CN103819507B - A kind of ethrel resets technique - Google Patents
A kind of ethrel resets technique Download PDFInfo
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- CN103819507B CN103819507B CN201410090994.0A CN201410090994A CN103819507B CN 103819507 B CN103819507 B CN 103819507B CN 201410090994 A CN201410090994 A CN 201410090994A CN 103819507 B CN103819507 B CN 103819507B
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Abstract
The invention discloses a kind of ethrel and reset technique, first three (2-chloroethyl) phosphorous acid ester enters stirred autoclave and carries out rearrangement reaction, and then flows into insulation reaction in vertical tube-type rearrangement device.Ethrel of the present invention resets technique increases a set of stirred autoclave before original vertical tube-type rearrangement device material inlet.This technique can make rearrangement reaction more fully and completely, heat transmits evenly effectively, thus the traditional rearrangement device temperature of effective solution is wayward, frequent temperature runaway, the series of problems such as punching material, back mixing occur, and make rearrangement device temperature easier in control, process unit consumption reduces, two ester conversion rates and yield increase, and produce more stable.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of ethrel and reset technique.
Background technology
Rearrangement is the committed step during ethrel is produced.Facts have proved that two ester content height play an important role to acidolysis reaction, two ester contents after rearrangement are higher, just can obtain the ethrel of high-content.Conventional ethylene profit resets explained hereafter, and great majority adopt vertical tube-type rearrangement device to produce.This rearrangement device takes into account preheating, reaction, insulation effect, and the preheating of this rearrangement technique is coupled with the height of reaction and causes that the operating restraint of rearrangement device is narrow, device stability is poor.Show as rearrangement device temperature wayward, frequent temperature runaway, the phenomenons such as punching material, back mixing occur.Reset material temperature out often can sharply raise, intermolecular rearrangement aggravates, and side reaction increases, three (2-chloroethyl) phosphorous acid ester low conversion rate; Intermolecular rearrangement produces a large amount of ethylene dichloride gas simultaneously, and entrained liquids flows out from rearrangement device top, causes process unit consumption to raise, causes diester yield to reduce, and produces unstable.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of ethrel and resets technique, and this technique can make rearrangement reaction more thorough, and heat transmission is evenly effectively.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of ethrel resets technique, and first three (2-chloroethyl) phosphorous acid ester enters stirred autoclave and carry out rearrangement reaction, and then flows into insulation reaction in vertical tube-type rearrangement device.
Wherein, described material flow controls at 0.6m
3/ h.
Wherein, the temperature of reaction of stirring-type reactor controls at 140 ~ 170 DEG C.
Wherein, the mixing speed of stirring-type reactor controls at 135r/min.
Wherein, the temperature of reaction of vertical tube-type rearrangement device controls at 150 ~ 180 DEG C.
Beneficial effect: ethrel of the present invention resets technique increases a set of stirred autoclave before original vertical tube-type rearrangement device material inlet.This technique can make rearrangement reaction more fully and completely, heat transmits evenly effectively, thus the traditional rearrangement device temperature of effective solution is wayward, frequent temperature runaway, the series of problems such as punching material, back mixing occur, and make rearrangement device temperature easier in control, process unit consumption reduces, two ester conversion rates and yield increase, and produce more stable.
Embodiment
According to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, the content described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
Embodiment 1:
A kind of ethrel resets technique, first three (2-chloroethyl) phosphorous acid ester enters stirred autoclave and carries out rearrangement reaction, the temperature of reaction of stirring-type reactor controls at 140 DEG C, the mixing speed of stirring-type reactor controls at 135r/min, and then flowing into 150 DEG C of insulation reaction in vertical tube-type rearrangement device, overall material flow controls at 0.6m3/h.As a result, diester average content is 94.8%.
Embodiment 2:
A kind of ethrel resets technique, first three (2-chloroethyl) phosphorous acid ester enters stirred autoclave and carries out rearrangement reaction, the temperature of reaction of stirring-type reactor controls at 160 DEG C, the mixing speed of stirring-type reactor controls at 135r/min, and then flowing into 160 DEG C of insulation reaction in vertical tube-type rearrangement device, overall material flow controls at 0.6m
3/ h.As a result, diester average content is 95.2%
Embodiment 3:
A kind of ethrel resets technique, first three (2-chloroethyl) phosphorous acid ester enters stirred autoclave and carries out rearrangement reaction, the temperature of reaction of stirring-type reactor controls at 170 DEG C, the mixing speed of stirring-type reactor controls at 135r/min, and then flowing into 180 DEG C of insulation reaction in vertical tube-type rearrangement device, overall material flow controls at 0.6m
3/ h.As a result, diester average content is 94.2%
Comparative example:
Before transformation, technique describes: three (2-chloroethyl) phosphorous acid ester is with flow velocity 0.6m
3/ h injects rearrangement device continuously by fresh feed pump, three (2-chloroethyl) phosphorous acid ester is carried out heating by rearrangement device bottom heating device makes temperature of charge in rearrangement device remain on 150 ~ 160 DEG C, there is rearrangement reaction and generate diester in three (2-chloroethyl) phosphorous acid ester, produce by product ethylene dichloride in rearrangement device simultaneously.As a result, the average content of diester is 88%.
Claims (1)
1. ethrel resets a technique, and it is characterized in that, first three (2-chloroethyl) phosphorous acid ester enters stirred autoclave and carry out rearrangement reaction, and then flows into insulation reaction in vertical tube-type rearrangement device;
Wherein, described material flow controls at 0.6m
3/ h;
The temperature of reaction of stirring-type reactor controls at 140 ~ 170 DEG C;
The mixing speed of stirring-type reactor controls at 135r/min;
The temperature of reaction of vertical tube-type rearrangement device controls at 150 ~ 180 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410090994.0A CN103819507B (en) | 2014-03-13 | 2014-03-13 | A kind of ethrel resets technique |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410090994.0A CN103819507B (en) | 2014-03-13 | 2014-03-13 | A kind of ethrel resets technique |
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| CN103819507A CN103819507A (en) | 2014-05-28 |
| CN103819507B true CN103819507B (en) | 2016-03-02 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410090994.0A Active CN103819507B (en) | 2014-03-13 | 2014-03-13 | A kind of ethrel resets technique |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107652322A (en) * | 2017-09-19 | 2018-02-02 | 江苏禾裕泰化学有限公司 | Rearranged reaction prepares 2 chloroethyl di(2-ethylhexyl)phosphates（2 chloroethyls）The method of ester |
| CN111533766A (en) * | 2020-03-25 | 2020-08-14 | 中棉小康生物科技有限公司 | Ethephon rearrangement process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2289793Y (en) * | 1997-04-09 | 1998-09-02 | 北京市房地产科学技术研究所 | Reactor for producing chloro-thyl phosphoric acid dichloride ethyl ester |
| CN201603559U (en) * | 2010-01-19 | 2010-10-13 | 江苏安邦电化有限公司 | Tower-type continuous rearrangement reactor |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IL41275A (en) * | 1967-04-27 | 1973-10-25 | Gen Aniline & Film Corp | Process for producing beta-haloethyl-phosphonic acids |
| US4311652A (en) * | 1980-05-28 | 1982-01-19 | Stauffer Chemical Company | Arbuzov reactions employing an aliphatic solvent |
| DE3033614A1 (en) * | 1980-09-06 | 1982-04-29 | Hoechst Ag, 6000 Frankfurt | METHOD FOR PRODUCING VINYLPHOSPHONIC ACID DICHLORIDE AND 2-CHLORETHANPHOSPHONIC ACID DICHLORIDE |
-
2014
- 2014-03-13 CN CN201410090994.0A patent/CN103819507B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2289793Y (en) * | 1997-04-09 | 1998-09-02 | 北京市房地产科学技术研究所 | Reactor for producing chloro-thyl phosphoric acid dichloride ethyl ester |
| CN201603559U (en) * | 2010-01-19 | 2010-10-13 | 江苏安邦电化有限公司 | Tower-type continuous rearrangement reactor |
Non-Patent Citations (2)
| Title |
|---|
| 乙烯利生产中重排反应器的研究;居宪民 等;《农药工业》;19800430(第4期);第42-43页 * |
| 乙烯利重排器的模拟分析与设计优化;张新平 等;《化工进展》;20111205;第30卷(第12期);摘要，第2616页左栏第2-3段，第2618页右栏—2620页左栏 * |
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Address after: 223002 No. 30, Chemical Road, Huaian, Jiangsu Patentee after: Andao mai'anbang (Jiangsu) Co., Ltd Address before: 223002 No. 30, Chemical Road, Huaian, Jiangsu Patentee before: JIANGSU ANPON ELECTROCHEMICAL Co.,Ltd. |
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