CN101225046A - Method for producing di(trichloromethyl) carbonate by semi-continuous process - Google Patents
Method for producing di(trichloromethyl) carbonate by semi-continuous process Download PDFInfo
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- CN101225046A CN101225046A CNA2008100015548A CN200810001554A CN101225046A CN 101225046 A CN101225046 A CN 101225046A CN A2008100015548 A CNA2008100015548 A CN A2008100015548A CN 200810001554 A CN200810001554 A CN 200810001554A CN 101225046 A CN101225046 A CN 101225046A
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Abstract
The invention relates to a semi-continuous production method for bis (trichloromethyl) carbonate. The material dimethyl carbonate is added to a column chlorination reactor from top to down, and the chlorine is pumped in for chlorination reaction under the irradiation of ultraviolet; the reaction rate is obviously decreased in the late reaction; when the chlorine incompletely reacts, part of the dimethyl carbonate is supplemented through the upper part of the reactor and the chlorine is continuously pumped in for chlorination reaction, and the unreacted chlorine at the bottom of the reactor can continuously react at the upper part of the reactor; the reaction rate is obviously decreased in the late reaction, when the chorine is stopped when incompletely reacts, the reaction production bis (trichloromethyl) carbonate reacted completely is emitted through the lower part of the reactor, and part of the dimethyl carbonate is supplemented through the upper part of the reactor and the chlorine is continuously pumped in for chlorination reaction.
Description
The present invention relates to a kind of semi-continuous process and produce the method for two (trichloromethyl) carbonic ether.
Two (trichloromethyl) carbonic ether has another name called triphosgene or solid phosgene, is the high material of a kind of reactive behavior, can substitute phosgene and carry out as chemical reactions such as chloromethane esterification, carbonic acid esterification, isocyanation esterification, isocyanideization, chlorination, chlorine formylations.At present, the method for domestic production two (trichloromethyl) carbonic ether is an interrupter method methylcarbonate chlorinated with chlorine, because chlorination late phase reaction difficulty, chlorine must be excessive, causes chlorine reaction incomplete, and the chlorine consumption is big, and production efficiency is low.Simultaneously owing to be mixed with a large amount of unreacted chlorine in the byproduct hydrogen chloride gas, water absorbs in the process of preparation hydrochloric acid, chlorine also is dissolved in wherein, form free chlorine, these free chlorines can come out in user's use, and production environment is caused severe contamination, also because free chlorine is very active, can participate in many chemical reactions, limit the application of this by-product hydrochloric acid greatly, cause many manufacturers can't use directly with its discharging because of by-product hydrochloric acid.Cause production cost to strengthen because of by-product hydrochloric acid can't reclaim on the one hand, the direct discharging of by-product hydrochloric acid has caused very serious pollution to environment on the other hand.
The purpose of this invention is to provide a kind of semi-continuous process and produce the method for two (trichloromethyl) carbonic ether, to solve the weak point that existing Technology exists.
A kind of semi-continuous process of the present invention is produced the method for two (trichloromethyl) carbonic ether, comprises the following steps:
(1), the material carbon dimethyl phthalate is added in the pillar chlorination reactor from top to bottom, under uviolizing, feed chlorine and carry out chlorination reaction;
(2) etc. reaction proceeds to the later stage, and speed of reaction obviously descends, and when chlorine reaction was incomplete, autoreactor upper supplementary part methylcarbonate continued logical chlorine and carries out chlorination reaction, continues reaction on reactor top at the unreacted chlorine of reactor lower part;
(3) etc. above-mentioned reaction proceeds to the later stage, speed of reaction obviously descends, when chlorine reaction is incomplete, stop logical chlorine, the autoreactor bottom emits reaction product two (trichloromethyl) carbonic ether that has reacted completely, autoreactor upper supplementary part methylcarbonate continues logical chlorine and carries out chlorination reaction;
(4) repeat above-mentioned steps (3), realize semi-continuous production.
The present invention has following advantage:
1, realized that production process is semicontinuous, production process is relatively stable, and production efficiency improves relatively;
2, chlorine consumption and production cost have been reduced;
3, can prepare qualified technical hydrochloric acid;
Further comment below by embodiment:
Embodiment:
1, the material carbon dimethyl phthalate is added in the pillar chlorination reactor from top to bottom, under uviolizing, feed chlorine and carry out chlorination reaction;
2, etc. after reaction was carried out 3-6 hour, speed of reaction obviously descended, and when chlorine reaction was incomplete, autoreactor upper supplementary part methylcarbonate continued logical chlorine and carries out chlorination reaction, continues reaction on reactor top at the unreacted chlorine of reactor lower part;
3, etc. above-mentioned reaction proceeds to the later stage, speed of reaction obviously descends, when chlorine reaction is incomplete, stop logical chlorine, the autoreactor bottom emits reaction product two (trichloromethyl) carbonic ether that has reacted completely, autoreactor upper supplementary part methylcarbonate continues logical chlorine and carries out chlorination reaction;
Claims (1)
1. semi-continuous process is produced the method for two (trichloromethyl) carbonic ether, it is characterized in that: (1), the material carbon dimethyl phthalate is added in the pillar chlorination reactor from top to bottom feeds chlorine and carries out chlorination reaction under uviolizing;
(2) etc. reaction proceeds to the later stage, and speed of reaction obviously descends, and when chlorine reaction was incomplete, autoreactor upper supplementary part methylcarbonate continued logical chlorine and carries out chlorination reaction, continues reaction on reactor top at the unreacted chlorine of reactor lower part;
(3) etc. above-mentioned reaction proceeds to the later stage, speed of reaction obviously descends, when chlorine reaction is incomplete, stop logical chlorine, the autoreactor bottom emits reaction product two (trichloromethyl) carbonic ether that has reacted completely, autoreactor upper supplementary part methylcarbonate continues logical chlorine and carries out chlorination reaction;
(4) repeat above-mentioned steps (3), realize semi-continuous production.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100015548A CN101225046A (en) | 2008-01-09 | 2008-01-09 | Method for producing di(trichloromethyl) carbonate by semi-continuous process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100015548A CN101225046A (en) | 2008-01-09 | 2008-01-09 | Method for producing di(trichloromethyl) carbonate by semi-continuous process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101225046A true CN101225046A (en) | 2008-07-23 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008100015548A Pending CN101225046A (en) | 2008-01-09 | 2008-01-09 | Method for producing di(trichloromethyl) carbonate by semi-continuous process |
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| CN (1) | CN101225046A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058961A (en) * | 2014-06-07 | 2014-09-24 | 李安民 | Process and equipment for continuously producing di(trichloromethyl)carbonate by adopting two-step chlorination method |
| CN104058970A (en) * | 2014-05-19 | 2014-09-24 | 李安民 | Process and equipment for producing di(trichloromethyl) carbonic ester by continuous chlorination process |
| CN104140369A (en) * | 2014-06-22 | 2014-11-12 | 李安民 | Technology and equipment for producing bis(trichloromethyl)carbonate through hermetical condensation and continuous packaging |
| CN111320544A (en) * | 2020-04-13 | 2020-06-23 | 湖北可赛化工有限公司 | Process and equipment for three-stage semi-continuous synthesis of bis (trichloromethyl) carbonate |
| CN114409543A (en) * | 2022-02-10 | 2022-04-29 | 宁夏华御化工有限公司 | Continuous preparation process of triphosgene |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH107623A (en) * | 1996-06-18 | 1998-01-13 | Nippon Kayaku Co Ltd | Production of bis(trichloromethyl) carbonate |
-
2008
- 2008-01-09 CN CNA2008100015548A patent/CN101225046A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH107623A (en) * | 1996-06-18 | 1998-01-13 | Nippon Kayaku Co Ltd | Production of bis(trichloromethyl) carbonate |
Non-Patent Citations (2)
| Title |
|---|
| 洪新民: "固体光气的合成与应用", 《化工中间体》 * |
| 王正平等: "三光气的合成及应用", 《化工进展》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058970A (en) * | 2014-05-19 | 2014-09-24 | 李安民 | Process and equipment for producing di(trichloromethyl) carbonic ester by continuous chlorination process |
| CN104058961A (en) * | 2014-06-07 | 2014-09-24 | 李安民 | Process and equipment for continuously producing di(trichloromethyl)carbonate by adopting two-step chlorination method |
| CN104140369A (en) * | 2014-06-22 | 2014-11-12 | 李安民 | Technology and equipment for producing bis(trichloromethyl)carbonate through hermetical condensation and continuous packaging |
| CN111320544A (en) * | 2020-04-13 | 2020-06-23 | 湖北可赛化工有限公司 | Process and equipment for three-stage semi-continuous synthesis of bis (trichloromethyl) carbonate |
| CN114409543A (en) * | 2022-02-10 | 2022-04-29 | 宁夏华御化工有限公司 | Continuous preparation process of triphosgene |
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Application publication date: 20080723 |