CN107857695A - The apparatus and method for improving 2 propoxyl group chloroethanes yields of production - Google Patents
The apparatus and method for improving 2 propoxyl group chloroethanes yields of production Download PDFInfo
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- CN107857695A CN107857695A CN201711242912.XA CN201711242912A CN107857695A CN 107857695 A CN107857695 A CN 107857695A CN 201711242912 A CN201711242912 A CN 201711242912A CN 107857695 A CN107857695 A CN 107857695A
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- thionyl chloride
- pipeline
- propoxyl group
- circulating tank
- tower
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/18—Preparation of ethers by reactions not forming ether-oxygen bonds
- C07C41/22—Preparation of ethers by reactions not forming ether-oxygen bonds by introduction of halogens; by substitution of halogen atoms by other halogen atoms
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of apparatus and method for improving 2 propoxyl group chloroethanes yields of production, belong to field of chemical equipment, including chlorine ether reactor, condenser, gas-liquid separator, thionyl chloride absorption plant and cyclone separator；The thionyl chloride absorption plant includes thionyl chloride circulating tank, circulating pump and caught except tower；Catch except tower bottom connection thionyl chloride circulating tank；Thionyl chloride circulating tank liquid outlet connects circulating pump, and circulation pump output terminal connects the first pipeline and the second pipeline respectively, and the connection of the first pipeline is caught except top of tower, at the top of the second pipeline connection chlorine ether reactor.Raw material and product the thionyl chloride dissolving carried secretly in tail gas recycle, and improve the yield of 2 propoxyl group chloroethanes, while thionyl chloride recycles, and saves operating procedure.
Description
Technical field
The present invention relates to a kind of apparatus and method for improving production 2- propoxyl group chloroethanes yields, belong to chemical industry equipment neck
Domain.
Background technology
2- propoxyl group chloroethanes is to prepare one of important source material of herbicide pretilachlor, the herbicide as low toxicity, spectrum,
Efficient major choice herbicide, is widely used, extensive market, domestic and international demand is big in Rice Cropping field.
At present, 2- propoxyl group chloroethanes is prepared mainly using ethylene glycol propyl ether as initiation material, using different chlorinating agents
By its hydroxy chloride generation.During the course of the reaction, part finished product 2- propoxyl group chloroethanes and raw material ethylene glycol propyl ether can be with tail gas
Enter together in exhaust treatment system, cause the yield of product to decline.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of improve to produce 2- propoxyl group chloroethanes yields
Device, improve product yield；There is provided method simultaneously.
A kind of device for improving production 2- propoxyl group chloroethanes yields of the present invention, including chlorine ether reactor, condensation
Device, gas-liquid separator, thionyl chloride absorption plant and cyclone separator；
The thionyl chloride absorption plant includes thionyl chloride circulating tank, circulating pump and caught except tower；Catch except tower bottom connects
Thionyl chloride circulating tank；Thionyl chloride circulating tank liquid outlet connect circulating pump, circulation pump output terminal connect respectively the first pipeline and
Second pipeline, the connection of the first pipeline are caught except top of tower, and at the top of the second pipeline connection chlorine ether reactor, the second pipeline is provided with flow
Meter and valve；
It is connected at the top of chlorine ether reactor with condenser overhead, at the top of condenser bottom connection gas-liquid separator, gas-liquid separation
With being connected at the top of chlorine ether reactor, gas-liquid separator is caught except top of tower and cyclone separator with catching except tower side is connected for device bottom
It is connected, at the top of cyclone separator bottom connection circulating tank, is connected at the top of cyclone separator with exhaust treatment system.
A kind of method for improving production 2- propoxyl group chloroethanes yields of the present invention, comprises the following steps：
1) ethylene glycol propyl ether is reacted with thionyl chloride in chlorine ether reactor, and the condensed device condensation of tail gas is laggard
Enter gas-liquid separator, gained liquid phase material, which enters in chlorine ether reactor, to be recycled, and gaseous phase materials, which enter, catches except in tower；
2) circulation fluid in thionyl chloride circulating tank is drawn through the first Pipeline transport to catching except in tower, catching and remove by circulating pump
The 2- propoxyl group chloroethanes and ethylene glycol propyl ether carried secretly in gaseous phase materials obtain secondary gas gas-phase objects into thionyl chloride circulating tank
Material；
3) for secondary gaseous phase materials after cyclone separator separates, the thionyl chloride of entrainment enters thionyl chloride circulating tank
In, circulation fluid is entered in chlorine ether reactor by the second pipeline through circulating pump and recycled in thionyl chloride circulating tank, passes through valve
Gate control circulation fluid rate of addition, pass through flowmeter metered application circulation fluid.
Thionyl chloride circulating tank in cyclone separator with being passed through refrigerant, and temperature control is at 0-5 DEG C.
The temperature control of chlorine ether reactor is at 90-100 DEG C.
The mass ratio of ethylene glycol propyl ether and thionyl chloride is 1 in chlorine ether reactor:1.2-1.3.
Compared with prior art, the present invention has advantages below：
The raw material and product thionyl chloride carried secretly in tail gas recycle to dissolving, improve 2- propoxyl group chloroethanes
Yield, yield bring up to 98.9% by 98.5%；Thionyl chloride recycles simultaneously, saves operating procedure.
Brief description of the drawings
Fig. 1 is the schematic device of the raising production 2- propoxyl group chloroethanes yields of the present invention.
In figure：1st, chlorine ether reactor；2nd, condenser；3rd, gas-liquid separator；4th, catch except tower；5th, thionyl chloride circulating tank；6、
Circulating pump；7th, the first pipeline；8th, the second pipeline；9th, flowmeter；10th, valve；11st, cyclone separator；12nd, exhaust treatment system.
Embodiment
With reference to embodiment, the present invention will be further described.
As shown in figure 1, a kind of device of raising production 2- propoxyl group chloroethanes yields of the present invention, including chlorine ether reactor
1st, condenser 2, gas-liquid separator 3, thionyl chloride absorption plant and cyclone separator 11；
The thionyl chloride absorption plant includes thionyl chloride circulating tank 5, circulating pump 6 and caught except tower 4；Catch and remove the bottom of tower 4
Connect thionyl chloride circulating tank 5；The liquid outlet of thionyl chloride circulating tank 5 connects circulating pump 6, and the output end of circulating pump 6 connects the respectively
One pipeline 7 and the second pipeline 8, the connection of the first pipeline 7 are caught except the top of tower 4, the second pipeline 7 are connected at the top of chlorine ether reactor 1, and second
Pipeline is provided with flowmeter 9 and valve 10；
The top of chlorine ether reactor 1 is connected with the top of condenser 2, the top of the bottom of condenser 2 connection gas-liquid separator 3, gas-liquid
The bottom of separator 3 is connected with the top of chlorine ether reactor 1, and gas-liquid separator 3 is caught except the top of tower 4 and rotation with catching except the side of tower 4 is connected
Wind separator 11 is connected, the top of the bottom of cyclone separator 11 connection thionyl chloride circulating tank 5, the top of cyclone separator 11 and tail gas
Processing system 12 is connected.
Embodiment 1
A kind of method of raising production 2- propoxyl group chloroethanes yields of the present invention, comprises the following steps：
1) ethylene glycol propyl ether and thionyl chloride in mass ratio 1:1.2 are reacted in chlorine ether reactor 1, and temperature is
90 DEG C, the condensed device 2 of tail gas enters gas-liquid separator 3 after condensing, and gained liquid phase material enters in chlorine ether reactor 1 to circulate and made
With gaseous phase materials, which enter, catches except in tower 4；
2) circulation fluid in thionyl chloride circulating tank 5 is drawn through the first pipeline 7 and is delivered to by circulating pump 6 catches except in tower 4,
Catch except the 2- propoxyl group chloroethanes and ethylene glycol propyl ether carried secretly in gaseous phase materials are into thionyl chloride circulating tank 5, obtain secondary
Gaseous phase materials；
3) for secondary gaseous phase materials after the separation of cyclone separator 11, remaining thionyl chloride enters thionyl chloride circulating tank
In 5, circulation fluid is entered in chlorine ether reactor 1 by the second pipeline 8 through circulating pump 6 and recycled in thionyl chloride circulating tank 5；It is logical
Cross valve 10 and control rate of addition, by the metered application circulating fluid volume of flowmeter 9, reach mass ratio 1:Control valve is closed down after 1.1
10, until reacting emission-free stopping.
Wherein, the temperature control of thionyl chloride circulating tank 5 and cyclone separator 11 is at 0 DEG C.
2- propoxyl group chloroethanes yield is 98.91%.
Embodiment 2
A kind of method of raising production 2- propoxyl group chloroethanes yields of the present invention, comprises the following steps：
1) ethylene glycol propyl ether and thionyl chloride in mass ratio 1:1.3 are reacted in chlorine ether reactor 1, and temperature is
55 DEG C, the condensed device 2 of tail gas enters gas-liquid separator 3 after condensing, and gained liquid phase material enters in chlorine ether reactor 1 to circulate and made
With gaseous phase materials, which enter, catches except in tower 4；
2) circulation fluid in thionyl chloride circulating tank 5 is drawn through the first pipeline 7 and is delivered to by circulating pump 6 catches except in tower 4,
Catch except the 2- propoxyl group chloroethanes and ethylene glycol propyl ether carried secretly in gaseous phase materials are into thionyl chloride circulating tank 5, obtain secondary
Gaseous phase materials；
3) for secondary gaseous phase materials after the separation of cyclone separator 11, remaining thionyl chloride enters thionyl chloride circulating tank
In 5, circulation fluid is entered in chlorine ether reactor 1 by the second pipeline 8 through circulating pump 6 and recycled in thionyl chloride circulating tank 5；It is logical
Cross valve 10 and control rate of addition, by the metered application circulating fluid volume of flowmeter 9, reach mass ratio 1:Control valve is closed down after 1.3
10, until reacting emission-free stopping.
Wherein, the temperature control of thionyl chloride circulating tank 5 and cyclone separator 11 is at 3 DEG C.
2- propoxyl group chloroethanes yield is 98.93%.
Embodiment 3
A kind of method of raising production 2- propoxyl group chloroethanes yields of the present invention, comprises the following steps：
1) ethylene glycol propyl ether and thionyl chloride in mass ratio 1:1.3 are reacted in chlorine ether reactor 1, and temperature is
55 DEG C, the condensed device 2 of tail gas enters gas-liquid separator 3 after condensing, and gained liquid phase material enters in chlorine ether reactor 1 to circulate and made
With gaseous phase materials, which enter, catches except in tower 4；
2) circulation fluid in thionyl chloride circulating tank 5 is drawn through the first pipeline 7 and is delivered to by circulating pump 6 catches except in tower 4,
Catch except the 2- propoxyl group chloroethanes and ethylene glycol propyl ether carried secretly in gaseous phase materials are into thionyl chloride circulating tank 5, obtain secondary
Gaseous phase materials；
3) for secondary gaseous phase materials after the separation of cyclone separator 11, remaining thionyl chloride enters thionyl chloride circulating tank
In 5, circulation fluid is entered in chlorine ether reactor 1 by the second pipeline 8 through circulating pump 6 and recycled in thionyl chloride circulating tank 5；It is logical
Cross valve 10 and control rate of addition, by the metered application circulating fluid volume of flowmeter 9, reach mass ratio 1:Control valve is closed down after 1.5
10, until reacting emission-free stopping.
Wherein, the temperature control of thionyl chloride circulating tank 5 and cyclone separator 11 is at 5 DEG C.
2- propoxyl group chloroethanes yield is 98.91%.
Claims (6)
- A kind of 1. device for improving production 2- propoxyl group chloroethanes yields, it is characterised in that：Including chlorine ether reactor (1), condenser (2), gas-liquid separator (3), thionyl chloride absorption plant and cyclone separator (11)；The thionyl chloride absorption plant includes thionyl chloride circulating tank (5), circulating pump (6) and caught except tower (4)；Catch and remove tower (4) Bottom connection thionyl chloride circulating tank (5)；Thionyl chloride circulating tank (5) liquid outlet connection circulating pump (6), circulating pump (6) output End connects the first pipeline (7) and the second pipeline (8) respectively, and the first pipeline (7) connection is caught except at the top of tower (4), the second pipeline (7) is even Connect at the top of chlorine ether reactor (1), the second pipeline is provided with flowmeter (9) and valve (10)；With being connected at the top of condenser (2) at the top of chlorine ether reactor (1), at the top of condenser (2) bottom connection gas-liquid separator (3), With being connected at the top of chlorine ether reactor (1), gas-liquid separator (3) is caught with catching except tower (4) side is connected for gas-liquid separator (3) bottom Except being connected at the top of tower (4) with cyclone separator (11), cyclone separator (11) bottom is connected at the top of thionyl chloride circulating tank (5).
- 2. the device according to claim 1 for improving production 2- propoxyl group chloroethanes yields, it is characterised in that：Cyclonic separation It is connected at the top of device (11) with exhaust treatment system (12).
- A kind of 3. method for improving production 2- propoxyl group chloroethanes yields, it is characterised in that：Comprise the following steps：1) ethylene glycol propyl ether is reacted with thionyl chloride in chlorine ether reactor (1), after the condensed device of tail gas (2) condensation Into gas-liquid separator (3), gained liquid phase material, which enters in chlorine ether reactor (1), to be recycled, and gaseous phase materials, which enter, catches except tower (4) in；2) circulation fluid in thionyl chloride circulating tank (5) is drawn through the first pipeline (7) and is delivered to by circulating pump (6) catches except tower (4) in, catch except the 2- propoxyl group chloroethanes and ethylene glycol propyl ether carried secretly in gaseous phase materials enter thionyl chloride circulating tank (5) In, obtain secondary gaseous phase materials；3) for secondary gaseous phase materials after cyclone separator (11) separation, the thionyl chloride of entrainment enters thionyl chloride circulating tank (5) in, circulation fluid is entered in chlorine ether reactor (1) through circulating pump (6) by the second pipeline (8) in thionyl chloride circulating tank (5) Recycle, circulation fluid rate of addition is controlled by valve (10), passes through flowmeter (9) metered application circulation fluid.
- 4. the method according to claim 3 for improving production 2- propoxyl group chloroethanes yields, it is characterised in that：Thionyl chloride Circulating tank (5) in cyclone separator (11) with being passed through refrigerant, and temperature control is at 0-5 DEG C.
- 5. the method according to claim 3 for improving production 2- propoxyl group chloroethanes yields, it is characterised in that：Chlorine ether reacts The temperature control of kettle (1) is at 90-100 DEG C.
- 6. the method according to claim 3 for improving production 2- propoxyl group chloroethanes yields, it is characterised in that：Chlorine ether reacts The mass ratio of ethylene glycol propyl ether and thionyl chloride is 1 in kettle (1):1.2-1.3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711242912.XA CN107857695B (en) | 2017-11-30 | 2017-11-30 | Device and method for improving yield of 2-propoxyl chloroethane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711242912.XA CN107857695B (en) | 2017-11-30 | 2017-11-30 | Device and method for improving yield of 2-propoxyl chloroethane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107857695A true CN107857695A (en) | 2018-03-30 |
| CN107857695B CN107857695B (en) | 2020-07-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201711242912.XA Active CN107857695B (en) | 2017-11-30 | 2017-11-30 | Device and method for improving yield of 2-propoxyl chloroethane |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116102408A (en) * | 2022-12-14 | 2023-05-12 | 首建科技有限公司 | Continuous synthesis process of 2-chloroethyl propyl ether and tail gas recovery process thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105348050A (en) * | 2015-12-14 | 2016-02-24 | 山东凯盛新材料有限公司 | Production process of 2-propoxy-chloroethane |
| WO2016202894A1 (en) * | 2015-06-17 | 2016-12-22 | Universitaet Des Saarlandes | Method of converting alcohol to halide |
| CN106310875A (en) * | 2015-07-01 | 2017-01-11 | 启东久星化工有限公司 | System for separating organic matter from mixture of hydrogen chloride and organic matter |
-
2017
- 2017-11-30 CN CN201711242912.XA patent/CN107857695B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016202894A1 (en) * | 2015-06-17 | 2016-12-22 | Universitaet Des Saarlandes | Method of converting alcohol to halide |
| CN106310875A (en) * | 2015-07-01 | 2017-01-11 | 启东久星化工有限公司 | System for separating organic matter from mixture of hydrogen chloride and organic matter |
| CN105348050A (en) * | 2015-12-14 | 2016-02-24 | 山东凯盛新材料有限公司 | Production process of 2-propoxy-chloroethane |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116102408A (en) * | 2022-12-14 | 2023-05-12 | 首建科技有限公司 | Continuous synthesis process of 2-chloroethyl propyl ether and tail gas recovery process thereof |
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| Publication number | Publication date |
|---|---|
| CN107857695B (en) | 2020-07-10 |
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