CN109364869A - A kind of device of gas-liquid countercurrent method continuous production chloro thing - Google Patents
A kind of device of gas-liquid countercurrent method continuous production chloro thing Download PDFInfo
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- CN109364869A CN109364869A CN201811540138.5A CN201811540138A CN109364869A CN 109364869 A CN109364869 A CN 109364869A CN 201811540138 A CN201811540138 A CN 201811540138A CN 109364869 A CN109364869 A CN 109364869A
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- kettle
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- absorption
- reaction kettle
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- 239000007788 liquid Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 29
- 125000001309 chloro group Chemical group Cl* 0.000 title claims abstract description 25
- 238000010924 continuous production Methods 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 146
- 238000010521 absorption reaction Methods 0.000 claims abstract description 101
- 239000012071 phase Substances 0.000 claims abstract description 50
- 238000004519 manufacturing process Methods 0.000 claims abstract description 39
- 239000000047 product Substances 0.000 claims abstract description 25
- 239000012188 paraffin wax Substances 0.000 claims abstract description 16
- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 claims abstract description 16
- 239000007791 liquid phase Substances 0.000 claims abstract description 13
- 238000012545 processing Methods 0.000 claims abstract description 10
- 239000012043 crude product Substances 0.000 claims abstract description 9
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 125000004122 cyclic group Chemical group 0.000 claims abstract 2
- 238000001816 cooling Methods 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 16
- 230000035484 reaction time Effects 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- 241001025261 Neoraja caerulea Species 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 210000003298 dental enamel Anatomy 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- -1 enamel Substances 0.000 claims 1
- 230000002779 inactivation Effects 0.000 claims 1
- 229920000642 polymer Polymers 0.000 claims 1
- 230000036632 reaction speed Effects 0.000 abstract description 12
- 239000007789 gas Substances 0.000 description 85
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 38
- 239000000460 chlorine Substances 0.000 description 38
- 229910052801 chlorine Inorganic materials 0.000 description 38
- 239000001993 wax Substances 0.000 description 22
- 230000008569 process Effects 0.000 description 15
- 238000005660 chlorination reaction Methods 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000011265 semifinished product Substances 0.000 description 8
- 238000012546 transfer Methods 0.000 description 8
- WFDIJRYMOXRFFG-UHFFFAOYSA-N acetic acid anhydride Natural products CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
- 238000010574 gas phase reaction Methods 0.000 description 3
- 239000011344 liquid material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 230000002411 adverse Effects 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 206010054949 Metaplasia Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 235000013409 condiments Nutrition 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000002649 leather substitute Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 238000005406 washing Methods 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
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/245—Stationary reactors without moving elements inside placed in series
-
- 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
- B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
-
- 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
-
- 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
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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
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/123—Ultraviolet light
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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
- B01J19/30—Loose or shaped packing elements, e.g. Raschig rings or Berl saddles, for pouring into the apparatus for mass or heat transfer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00002—Chemical plants
- B01J2219/00027—Process aspects
- B01J2219/00033—Continuous processes
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- 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
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- 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
- B01J2219/00103—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor in a heat exchanger separate from the reactor
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- B01J2219/30408—Metal
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- B01J2219/30—Details relating to random packing elements
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of device of gas-liquid countercurrent method continuous production chloro thing, can be used for the continuous production of chlorinated paraffin, monoxone, chloromethanes etc..Including absorption tower, reaction kettle, absorption kettle, heat exchanger and exhaust gas processing device, absorption tower is connect with reaction kettle, can be equipped with heat exchanger between the two, and reaction kettle can be set as 1-5, absorption kettle is connected with after reaction kettle.Gas phase continuously enters absorption tower and reaction kettle respectively under steady production state；Liquid phase is continuously added to by absorption kettle, and reaction kettle and absorption tower are countercurrently passed through after pre-reaction, and cyclic absorption gas phase and continuous discharge liquid crude product after reaction in absorption tower and the first reaction kettle.The gas formed in absorption tower enters absorption kettle after each reaction kettle successively collects, and vent gas treatment or gas products collection device are removed after pre-reaction.The present apparatus realizes the serialization of chloro thing production, improves production efficiency and product yield, and in each reaction kettle reaction speed and thermal discharge relative equilibrium, the control performance of intensified response.
Description
Technical field
The invention belongs to chloro thing process units fields.Joined more particularly to a kind of using absorption tower, reaction kettle and absorption kettle
Equipment is closed, is reacted by gas-liquid two-phase counter current contacting, continuous high-efficient produces the new method of chloro thing.
Background technique
Chloro thing is important industrial chemicals needed for the national economic development, as chlorinated paraffin have volatility it is low, it is fire-retardant,
Many excellent physicochemical properties such as electrical insulating property is good and resistant to chemical etching, can be used as fire retardant polyvinyl chloride secondary plasticizer(-iser) etc., quilt
Be widely used in production plastics, cable, plate, hose, artificial leather and rubber product etc., it can also be used to paint, coating and profit
The additive of lubricating oil etc..Other chlorides such as monoxone is for pesticide processed and makees organic synthesis intermediate etc.；Chloromethanes can be made to have
The raw material of machine silicon also serves as solvent, refrigerant, fragrance etc..
The production of industrial chloro thing is based on batch tank liquid phase reactor, i.e., direct by chlorine or hydrogen chloride gas at present
It is passed into liquid charging stock or liquid catalyst, occurs at certain temperature and catalytic condition to introducing chlorine in raw molecule
The chlorination of atom.But since the solution rate of gas-liquid two-phase during chlorination is less than reaction speed, and reaction speed
It is inversely proportional with the carry out degree reacted, causes current chloro thing process units there are total reaction times that long, production efficiency is low, reaction
The features such as each elementary reaction speed, thermal discharge difference are big, react poor controllability.
It, should if the Chinese patent of Publication No. CN105154136A discloses the production technology and equipment of a kind of chlorinated paraffin
Patent uses reaction tower, reaction kettle and the united mode of secondary kettle, by chlorine in existing chlorinated paraffin production process into liquid wax
It dissolves and reacts while be decomposed into gas-liquid two-phase in reaction tower and dissolve and absorb, the progress of two steps is reacted in catalysis in reaction kettle, will
The reaction time of chlorinated paraffin is down to 4-10h by 20h or more.But disadvantage is that first its be intermittent reaction, Bu Nengshi
The serialization of existing production process, production efficiency not can be further improved；Second reaction speed is fast, and mainly in reaction tower and reaction
It is carried out in kettle, exothermic heat of reaction is big, and reaction controlling difficulty is big.
The Chinese patent of publication number CN105112100B discloses a kind of chlorinated paraffin continuous production processes, which uses
The reaction kettle group of six reaction kettles composition, liquid wax are continuously entered by the first reaction kettle, and chlorine after control flow by each leading into
In six reaction kettles, satisfactory chlorinated paraffin and continuous discharge are generated in the last one reaction kettle, realizes chlorination stone
The continuous production of wax.But disadvantage is that the mass-transfer efficiency of the first chlorine and liquid wax is not high, lead to average reaction time
More than 20h；Reaction speed is unbalanced in second entire process units, and reaction speed difference is larger in each reaction kettle, occurs
Heat of reaction cannot be removed in time or the possibility of explosive reaction, reaction controlling difficulty are big；Third is its biphase gas and liquid flow
Dynamic direction is consistent, and the reaction in rear class reaction kettle gradually tends to balance, consumption of the reaction to chlorine in tail gas in afterbody kettle
Measure limited, chlorine content is higher in tail gas.
Publication number CN102875357A discloses the chlorination tank that large-scale chlorination tank produces chloroacetic technique and its reaction,
Batch production device is formed using " two main one is secondary " three reaction kettles, liquid phase is added at one time main still and time kettle, into main still
Logical chlorine reaction, tail gas is passed through time kettle, and the reaction was continued, and deficiency is not to be able to achieve the serialization of production process and effectively improve
The speed etc. of reaction.
Summary of the invention
Absorption tower, reaction kettle and absorption kettle are utilized it is an object of the invention to overcome the deficiencies of the prior art and provide a kind of
The new equipment of combination plant continuous high-efficient production chloro thing.The device is using gas-liquid two-phase in absorption tower, reaction kettle and absorption kettle
Chloro thing is greatly decreased in the way of the mass transfer absorption of tower equipment promotion gas-liquid two-phase in internal counter-current absorption and reaction
The time is generated, so that reaction speed and thermal discharge in reaction kettle is tended to balance, as the equipment can be by the chlorinated paraffin -52 reaction time
Foreshorten to 6h or so.The device greatly reduces the generation time of chloro thing while realizing continuous production, improves production effect
Rate, and the device controllability is strong, operating flexibility is big, safety coefficient is high, the consumption of raw material reduces, and has greatly saved production operation
Cost, process units construction cost and cost of land.
The technical solution of the present invention is as follows:
Production equipment of the invention mainly includes absorption tower, reaction kettle, absorption kettle, heat exchanger and exhaust gas processing device.Benefit
First increase the characteristics of reducing afterwards with chlorination speed, continuous flow upstream reacts in production equipment using gas-liquid two-phase, and reaction exists
The fast reaction in reaction kettle after causing in absorption kettle；After carrying out reaction speed reduction with reaction, gas in tower equipment is utilized
The features such as liquid two-phase contact area is big, time of contact is long, mass-transfer efficiency is high, the material gas-liquid two being continuously transferred in absorption tower
The area that is in contact increases, and has ensured quickly generating for chloro thing.
Absorption tower lower part is equipped with inlet port and outlet port, is respectively used to as the saturation after fresh gas-phase feed and absorption gas phase
Liquid material discharging, feed inlet are connected with gas phase feed-inputing branched pipe, the feed inlet connection on discharge port and the first reaction kettle top；Top
Equipped with feed inlet and gas vent, connect respectively with the outlet of the liquid material of reaction kettle lower part and the gas feed on reaction kettle top
It connects.Absorption tower is that sieve-plate tower perhaps fill out by the optional glass filler of packed tower filler, ceramic condiment, metal packing or macromolecule
Material it is one of or several.
First reaction kettle lower part sets and is separately connected the feed inlet on absorption tower top there are two discharge port, as crude product or
The discharge port of person's decaying catalyst is connected with heat exchanger between the first reaction kettle and absorption tower；Top is set there are two feed inlet, point
It is not connect with the liquid outlet opening of absorption tower lower part, junior's kettle lower part discharge port, furthermore top is additionally provided with gas feed and gas
Outlet, connect with the gas feed of the gas vent on absorption tower top and junior's kettle respectively.
Other reaction kettle lower parts are equipped with discharge port, connect with higher level's reaction kettle upper feed inlet；Top is equipped with fresh gas phase
With liquid material feed inlet and gas feed and gas vent, respectively with gas-phase feed branch pipe, junior's kettle lower part discharge port, on
The outlet of grade kettle upper gas is connected with junior's kettle upper gas import.
Absorption kettle lower part is equipped with discharge port, connect with the feed inlet on most end first order reaction kettle top；Top is equipped with fresh liquid
Phase feed inlet, gas feed, gas vent, respectively and at fresh liquid phase material slot, reaction kettle gas vent, tail gas or product
Manage device connection.
Exhaust gas processing device is handled using three-level adverse current water scrubber and caustic wash tower, and washing lotion relies on liquid in three-level adverse current water scrubber
Potential difference nature overflow.
In above scheme, reaction kettle can be set as 1-5 according to production requirement.
In above scheme, ultraviolet lamp, fluorescent lamp or blue-ray light can be set in kettle according to the catalysis demand of reaction and urged
Change.
In above scheme, the type of cooling on absorption tower, reaction kettle and absorption kettle can be using collet cooling, external heat exchanger
It is cooling or the modes such as be used in combination.Room temperature water cooling or sub-cooled, preferred room temperature cooling can be used in collet and heat exchanger；It changes
The materials such as the optional stainless steel of hot equipment matter, enamel, graphite, preferred graphite heat exchanger.
In above scheme, the side of kettle, and the plumb line with kettle are set into the gas feed of reaction kettle and absorption kettle
It keeps 30 ° -60 ° of angle rather than is passed through vertically downward, flowed by gas phase and push material stirring in kettle and increase gas phase in kettle
The interior residence time.
In above scheme, the measuring devices such as temperature, pressure, flow, density and related control should be also set according to production needs
Control equipment.
Flow direction of material under steady production state in the device is as follows:
Gas phase enters gas phase branch pipe by gas phase general pipeline, absorption tower is respectively enterd after adjusting flow, metering and and except first
Other reaction kettles outside reaction kettle.
Liquid phase is continuously added to by the liquid phase feeding mouth on absorption kettle top, and pre-reaction occurs with unreacted gas phase in absorption kettle
Most end first order reaction kettle upper aqueous phase feed inlet is passed through by lower liquid discharge port afterwards, successively in reaction kettles at different levels with higher level's kettle
Enter absorption tower after interior unreacted gas phase and the gas phase countercurrent reaction being newly passed through, and recycles and inhale in absorption tower and the first reaction kettle
Getter phase reacts, and is liquid for product, the crude product for reacting formation is continuously gone out by the first reaction kettle lower part discharge port
Material.
The tail gas that generates or gas products enter the first reaction kettle, reaction after unreacted gas phase and reaction in absorption tower
After collect reaction gas reactor after be passed through junior's reaction kettle, then be passed through absorption kettle after successively collecting, through with fresh liquid in absorption kettle
It is passed through exhaust gas processing device after phase reaction, product collecting device is passed through for gas for product.
The invention has the following advantages:
1. realizing the serialization of production process, the Safety and Environmental Protection of device is improved.It is different from existing process units liquid phase
Material is continuously passed through gas phase after disposably feeding and is reacted, the batch production method disposably to discharge after the reaction was completed, the dress
It sets gas phase and absorption tower and reaction kettle is respectively enterd by gas phase branch pipe, liquid phase is continuously added to by absorption kettle, and flows through reaction according to this
Crude product is generated after kettle and absorption tower with gas phase reaction, crude product continuously removes out of reaction kettle and generates final products through processing.
Continuous production can greatly improve production efficiency, reduce manually-operated intensity, be conducive to reaction system and realize automation control
System, decreases operation error etc., improves the essential safety performance and environmental-protecting performance of device while saving artificial.
2. shortening the reaction time, production cost is reduced.It is passed directly into reaction kettle and occurs relative to traditional equipment gas phase
Reaction, device gas-liquid two-phase counter current contacting mass transfer in absorption tower greatly strengthen the efficiency of mass transfer；Absorbed gas phase saturation
Liquid phase stream afterwards is recycled into reaction kettle, gas-liquid two-phase fast reaction at higher temperature and catalytic condition.It absorbs and anti-
The separation of process is answered to improve the mass-transfer efficiency and reaction speed of gas-liquid two-phase, same production capacity needs less operating cost, builds
It is set as this and industrial land etc..
3. reaction speed is balanced, device it is handling strong.First increase the characteristics of reducing afterwards, gas-liquid using chlorination speed
Liquid phase is transferred in reaction kettle after pre-reaction by two-phase in absorption kettle, quick with unreacted gas phase in fresh gas phase and higher level's kettle
Reaction, with the progress of reaction, reaction speed is reduced and is transferred in absorption tower, is contacted using gas-liquid two-phase in tower equipment
The features such as area is big, time of contact is long, mass-transfer efficiency is high increases gas-liquid two-phase contact area, pushes the process of chlorination, make
The generation of chloro thing remains at fair speed.And formation speed of the chloro thing in each reaction kettle tends to balance, it is each
Heat release in reaction kettle is also more balanced, in addition, liquid phase material cools down before entering absorption tower through heat exchange, lower temperature increases
The solubility for having added gas phase, is more advantageous to the mass transfer of gas-liquid two-phase, while reducing reactivity, these all reduce appearance cannot and
When by heat of reaction remove or explosive reaction possibility, improve the operability of device.
4. reaction mass high income, by-product quality is high.Fresh liquid reactants or catalyst in absorption kettle with
Unreacted gas phase reaction in prime kettle, biggish reactant or catalyst concn promote chlorination forward direction to carry out, and to the greatest extent may be used
Energy consumes unreacted gas phase, improves the utilization rate of gas phase, improves the quality of by-product hydrochloric acid.
Detailed description of the invention
Fig. 1 is the production technological process for producing chlorinated paraffin, and Fig. 2 is chloroacetic production technological process, and Fig. 3 is chlorine
The production technological process of methane.
Specific embodiment
Continous way chloro process units of the present invention is described further by embodiment with reference to the accompanying drawing.
Embodiment 1: the production technology device of chlorinated paraffin
As shown in Figure 1, the production equipment of chlorinated paraffin mainly includes absorption tower 1, reaction kettle 2,3,4,5, absorption kettle 6 is changed
Hot device 7,8.
Glass filler tower is selected on absorption tower 1, and its underpart is equipped with chlorine feed mouth and chlorinated paraffin intermediate product (hereinafter referred to as
" chlorine wax ") outlet, be respectively used to chlorine feed and absorb chlorine after saturation chlorine wax discharging, chlorine wax outlet by circulating pump 9 with
The upper feed inlet of reaction kettle 2 connects；1 top of absorption tower be equipped with chlorine wax feed inlet and offgas outlet each one, respectively with react
The chlorine wax discharge port of 2 lower part of kettle is connected with 2 top inlet exhaust gas of reaction kettle.
Reaction kettle 2 is using collet and the joint cooling of external heat exchanger 8, and its underpart is set there are two chlorine wax discharge port, and one logical
It is connect after crossing circulating pump 10, heat exchanger 7 with the feed inlet on 1 top of absorption tower, another is outlet for product, the crude product of generation
Product chlorinated paraffin is treated as through degassing etc. after discharging；Top is set there are two feed inlet, respectively with the chlorine wax of 1 lower part of absorption tower
Discharge port, the connection of 3 lower part discharge port of reaction kettle, furthermore top is additionally provided with inlet exhaust gas and offgas outlet, respectively and on absorption tower 1
The offgas outlet in portion is connected with the inlet exhaust gas on 3 top of reaction kettle.
Reaction kettle 3,4,5 is cooling using collet, and its underpart is respectively provided with a chlorine wax discharge port, respectively by delivery pump 11,
12, it 13 is connect with upper level reaction kettle top chlorine wax feed inlet；Top be equipped with fresh chlorine and chlorine wax feed inlet, inlet exhaust gas,
Offgas outlet, respectively and on chlorine feed branch pipe, junior's kettle lower part chlorine wax discharge port, higher level's kettle top offgas outlet, junior's kettle
The connection of portion's inlet exhaust gas.
Absorption kettle 6 is cooling using collet, and its underpart is equipped with a chlorine wax discharge port, by delivery pump 14 and reaction kettle 5
The feed inlet in portion connects；Top be equipped with fresh liquid wax feed inlet, inlet exhaust gas, offgas outlet, respectively with fresh liquid wax pan, react
5 offgas outlet of kettle is connected with exhaust treatment system.
Heat exchanger 7,8 selects room temperature water cooling graphite heat exchanger；To ensure reactivity, reaction kettle 2,3,4,5 and absorption kettle 6
Inside is additionally provided with ultraviolet lamp 15,16,17,18,19 and makees catalyst；To promote the mixed effect of reaction mass and increasing chlorine in kettle
The interior residence time, inlet exhaust gas is non-perpendicular downward but 45 ° of angle is kept with the plumb line of kettle, and air-flow is made to push object in kettle
Material stirring.
The flow direction of material of the steady production state device are as follows: chlorine is connected respectively with different flow after adjusting flow, metering
It is continuous to enter absorption tower 1 and reaction kettle 3,4,5.Fresh liquid wax is continuously added to certain flow by absorption kettle 6, with identical flow according to
This, which send into reaction kettle 5,4,3,2, is reacted, and is recycled in reaction kettle 2 and absorption tower 1, reach after certain density by
2 continuous discharge of reaction kettle, is packaged as finished product chlorinated paraffin after degassed processing.The tail gas and unreacted chlorine that reaction tower 1 generates
Gas passes sequentially through reaction kettle 2,3,4,5, and is passed through absorption kettle 6, the chlorine being mingled in tail gas after collecting the gas generated in kettle on the way
Gas is reacted with fresh liquid wax, and reacted purified tail gas is passed through vent gas treatment facility or the raw material as other reactions.
Average reaction time is 6h or so when the continous way chloro process units produces chlorinated paraffin -52, produces chlorination stone
Average reaction time is 4h or so when wax -42, and the total feeding quantity of chlorine is no more than charging liquid wax theory chlorine consumption
102%, shorten 1 times or more compared with prior art average reaction time, chlorine content reduces about half in tail gas, and realizes continuous
Metaplasia produces.
Embodiment 2: chloroacetic production technology device
As shown in Fig. 2, chloroacetic production equipment mainly includes absorption tower 1, reaction kettle 2,3, absorption kettle 4, heat exchanger 5,6
And exhaust gas processing device.
Glass filler tower is selected on absorption tower 1, and its underpart is equipped with chlorine feed mouth and monoxone semi-finished product discharge port, uses respectively
In chlorine feed and the saturation monoxone semi-finished product discharging after absorption gas phase, monoxone export of goods in process of manufacture is by circulating pump 7 and instead
The upper feed inlet of kettle 2 is answered to connect；1 top of absorption tower be equipped with monoxone semi-finished product feed inlet and offgas outlet, respectively with react
The monoxone export of goods in process of manufacture of 2 lower part of kettle is connected with 2 top inlet exhaust gas of reaction kettle.
Reaction kettle 2 is set using collet and the joint cooling of external heat exchanger 6, its underpart there are two discharge port, and one by following
It is connect after ring pump 8, heat exchanger 5 with the feed inlet on 1 top of absorption tower, another is as monoxone crude product discharge port, after reaction
Monoxone crude product crystallized etc. be treated as product monoxone；Top is set there are two feed inlet, respectively with 1 lower part of absorption tower
Monoxone semi-finished product discharge port, 3 lower part discharge port of reaction kettle connection, furthermore top is additionally provided with inlet exhaust gas and offgas outlet,
It is connect respectively with the inlet exhaust gas on 3 top of the offgas outlet on 1 top of absorption tower and reaction kettle.
Reaction kettle 3 is cooling using collet, and its underpart is equipped with a monoxone semi-finished product discharge port, by delivery pump 9 and instead
2 upper feed inlet of kettle is answered to be connected；Top is equipped with fresh chlorine and monoxone semi-finished product feed inlet, inlet exhaust gas, offgas outlet, point
Not and on chlorine feed branch pipe, 4 lower part monoxone semi-finished product discharge port of absorption kettle, 2 top offgas outlet of reaction kettle, absorption kettle 4
The connection of portion's inlet exhaust gas.
Absorption kettle 4 is cooling using collet, and its underpart is equipped with a monoxone semi-finished product discharge port, by delivery pump 10 and instead
The feed inlet on 3 top of kettle is answered to connect；Top is equipped with fresh acetic acid and aceticanhydride feed inlet, inlet exhaust gas, offgas outlet, respectively and newly
Fresh acetic acid is connected with the offgas outlet of aceticanhydride material trough, 3 top of reaction kettle with exhaust gas processing device.
Heat exchanger 5,6 is using selection room temperature water cooling graphite heat exchanger；To promote the mixed effect of reaction mass and increasing chlorine
Residence time of the gas in kettle, inlet exhaust gas is non-perpendicular downward but 45 ° of angle is kept with the plumb line of kettle, pushes air-flow
Material stirring in kettle.
Embodiment 3: the production technology device of chloromethanes
As shown in figure 3, the production equipment of chloromethanes mainly includes absorption tower 1, reaction kettle 2, absorption kettle 3, heat exchanger 4.
Sieve-plate tower is selected on absorption tower 1, and its underpart is equipped with hydrogen chloride and methanol gas feed inlet and catalyst discharge port, respectively
For the catalyst discharging of the saturation after hydrogen chloride and methanol gas charging and absorption gas phase, catalyst discharge port passes through circulating pump
5 connect with the upper feed inlet of reaction kettle 2；1 top of absorption tower is equipped with catalyst feeds and product and tail gas discharge port, respectively
It is connect with the catalyst discharge port of 2 lower part of reaction kettle and 2 upper product of reaction kettle and inlet exhaust gas.
Reaction kettle 2 is cooling using collet, and its underpart sets that there are two catalyst discharge ports, passes through circulating pump 6, heat exchanger respectively
Connect after 4 with the feed inlet on 1 top of absorption tower and as decaying catalyst outlet, heat exchanger 4 is using selecting room temperature water cooling stone
Black heat exchanger；Top is set there are two feed inlet, respectively with 1 top of catalyst discharge port and absorption tower with 1 lower part of absorption tower
Product is connected with offgas outlet, and top is additionally provided with the inlet port and outlet port of product and tail gas, respectively with 1 upper outlet of absorption tower
Mouth is connected with 3 upper feed inlet of absorption kettle.
Absorption kettle 3 is cooling using collet, and lower part is equipped with catalyst discharge port, is fed by delivery pump 7 and 2 top of reaction kettle
Mouth connection；Top is equipped with catalyst feeds, product and tail gas inlet port and outlet port, product and tail gas feed inlet and reaction kettle
The connection of 2 upper part discharge ports, product and tail gas discharge port are connected with product treatment and exhaust treatment system.
To promote the mixed effect of reaction mass and increasing residence time in kettle of hydrogen chloride and methanol gas, tail gas into
Mouth is non-perpendicular downward but 45 ° of angle is kept with the plumb line of kettle, and air-flow is made to push material stirring in kettle.
Claims (7)
1. a kind of device of gas-liquid countercurrent method continuous production chloro thing, it is characterised in that be able to achieve chlorinated paraffin, monoxone, chloromethane
The serialization of the chloro things such as alkane production, shortens the reaction time, improves production efficiency and product yield, realizes reaction in each reaction kettle
The relative equilibrium of speed and thermal discharge, the control performance of intensified response, the device include absorption tower, reaction kettle, absorption kettle, heat exchange
Device and exhaust gas processing device, absorption tower are connect by pipeline with reaction kettle, can be equipped with heat exchanger between the two, be connected after reaction kettle
There are absorption kettle, gas products collection or exhaust gas processing device；
Gas phase continuously enters absorption tower and reaction kettle respectively under steady production state；Liquid phase is continuously added to by absorption kettle, and not anti-
It is countercurrently passed through reaction kettle and absorption tower after the gas phase pre-reaction answered, cyclic absorption gas phase, hair in absorption tower and the first reaction kettle
Raw reaction, and the catalyst through the first reaction kettle continuous discharge liquid crude product or inactivation；The gas formed in absorption tower is raw
Enter absorption kettle, warp after successively collecting gaseous products and unreacted gas phase in each reaction kettle at object and unreacted gas phase
Vent gas treatment or gas products collection device are removed after pre-reaction.
2. the device of gas-liquid countercurrent method continuous production chloro thing according to claim 1, it is characterised in that absorption tower is sieve
Perhaps packed tower filler selects the one of or several of glass filler, ceramic packing, metal packing or polymer carrier to plate tower
Kind.
3. the device of gas-liquid countercurrent method continuous production chloro thing according to claim 1, it is characterised in that reaction kettle quantity
It is 1-5.
4. the device of gas-liquid countercurrent method continuous production chloro thing according to claim 1, root is it is characterized in that according to reaction
Catalysis demand can set ultraviolet lamp, fluorescent lamp or blue-ray light etc. in reaction kettle and absorption kettle and is catalyzed.
5. the device of gas-liquid countercurrent method continuous production chloro thing according to claim 1, it is characterised in that absorption tower, reaction
The type of cooling of kettle and absorption kettle can use the modes such as collet is cooling, external heat exchanger is cooling or is used in combination；Collet and
Room temperature water cooling or sub-cooled, preferred room temperature cooling can be used in heat exchanger；The optional stainless steel of heat exchanger material, enamel, graphite
Equal materials, preferred graphite heat exchanger.
6. the device of gas-liquid countercurrent method continuous production chloro thing according to claim 1, it is characterised in that enter reaction kettle
The side of kettle is set with the inlet exhaust gas of absorption kettle, and with the plumb line of kettle keep 30 ° -60 ° angle rather than vertically downward
It is passed through, is flowed by gas phase and push material stirring in kettle and increase residence time of the gas phase in kettle.
7. the device of gas-liquid countercurrent method continuous production chloro thing according to claim 1, it is characterised in that can be according to production
Need to be arranged the measuring devices such as temperature, pressure, flow, density and related control device.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114904464A (en) * | 2022-05-11 | 2022-08-16 | 上海华谊（集团）公司 | Reaction system for gas-liquid phase reaction and use thereof |
| CN116078292A (en) * | 2021-11-08 | 2023-05-09 | 中化蓝天集团有限公司 | Synthesis reactor of lithium hexafluorophosphate, continuous synthesis reaction system and process |
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| CN105154136A (en) * | 2015-07-14 | 2015-12-16 | 马春磊 | Production method and equipment for chlorinated paraffin |
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| CN105154136A (en) * | 2015-07-14 | 2015-12-16 | 马春磊 | Production method and equipment for chlorinated paraffin |
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| W.雷斯尼克: "《化工过程分析与设计》", 31 December 1985, 化学工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116078292A (en) * | 2021-11-08 | 2023-05-09 | 中化蓝天集团有限公司 | Synthesis reactor of lithium hexafluorophosphate, continuous synthesis reaction system and process |
| CN114904464A (en) * | 2022-05-11 | 2022-08-16 | 上海华谊（集团）公司 | Reaction system for gas-liquid phase reaction and use thereof |
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