CN201793508U - Device for producing dichloroethane - Google Patents

Device for producing dichloroethane Download PDF

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Publication number
CN201793508U
CN201793508U CN 201020292359 CN201020292359U CN201793508U CN 201793508 U CN201793508 U CN 201793508U CN 201020292359 CN201020292359 CN 201020292359 CN 201020292359 U CN201020292359 U CN 201020292359U CN 201793508 U CN201793508 U CN 201793508U
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China
Prior art keywords
stirring
inlet
still
reaction
condenser
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Expired - Lifetime
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CN 201020292359
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Chinese (zh)
Inventor
崔巍
袁茂全
陈斌武
胡妹华
马斌全
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Shanghai Chlor Alkali Chemical Co Ltd
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Shanghai Chlor Alkali Chemical Co Ltd
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Abstract

The utility model relates to a device for producing dichloroethane. The device comprises a stirring and preheating kettle, a pre-reaction packing tower provided with a first condenser at the top, and n stirring absorption kettles connected in series and provided with second condensers at the tops, wherein, n is an integer greater than or equal to 1 and smaller than or equal to 5; an initiator inlet and a 1,2-dichloroethane inlet are formed at the top of the stirring and preheating kettle; a fixed liquid raw material outlet of the stirring and preheating kettle is connected with a pre-reaction raw material inlet; a circulating gas inlet is formed at the bottom of the pre-reaction packing tower; the product outlet of the pre-reaction packing tower is connected with the inlet of the first stirring absorption kettle; the vapor phase outlets of the stirring absorption kettles are connected with the gas inlet of the first condenser; a chlorine gas inlet is formed at the bottom of each stirring absorption kettle; a reaction product outlet is formed at the upper part of each stirring absorption kettle; and the gas outlets of the second condensers are connected with the circulating gas inlet of the pre-reaction packing tower. The utility model has the advantages of improved utilization ratio of raw materials, less three-waste, great reduction of energy consumption and unit consumption, and suitability of industrial production.

Description

Produce the device of trichloroethane
Technical field
The utility model relates to the device of producing trichloroethane.
Background technology
Trichloroethane, especially vinyl trichloride are a kind of important organic intermediates, can be used for producing vinylidene chloride (VDC) monomer.Preparation of industrialization 1,1, the method of 2-trichloroethane mainly contains vinylchlorid (VCM) chlorination process and ethylene dichloride (EDC) chlorination process, because VCM chlorination process mild condition, the technology comparative maturity, domestic manufacturer nearly all adopts this route, the relevant patent of application has CN1440959A, CN1793093A, CN02127809.11, CN200510111981.8 etc., but lasting high along with international oil price in recent years, production cost is constantly soaring, and therefore, the EDC chlorination process is because of its raw materials cost advantage, become trend of the times, all eliminate the VCM chlorination process abroad and use the EDC chlorination process instead, having introduced rayed as patent US2174737 brings out 1, and the chlorination of 2-ethylene dichloride generates 1,1,2-trichloroethane, patent US2140549 have been introduced gas phase ethylene dichloride and chlorine have been passed through melt metal muriate (iron, sodium, zinc, aluminium etc.) produce 1,1, the 2-trichloroethane, patent US3173963 and US3344197 metal chloride (FeCl 3) be catalyzer, ethene and chlorine are introduced 1,2-ethylene dichloride and 1,1,2 trichloroethane mixed solutions are to generate 1 in the reactor of medium, 1,2-trichloroethane, patent US3919337 have been introduced a kind of catalyzer that do not use, under higher temperature and pressure by 1,2-ethylene dichloride direct chlorination generates the method for vinyl trichloride.More than the shortcoming of these methods be that the selectivity of reaction is relatively poor, side reaction is many, causes the difficulty of later separation, the equipment that has is very complicated, is not suitable for large-scale industrial production.
Applicant's patent CN200510029868.5, produce 1 in development on the basis of U.S. Pat 2621153 and the perfect reaction rectification method that uses under the catalyst-free condition, 1, the technology of 2-trichloroethane, operational condition is reaction pressure 0.1MPa, tower still Heating temperature is about 114 ℃, higher transformation efficiency and selectivity have been obtained, but the shortcoming of reactive distillation is also very obvious, because 1,2-ethylene dichloride chlorination reaction velocity is slower, under above-mentioned operational condition, stripping section has a large amount of unreacted 1 in the reaction fractionating tower, the 2-ethylene dichloride becomes gas phase, for reducing loss of material, need it be cooled off at rectifying section, cause a large amount of energy consumptions thus, and treatment capacity can only maintain lower level, according to the embodiment in the patent, in virtual height is 4 meters reaction fractionating tower, 1, the input speed of 2-ethylene dichloride is the highest has only 0.15 kilogram/hour, though transformation efficiency and selection rate reach 96.2% and 93% respectively, the output of its vinyl trichloride also has only 0.18 kilogram/hour, if be amplified to industrially scalable, the liquid holdup of reaction fractionating tower and energy consumption will be very huge.
Summary of the invention
The purpose of this utility model provides a kind of device of producing trichloroethane, to overcome the above-mentioned defective that prior art exists.
The device of production trichloroethane of the present utility model comprises that stirring still preheater, top are provided with the pre-reaction packing tower of first condenser and the stirring absorption still that is connected in series that the top is provided with second condenser 4; N is 1~5 integer;
The top of described stirring still preheater is provided with initiator inlet and 1,2-ethylene dichloride inlet, the mixing raw material liquid outlet of stirring still preheater is connected with the pre-reaction feed(raw material)inlet that is arranged on pre-reaction packing tower middle part by pump, pre-reaction packing tower bottom is provided with the circulation gas inlet, the product outlet of pre-reaction packing tower bottom is stirred the inlet that absorbs still by pipeline and first and is connected, the gaseous phase outlet that stirs the top that absorbs still is connected with the gas inlet of first condenser, the chlorine inlet is arranged on and stirs the bottom that absorbs still, reacting product outlet is arranged on and stirs the top that absorbs still, and the pneumatic outlet of second condenser is connected with the circulation gas inlet of the tower still bottom of pre-reaction packing tower;
Device of the present utility model, operational path is fairly simple, and whole process is carried out under normal pressure, and temperature of reaction is lower, significantly reduced 1, the condensation number of 2-ethylene dichloride steam, multistage absorption makes 1, and the utilization ratio of 2-ethylene dichloride improves, the three wastes are less, energy consumption and unit consumption all are significantly reduced, and the stability of technology and ease for operation are also strengthened to some extent, are suitable for commercial scale production.
Description of drawings
Fig. 1 is the structural representation of device.
Embodiment
Referring to Fig. 1, the device of production trichloroethane of the present utility model comprises that stirring still preheater 1, top are provided with the pre-reaction packing tower 2 of first condenser 204 and the n that is connected in series the stirring absorption still 3 that the top is provided with second condenser 4;
N is 1~5 integer, and preferred, n is 2;
The top of described stirring still preheater 1 is provided with initiator inlet and 1,2-ethylene dichloride inlet, the mixing raw material liquid outlet of stirring still preheater 1 is connected with the pre-reaction feed(raw material)inlet 201 that is arranged on pre-reaction packing tower 2 middle parts by pump 5, pre-reaction packing tower 2 bottoms are provided with circulation gas inlet 203, the product outlet 202 of pre-reaction packing tower 2 bottoms is stirred the inlet 301 that absorbs still 3 by pipeline and first and is connected, the gaseous phase outlet 302 that stirs the top that absorbs still 3 is connected with the gas inlet of first condenser 304, chlorine inlet 303 is arranged on and stirs the bottom that absorbs still 3, reacting product outlet 304 is arranged on and stirs the top that absorbs still 3, and the pneumatic outlet of second condenser 4 is connected with the circulation gas inlet 203 of the tower still bottom of pre-reaction packing tower 2;
Further, the top of described stirring still preheater 1 is provided with raw material condenser 103;
For guaranteeing the stable of discharging, adjacent two stir the gaseous phase outlet pipe that absorbs still is interconnected;
Stir absorption still 3 and can use anchor formula stirring rake, also can adopt Rushton stirring rake, turbine oar or MULTILAYER COMPOSITE stirring rake.
Device of the present utility model can the continuous production vinyl trichloride, and production method comprises the steps: 1, and 2-ethylene dichloride and initiator add and stir in the still preheater 1, preheating, and 1 of evaporation, the 2-ethylene dichloride is by raw material condenser 103 condensing refluxes;
Mixed stock liquid is sent into pre-reaction packing tower 2 by pump 5 from the middle part, react with circulation gas inlet 203 chlorine that enter, 1 of HCl, non-condensable gases and the evaporation that generates, the 2-ethylene dichloride, after 204 condensations of first condenser, the liquid phase total reflux enters in the tower, and gas phase is sent to vent gas treatment workshop section;
The bottom product of pre-reaction packing tower 2, enter n the stirring that is connected in series and absorb still 3, chlorine is entered to stir by chlorine inlet 303 and absorbs still 3, under action of evocating with 1, the reaction of 2-ethylene dichloride, 1 of HCl, non-condensable gases, unreacted chlorine and the evaporation that generates, the 2-ethylene dichloride, enter 4 condensations of second condenser by gaseous phase outlet 302, the liquid phase total reflux, gas phase feeds pre-reaction packing tower 2 by circulation gas inlet 203, contains 1,1, the reaction product of 2-trichloroethane is discharged by reacting product outlet 304.
Described initiator is dioxygen class or azo compound, preferably, initiator comprises dibenzoyl peroxide, peroxidized t-butyl perbenzoate, tertbutyl peroxide, dicumyl peroxide, Cellmic C 121, diisopropyl azodiformate, Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile) or 2,2'-Azobis(2,4-dimethylvaleronitrile) etc.

Claims (5)

1. produce the device of trichloroethane, it is characterized in that, comprise that stirring still preheater (1), top are provided with the pre-reaction packing tower (2) of first condenser (204) and the n that is connected in series the stirring absorption still (3) that the top is provided with second condenser (4), n is 1~5 integer;
The top of described stirring still preheater (1) is provided with initiator inlet and 1,2-ethylene dichloride inlet, the mixing raw material liquid outlet of stirring still preheater (1) is connected with the pre-reaction feed(raw material)inlet (201) that is arranged on pre-reaction packing tower (2) middle part by pump (5), pre-reaction packing tower (2) bottom is provided with circulation gas inlet (203), the product outlet (202) of pre-reaction packing tower (2) bottom is stirred the inlet (301) that absorbs still (3) by pipeline and first and is connected, the gaseous phase outlet (302) that stirs the top that absorbs still (3) is connected with the gas inlet of first condenser (304), chlorine inlet (303) is arranged on and stirs the bottom that absorbs still (3), reacting product outlet (304) is arranged on and stirs the top that absorbs still (3), and the pneumatic outlet of second condenser (4) is connected with the circulation gas inlet (203) of the tower still bottom of pre-reaction packing tower (2).
2. the device of production trichloroethane according to claim 1 is characterized in that, n is 2.
3. the device of production trichloroethane according to claim 1 is characterized in that, the top of described stirring still preheater (1) is provided with raw material condenser (103).
4. the device of production trichloroethane according to claim 1 is characterized in that, adjacent two stir the gaseous phase outlet pipe that absorbs still is interconnected.
5. according to the device of each described production trichloroethane of claim 1~4, it is characterized in that, stir absorption still (3) and use anchor formula stirring rake, Rushton stirring rake, turbine oar or MULTILAYER COMPOSITE stirring rake.
CN 201020292359 2010-08-12 2010-08-12 Device for producing dichloroethane Expired - Lifetime CN201793508U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201020292359 CN201793508U (en) 2010-08-12 2010-08-12 Device for producing dichloroethane

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Application Number Priority Date Filing Date Title
CN 201020292359 CN201793508U (en) 2010-08-12 2010-08-12 Device for producing dichloroethane

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CN201793508U true CN201793508U (en) 2011-04-13

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103157425A (en) * 2011-12-13 2013-06-19 中国科学院大连化学物理研究所 Continuous production device for catalytic reaction by adopting phase transfer catalyst

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103157425A (en) * 2011-12-13 2013-06-19 中国科学院大连化学物理研究所 Continuous production device for catalytic reaction by adopting phase transfer catalyst
CN103157425B (en) * 2011-12-13 2015-01-07 中国科学院大连化学物理研究所 Continuous production device for catalytic reaction by adopting phase transfer catalyst

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Granted publication date: 20110413