CN109970522A - A kind of deacidification technique in 2- chloroethyl propyl ether production process - Google Patents
A kind of deacidification technique in 2- chloroethyl propyl ether production process Download PDFInfo
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- CN109970522A CN109970522A CN201711452527.8A CN201711452527A CN109970522A CN 109970522 A CN109970522 A CN 109970522A CN 201711452527 A CN201711452527 A CN 201711452527A CN 109970522 A CN109970522 A CN 109970522A
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- propyl ether
- chloroethyl propyl
- chloroethyl
- thionyl chloride
- deacidification
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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
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
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- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses the deacidification techniques in a kind of 2- chloroethyl propyl ether production process, it is characterized in that, deacidification technique needs two-step process: (1) removal for thionyl chloride or other chlorinating agents production 2- chloroethyl propyl ether and other Related product middle acid substances；(2) acidic materials of 2- chloroethyl propyl ether and Related product are removed by physical methods such as decompression, flash distillation, condensation, separation；Wherein, the air pressure of decompression is -0.06MPa；The temperature of flash distillation is 50 DEG C；In separation process in terms of CL-, acidity≤0.03 of 2- chloroethyl propyl ether.The depickling distillation technique of 2- chloroethyl propyl ether of the invention is compared with traditional alkali washing process, not only in terms of economic, environmental protection with greater advantage, but also simple process, low in cost, energy conservation and environmental protection.
Description
Technical field
The present invention relates to 2- chloroethyl propyl ether technical field, more particularly to a kind of 2- chloroethyl propyl ether is raw
Deacidification technique during production.
Background technique
2- chloroethyl propyl ether is to prepare one of primary raw material of herbicide pretilachlor, which is a kind of efficient, low
The rice field major selection preemergence herbicide of poison, early stage wide spectrum.The production of 2- chloroethyl propyl ether at present mainly with ethylene glycol just
Propyl ether is primary raw material, carries out chlorine substitution reaction with it using different chlorinating agents and forms.
1, the mainly cheap excessive thionyl chloride of present 2- chloroethyl propyl ether industrialized production and ethylene glycol positive propyl ether
Based on synthesis.
2,2- chloroethyl propyl ether is synthesized by the above method at present, after completion of the reaction, due to using excessive chlorination
Sulfoxide and generation volume SO2, HCL presence so that material acidity is bigger than normal, reduce acidity conventional method be using alkali washing process,
Unreacted thionyl chloride is set to be hydrolyzed into SO2, HCL, and then react with NaOH and to generate NaCL, Na2SO3、H2O。
By the mixed solution of NaCL, Na2SO3 obtained by the above method, treatment process is cumbersome, higher cost, and washes
2- chloroethyl propyl ether in part is soluble in water in the process, so that 2- chloroethyl propyl ether yield reduces.
Therefore, how to provide it is a kind of not only in terms of economic, environmental protection with greater advantage, but also simple process, cost
Deacidification technique in cheap, energy-saving and environment-friendly 2- chloroethyl propyl ether production process is asking for those skilled in the art's urgent need to resolve
Topic.
Summary of the invention
In view of this, the present invention provides it is a kind of not only in terms of economic, environmental protection with greater advantage, but also technique is simple
Deacidification technique in single, low in cost, energy-saving and environment-friendly 2- chloroethyl propyl ether production process.
To achieve the above object, the invention provides the following technical scheme:
Deacidification technique in a kind of 2- chloroethyl propyl ether production process, which is characterized in that deacidification technique needs two-step process:
(1) removal for thionyl chloride or other chlorinating agents production 2- chloroethyl propyl ether and other Related product middle acid substances；
(2) acidic materials of 2- chloroethyl propyl ether and Related product are removed by physical methods such as decompression, flash distillation, condensation, separation；Its
In, the air pressure of decompression is -0. 06MPa；The temperature of flash distillation is 50 DEG C；With CL in separation process—Meter, 2- chloroethyl propyl ether
Acidity≤0.03.
Preferably, in the deacidification technique in a kind of above-mentioned 2- chloroethyl propyl ether production process, specific process
Are as follows:
A, after with excessive thionyl chloride and ethylene glycol positive propyl ether synthesis 2- chloroethyl propyl ether, in deacidification, by 2- chlorine
Ethyl propyl ether, unreacted thionyl chloride and the SO being dissolved in liquid material2, enter distillation still after HCL gas pressurized
Interior efficient distributor is dispersed, and is depressurized, flashed in it, make thionyl chloride vaporize and with SO2, HCL gas one
It rises and is separated with 2- chloroethyl propyl ether；
B, the thionyl chloride after vaporization passes through condensation liquefaction, makes liquid chlorine sulfoxide and SO by separation2, HCL gas divided
From thionyl chloride backs within synthesis procedure and applies；
C, the SO after separation2, HCL and synthesis 2- chloroethyl propyl ether during generate SO2, HCL enter together tail gas purifying
System, recycling obtains finished product later.
It can be seen via above technical scheme that compared with prior art, the invention has the characteristics that:
(1) it by above-mentioned technique, can solve in original technique 2- chloroethyl propyl ether deacidification, avoid because of thionyl chloride point
It solves SO2, the HCL generated and is dissolved in the absorption of liquid intracorporal SO2, HCL and generates with high salt, high-COD waste water situation.
(2) because having recycled the thionyl chloride being excessively used, the liquid alkaline used because absorbing SO2, HCL is eliminated.
(3) utilization rate and 2- of raw material can be improved in the pyrolytic that 2- chloroethyl propyl ether is avoided by low-flash
The yield of chloroethyl propyl ether.
(4) the 2- chloroethyl propyl ether dissolved in water in alkaline cleaning procedure is eliminated.
(5) economic, environmental protection.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 attached drawing is process flow diagram of the invention.
In Fig. 1: 1 be glycol propyl ether measuring tank, 2 be thionyl chloride measuring tank, 3 be chlorine ether reaction kettle, 4 be chlorine ether turn
Material pump, 5 be chlorine ether distillation still, 6 be chlorine ether receiving tank, 7 be thionyl chloride receiving tank, 8 be thionyl chloride transfering material pump, 9 be vacuum
Surge tank, 10 be dry vacuum pump, 11 be reflux condenser, 12 be distiller condenser.
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.
The embodiment of the invention discloses it is a kind of not only in terms of economic, environmental protection with greater advantage, but also simple process,
Deacidification technique in low in cost, energy-saving and environment-friendly 2- chloroethyl propyl ether production process.
Attached drawing 1 is please referred to, is the deacidification technique in a kind of 2- chloroethyl propyl ether production process disclosed by the invention, specifically
Include:
Deacidification technique needs two-step process: (1) for thionyl chloride or other chlorinating agents production 2- chloroethyl propyl ether and other
The removal of Related product middle acid substance；(2) 2- chloroethyl propyl is removed by physical methods such as decompression, flash distillation, condensation, separation
The acidic materials of ether and Related product；Wherein, the air pressure of decompression is -0. 06MPa；The temperature of flash distillation is 50 DEG C；In separation process
With CL—Meter, acidity≤0.03 of 2- chloroethyl propyl ether.
The depickling distillation technique of 2- chloroethyl propyl ether of the invention compared with traditional alkali washing process, not only it is economical,
Environmentally friendly aspect with greater advantage, and simple process, low in cost, energy conservation and environmental protection.
In order to further optimize the above technical scheme, specific process are as follows:
A, after with excessive thionyl chloride and ethylene glycol positive propyl ether synthesis 2- chloroethyl propyl ether, in deacidification, by 2- chlorine
Ethyl propyl ether, unreacted thionyl chloride and the SO being dissolved in liquid material2, enter distillation still after HCL gas pressurized
Interior efficient distributor is dispersed, and is depressurized, flashed in it, make thionyl chloride vaporize and with SO2, HCL gas one
It rises and is separated with 2- chloroethyl propyl ether；
B, the thionyl chloride after vaporization passes through condensation liquefaction, makes liquid chlorine sulfoxide and SO by separation2, HCL gas divided
From thionyl chloride backs within synthesis procedure and applies；
C, the SO after separation2, HCL and synthesis 2- chloroethyl propyl ether during generate SO2, HCL enter together tail gas purifying
System, recycling obtains finished product later.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other
The difference of embodiment, the same or similar parts in each embodiment may refer to each other.For device disclosed in embodiment
For, since it is corresponded to the methods disclosed in the examples, so being described relatively simple, related place is said referring to method part
It is bright.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (2)
1. the deacidification technique in a kind of 2- chloroethyl propyl ether production process, which is characterized in that deacidification technique needs two-step process:
(1) removal for thionyl chloride or other chlorinating agents production 2- chloroethyl propyl ether and other Related product middle acid substances；
(2) acidic materials of 2- chloroethyl propyl ether and Related product are removed by physical methods such as decompression, flash distillation, condensation, separation；Its
In, the air pressure of decompression is -0. 06MPa；The temperature of flash distillation is 50 DEG C；With CL in separation process—Meter, 2- chloroethyl propyl ether
Acidity≤0.03.
2. the deacidification technique in a kind of 2- chloroethyl propyl ether production process according to claim 1, which is characterized in that tool
The process of body are as follows:
A, after with excessive thionyl chloride and ethylene glycol positive propyl ether synthesis 2- chloroethyl propyl ether, in deacidification, by 2- chlorine
Ethyl propyl ether, unreacted thionyl chloride and the SO being dissolved in liquid material2, enter distillation still after HCL gas pressurized
Interior efficient distributor is dispersed, and is depressurized, flashed in it, make thionyl chloride vaporize and with SO2, HCL gas one
It rises and is separated with 2- chloroethyl propyl ether；
B, the thionyl chloride after vaporization passes through condensation liquefaction, makes liquid chlorine sulfoxide and SO by separation2, HCL gas divided
From thionyl chloride backs within synthesis procedure and applies；
C, the SO after separation2, HCL and synthesis 2- chloroethyl propyl ether during generate SO2, HCL enter together tail gas purifying system
System, recycling obtains finished product later.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711452527.8A CN109970522A (en) | 2017-12-28 | 2017-12-28 | A kind of deacidification technique in 2- chloroethyl propyl ether production process |
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| CN201711452527.8A CN109970522A (en) | 2017-12-28 | 2017-12-28 | A kind of deacidification technique in 2- chloroethyl propyl ether production process |
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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 (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295537A (en) * | 2010-06-25 | 2011-12-28 | 吉林师范大学 | Method for producing methoxyethyl chloromethyl ether |
| CN104591099A (en) * | 2015-01-08 | 2015-05-06 | 青岛科技大学 | Method and device for refining sulfoxide chloride |
| CN105384612A (en) * | 2015-12-14 | 2016-03-09 | 山东凯盛新材料有限公司 | Preparation method of chloroethyl-n-propylether |
| CN105461520A (en) * | 2015-12-14 | 2016-04-06 | 山东凯盛新材料有限公司 | Synthetic method for 2-propoxyethyl chloride |
| CN105461521A (en) * | 2015-12-14 | 2016-04-06 | 山东凯盛新材料有限公司 | Method for synthesizing 2-chloroethyl-propylether |
| CN105523902A (en) * | 2015-12-14 | 2016-04-27 | 山东凯盛新材料有限公司 | Preparation method of 1-(2-chloroethoxy)propane |
-
2017
- 2017-12-28 CN CN201711452527.8A patent/CN109970522A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295537A (en) * | 2010-06-25 | 2011-12-28 | 吉林师范大学 | Method for producing methoxyethyl chloromethyl ether |
| CN104591099A (en) * | 2015-01-08 | 2015-05-06 | 青岛科技大学 | Method and device for refining sulfoxide chloride |
| CN105384612A (en) * | 2015-12-14 | 2016-03-09 | 山东凯盛新材料有限公司 | Preparation method of chloroethyl-n-propylether |
| CN105461520A (en) * | 2015-12-14 | 2016-04-06 | 山东凯盛新材料有限公司 | Synthetic method for 2-propoxyethyl chloride |
| CN105461521A (en) * | 2015-12-14 | 2016-04-06 | 山东凯盛新材料有限公司 | Method for synthesizing 2-chloroethyl-propylether |
| CN105523902A (en) * | 2015-12-14 | 2016-04-27 | 山东凯盛新材料有限公司 | Preparation method of 1-(2-chloroethoxy)propane |
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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| TA01 | Transfer of patent application right |
Effective date of registration: 20201224 Address after: 256600 south side of xinyongxin Road, Binbei office, Bincheng District, Binzhou City, Shandong Province Applicant after: Shoujian Technology Co.,Ltd. Address before: 256600 south side of xinyongxin Road, Binbei office, Bincheng District, Binzhou City, Shandong Province Applicant before: SHANDONG QIAOCHANG CHEMICAL Co.,Ltd. |
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Application publication date: 20190705 |
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