacts that (reaction temperature 42, reaction pressure are in pre-reactor 2
It 165KPa) and rises to pre-reactor separation chamber 204, after being mixed with the pinacolone that pinacolone feed opening 202 is added, recycles herein
The liquid of entrainment, hydrogen chloride gas is discharged into demister from pre-reactor discharge port 203, by pre- when pre-reactor 2 reacts
Cooling water in reactor shell side 201 is cooling；
Step 4: demister retains the hydrogen chloride drop carried secretly in hydrogen chloride gas, and hydrogen chloride gas enters hydrogen chloride suction
Receiving unit；
Step 5: the mixed liquor that the hydrogen chloride drop and separator discharge port 302 separated in demister comes out passes through after converging
Circulating pump is squeezed into main reactor 1.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
Claims (8)
1. a kind of device of differential circulation continuous production dichloro pinacolone, including main reactor, pre-reactor, separator, circulation
Pump, discharging pump, demister and pipeline and automatic instrument(s), it is characterised in that: the main reactor is that tubular type microchannel plate should change
Hot device, with multiple longitudinal main reactor tube sides and multiple lateral main reactor shell sides, main reactor shell side both ends point
It is not connected at the main reactor cooling water inlet and main reactor cooling water outlet of main reactor two sides, the main reactor bottom
Portion is provided with gas-liquid mixed room, and gas-liquid mixed room bottom offers main reactor gas access, and side offers main reaction
Device liquid inlet sets efficient mixed structure body in the gas-liquid mixed room, is equipped with gas distributor in the middle part of the main reactor,
Gas distributor is equipped with main reactor chlorine inlet, and the main reactor tube side upper and lower ends are separately connected at the top of main reactor
Main reactor discharge port and gas-liquid mixing chamber；
The pre-reactor is that tubular type microchannel plate answers heat exchanger, with multiple longitudinal pre-reactor tube sides and multiple transverse directions
Pre-reactor shell side, upper end is provided with packed tower section in the pre-reactor, and pre-reactor shell side both ends, which are separately connected, to be set to
The pre-reactor cooling water inlet and pre-reactor cooling water outlet of pre-reactor two sides, the pre-reactor bottom are equipped with pre- anti-
Device mixing chamber is answered, pre-reactor mixing chamber bottom is equipped with pre-reactor mixture export, and side is equipped with pre-reactor gas access,
Pre-reactor separation chamber is equipped at the top of pre-reactor, pre-reactor separation chamber side is equipped with pinacolone feed opening, and top is equipped with pre-
Reactor discharge port；
Separator feeding inlet, separator gas outlet are equipped at the top of the separator, separator bottom is equipped with separator chlorine inlet
With separator discharge port；
The main reactor gas access and main reactor gas access are passed through chlorine, and main reactor discharge port connection separator enters
Material mouth, the pre-reactor gas access connect separator gas outlet, and pre-reactor discharge port connects the entrance of demister, demisting
The outlet liquid phase of device connects and pump entry, and gas phase connects hydrogen chloride absorption equipment, and the outlet of circulating pump connects main reactor
Liquid inlet, separator chlorine inlet are passed through chlorine, and separator discharge port connects the entrance of circulating pump and the entrance of discharging pump, out
Expect the outlet device for separating connection of pump.
2. a kind of device of differential circulation continuous production dichloro pinacolone according to claim 1, it is characterised in that: described
In main reactor tube side and pre-reactor tube side be filled with microchannel ceramic packing, the microchannel ceramic packing diameter be 8~
100mm, the diameter of main reactor tube side are 10~110mm, and the diameter of pre-reactor tube side is 8~120mm.
3. a kind of device of differential circulation continuous production dichloro pinacolone according to claim 2, it is characterised in that: described
Microchannel ceramic packing diameter is 14~64mm, and main reactor tube side diameter is 15~65mm, and pre-reactor tube side diameter is 30
~100mm.
4. a kind of device of differential circulation continuous production dichloro pinacolone according to claim 1, it is characterised in that: described
The main body of main reactor and pre-reactor is main by being made of the one or more of titanium alloy, impregnated graphite, carbon steel, silicon carbide
The shell of reactor and pre-reactor is carbon steel.
5. a kind of device of differential circulation continuous production dichloro pinacolone according to claim 1, it is characterised in that: described
Separator refluxing opening is equipped at the top of separator, which connects pre-reactor mixture export.
6. a kind of described in any item techniques of differential circulation continuous production dichloro pinacolone of claim 1-5, it is characterised in that:
The following steps are included:
Step 1: the chlorine that the chlorated liquid in separator is passed through with separator chlorine inlet chemically reacts, and is gone out by separator
Material mouth is discharged and by entering gas-liquid mixed room from main reactor liquid inlet after circulating pump pressurization, with main reactor gas access
The chlorine being passed through is sufficiently mixed under the action of efficient mixed structure body, and mixed mixed liquor enters the progress of main reactor tube side
Chemical reaction, chlorine enters after gas distributor is uniformly dispersed and in main reactor tube side from main reactor chlorine inlet all the way
Mixed liquor chemically reacted, while cooling by the cooling water in main reactor shell side, the mixed liquor after reaction is by master
Reactor discharge port and separator feeding inlet, which flow back into, carries out gas-liquid separation in separator；
Step 2: the hydrogen chloride gas after separation is entered after the discharge of separator gas outlet by pre-reactor gas access pre- anti-
Device mixing chamber is answered, chlorated liquid again through circulating pump enters main reactor the reaction was continued in separator；
When the dichloro pinacolone concentration of chlorated liquid in separator reaches 97% or more, then chlorated liquid is got by discharging pump,
It send to dehydrochlorination equipment, under vacuum removes the hydrogen chloride gas dissolved in chlorated liquid, solution is through crystallisation by cooling at dichloro
Pinacolone, hydrogen chloride absorb hydrochloric acid with water；
Step 3: the free chlorine of hydrogen chloride gas entrainment reacts in pre-reactor and rises to pre-reactor separation chamber, with frequency
After the pinacolone mixing that ketone feed opening is added, the liquid of entrainment is recycled herein, and hydrogen chloride gas is discharged from pre-reactor discharge port
It is cooling by the cooling water in pre-reactor shell side when pre-reactor reacts into demister；
Step 4: demister retains the hydrogen chloride drop carried secretly in hydrogen chloride gas, and hydrogen chloride gas enters hydrogen chloride absorption and sets
It is standby；
Step 5: the mixed liquor that the hydrogen chloride drop and separator discharge port separated in demister comes out passes through circulating pump after converging
It squeezes into main reactor.
7. a kind of technique of differential circulation continuous production dichloro pinacolone as claimed in claim 6, it is characterised in that: the step
Reaction temperature in 1 is 35~75 DEG C, and reaction pressure is 80~250 KPa.
8. a kind of technique of differential circulation continuous production dichloro pinacolone as claimed in claim 6, it is characterised in that: the step
Reaction temperature is 20~65 DEG C in 3, and reaction pressure is 80~250 KPa.
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