CN105712856A - Production process and apparatus of p-benzoquinone - Google Patents
Production process and apparatus of p-benzoquinone Download PDFInfo
- Publication number
- CN105712856A CN105712856A CN201610051955.9A CN201610051955A CN105712856A CN 105712856 A CN105712856 A CN 105712856A CN 201610051955 A CN201610051955 A CN 201610051955A CN 105712856 A CN105712856 A CN 105712856A
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- crystallization
- distillation column
- temperature
- benzoquinone
- kettle
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C46/00—Preparation of quinones
- C07C46/02—Preparation of quinones by oxidation giving rise to quinoid structures
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C46/00—Preparation of quinones
- C07C46/10—Separation; Purification; Stabilisation; Use of additives
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a production process and apparatus of p-benzoquinone. The process comprises: oxidative reaction, distillation, crystallization and centrifugation. The apparatus comprises an oxidation tank provided with a remote-transmitting integrated temperature meter, the oxidation tank is connected with a temporary storage kettle, the temporary storage kettle is connected with a high-position tank through a transfer pump, the high-position tank is connected with a plurality of distilling columns, each distilling column is provided with a steam flow and steam regulating valves. The production process and apparatus have the advantages that the field remote-transmitting integrated temperature meter is added to an oxidation station feeding kettle, tendency inspection is available for past operation temperature, reaction temperature fluctuation is can be reduced as far as possible, temperature control is more accurate, and conversion rate is increased. Steam flow is regulated through top and bottom temperature changes, so that operation error is reduced and efficiency is improved, and the lower portion of a discharge pipe is added with a sensitive board so that prediction and and timely regulation may be made before top temperature is abnormal.
Description
Technical field
The invention belongs to chemical industry and field of chemical equipment, especially relate to production technology and the equipment of 1,4-benzoquinone.
Background technology
1,4-benzoquinone (C6H4O2) it is a kind of important chemical products, it is mainly used as oxidant, polymerization inhibitor, dyestuff intermediate and rubber antioxidant, also acts as gather qi together reaction initiator and produce the raw material of hydroquinone.One of method of current industrial production 1,4-benzoquinone is, lower than under 20 DEG C of conditions, in oxidation trough, in being dissolved with manganese dioxide (MnO2) acid solution in dropping aniline (C6H5NH2), to allow the manganese dioxide in this acid solution that aniline to be aoxidized；Then obtain then through distillation, crystallization, dehydrate.Existing technique is, in oxidation reaction part, after dripping aniline after adding manganese dioxide and sulphuric acid, sees that scene temperature table controls the speed of dropping aniline, and shortcoming is that trendless can be looked into；The operation of distillation fraction, principal element has top temperature, end temperature, backflow (drench material blanking and be equivalent to backflow).Operation before have top temperature, end temperature, top pressure, base pressure remote transfer signal show, but not do not control, rule of thumb and feel can only pass through material color etc. and operate, extremely unstable.Top temperature is too high, can go out black material.Temperature too low quinone in the end can fall at the bottom of tower, together discharges with waste water, efficiency and quality extremely unstable,
Summary of the invention
In view of the deficiencies in the prior art, the present invention provides the technique preparing 1,4-benzoquinone and the equipment of a kind of automatization, specifically, the technical scheme is that
The production technology of 1,4-benzoquinone, including oxidation reaction, distillation and crystallization；
(1) oxidation reaction: be added in reactor by manganese dioxide and sulphuric acid, then drips aniline in reactor, and during dropping aniline, the speed trend according to temperature, is that temperature trend keeps constant；
(2) distillation, joins in distillation column by oxidation liquid with certain speed, observes the temperature of the top of distillation column, middle part and bottom, determines that steam enters the amount of distillation column according to the temperature of each several part of display end；
(3) crystallization, is lowered the temperature by chilled brine, crystallization, respectively through primary crystallization and secondary crystallization.
(4) 1,4-benzoquinone after crystallization, to obtain finished product through being centrifuged and drying.
Realize the equipment of the production technology of above 1,4-benzoquinone, including oxidation trough, oxidation trough is provided with teletransmission one thermometer, oxidation trough is connected with temporary storage kettle, described temporary storage kettle by transfering material pump and head tank together with, head tank connects several distillation column, it is in parallel between described distillation column, the feed pipe of described distillation column is provided with feed flow meter, it is provided with charging in the lower end of feed flow meter and regulates valve, tower top temperature sensor and tower top pressure sensor it is provided with in the upper end of distillation column, and it is respectively equipped with in tower in the centre of distillation column and bottom temperature sensor and column bottom temperature sensor, the pipeline that distillation column is connected with vapor phase is provided with steam control valve and steam-flow meter, the upper end of distillation column is connected with crystallization kettle by pipeline, also it is in series with crystallization kettle after crystallization kettle and is used as secondary crystallization, the crystallization kettle of secondary crystallization connects centrifuge.
Process above and equipment application in the adjacent methyl hydroquinone of preparation.
Further, the pipeline between distillation column and crystallization kettle is provided with cooling jacket pipe.Preferably, for cooling water in described cooling jacket pipe.
Further, described temporary storage kettle is provided with valve and is connected with the pipeline of 1,4-benzoquinone liquid.
Further, described distillation column is identical with the number of crystallization kettle still, is 3.
Further, described temporary storage kettle is two, is provided with stirring rod in temporary storage kettle.
Further, described transfering material pump is two, and is set up in parallel, and the upper end of each transfering material pump is equipped with valve.
Compared with prior art, the present invention has the advantage that and has the benefit effect that
(1) still that feeds intake in oxidation post has installed on-the-spot teletransmission one thermometer additional, in being accessed by remote transfer signal, control PLC system, has trend to look into the operation temperature in past, as much as possible reduces reaction temperature fluctuation, temperature is made to control more accurate, thus improving conversion ratio.
(2) tremie pipe lower part is computed one piece of sensitive plate of shortcoming, with look-ahead variations in temperature, in order to control in advance.
(3) by pushing up the change adjustment steam flow of gentle end temperature, can be expected, and feed rate and top temperature set tandem operation by pouring for fixed steam flow during steam stable, or after fixing for feed rate, steam and top temperature set tandem and can realize Automated condtrol, reduce operating error and improve efficiency, after feed pipe lower part installs sensitive plate additional, can predict in advance when the no abnormal change of top temperature and carry out adjustment in time.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Fig. 2 is oxidation trough and the schematic diagram of part distillation and crystallization apparatus.
In figure, 1 is oxidation trough, and 2 is teletransmission one thermometer, 3 is temporary storage kettle, and 4 is transfering material pump, and 5 is head tank, 6 is distillation column, and 7 is crystallization kettle, and 8 is feed flow meter, 9 regulate valve for charging, and 10 is tower top temperature sensor, and 11 is tower top pressure sensor, 12 is temperature sensor in tower, and 13 is column bottom temperature sensor, and 14 is steam control valve, 15 is steam-flow meter, and 16 is cooling jacket pipe.
Detailed description of the invention
Below in conjunction with embodiment, the specific embodiment of the present invention is described in further detail.Be will assist in by following embodiment and understand the present invention, but do not limit technical scheme in any form.
The production technology of 1,4-benzoquinone, including oxidation reaction, distillation and crystallization；
(1) oxidation reaction: be added in reactor by manganese dioxide and sulphuric acid, then drips aniline in reactor, and during dropping aniline, the speed trend according to temperature, is that temperature trend keeps constant；
(2) distillation, joins in distillation column 6 by oxidation liquid with certain speed, observes the temperature of the top of distillation column, middle part and bottom, determines that steam enters the amount of distillation column 6 according to the temperature of each several part of display end；
(3) crystallization, is lowered the temperature by chilled brine, crystallization, respectively through primary crystallization and secondary crystallization.
(4) 1,4-benzoquinone after crystallization, to obtain finished product through being centrifuged and drying.
Realize the equipment of the production technology of above 1,4-benzoquinone, including oxidation trough 1, oxidation trough 1 is provided with teletransmission one thermometer 2, oxidation trough 1 is connected with temporary storage kettle 3, described temporary storage kettle 3 by transfering material pump 4 and head tank 5 together with, head tank 5 connects several distillation column 6, it is in parallel between described distillation column 6, the feed pipe of described distillation column 6 is provided with feed flow meter 8, it is provided with charging in the lower end of feed flow meter 8 and regulates valve 9, tower top temperature sensor 10 and tower top pressure sensor 11 it is provided with in the upper end of distillation column 6, and it is respectively equipped with in tower in the centre of distillation column 6 and bottom temperature sensor 12 and column bottom temperature sensor 13, the pipeline that distillation column 6 is connected with vapor phase is provided with steam control valve 14 and steam-flow meter 15, the upper end of distillation column 6 is connected with crystallization kettle 7 by pipeline, also it is in series with crystallization kettle 7 after crystallization kettle 7 and is used as secondary crystallization, the crystallization kettle 7 of secondary crystallization connects centrifuge.
In the present embodiment, the pipeline between distillation column 6 and crystallization kettle 7 is provided with cooling jacket pipe 16.Preferably, for cooling water in described cooling jacket pipe 16.Described temporary storage kettle 3 is provided with valve and is connected with the pipeline of 1,4-benzoquinone liquid.Described distillation column 6 is identical with the number of crystallization kettle 7, is 3.Described temporary storage kettle 3 is two, is provided with stirring rod in temporary storage kettle 3.Described transfering material pump 4 is two, and is set up in parallel, and the upper end of each transfering material pump 4 is equipped with valve.
Above specific embodiments of the invention are described in detail, but described content has been only presently preferred embodiments of the present invention, it is impossible to be considered the practical range for limiting the present invention.All equalizations made according to the present patent application scope change and improvement etc., all should still belong within the patent covering scope of the present invention.
Claims (9)
1. the production technology to this quinone product, including oxidation reaction, distillation and crystallization；It is characterized in that:
1) oxidation reaction: be added in reactor by manganese dioxide and sulphuric acid, then drips aniline in reactor, and during dropping aniline, the speed trend according to temperature, is that temperature trend keeps constant；
2) distillation, joins in distillation column by oxidation liquid with certain speed, observes the temperature of the top of distillation column, middle part and bottom, determines that steam enters the amount of distillation column according to the temperature of each several part of display end；
3) crystallization, is lowered the temperature by chilled brine, crystallization, respectively through primary crystallization and secondary crystallization.
4) 1,4-benzoquinone after crystallization, to obtain finished product through being centrifuged and drying.
2. realize the equipment of the production technology of claim 1 1,4-benzoquinone, it is characterized in that: include oxidation trough, oxidation trough is provided with teletransmission one thermometer, oxidation trough is connected with temporary storage kettle, described temporary storage kettle by transfering material pump and head tank together with, head tank connects several distillation column, it is in parallel between described distillation column, the feed pipe of described distillation column is provided with feed flow meter, it is provided with charging in the lower end of feed flow meter and regulates valve, tower top temperature sensor and tower top pressure sensor it is provided with in the upper end of distillation column, and it is respectively equipped with in tower in the centre of distillation column and bottom temperature sensor and column bottom temperature sensor, the pipeline that distillation column is connected with vapor phase is provided with steam control valve and steam-flow meter, the upper end of distillation column is connected with crystallization kettle by pipeline, also it is in series with crystallization kettle after crystallization kettle and is used as secondary crystallization, the crystallization kettle of secondary crystallization connects centrifuge.
3. the technique of claim 1 and the application in the adjacent methyl hydroquinone of preparation of the equipment of claim 2.
4. the equipment of the production technology of 1,4-benzoquinone according to claim 2, it is characterised in that: the pipeline between distillation column and crystallization kettle is provided with cooling jacket pipe.
5. the equipment of the production technology of 1,4-benzoquinone according to claim 4, it is characterised in that: for cooling water in described cooling jacket pipe.
6. the equipment of the production technology of 1,4-benzoquinone according to claim 2, it is characterised in that: described temporary storage kettle is provided with valve and is connected with the pipeline of 1,4-benzoquinone liquid.
7. the equipment of the production technology of 1,4-benzoquinone according to claim 2, it is characterised in that: described distillation column is identical with the number of crystallization kettle still, is 3.
8. the equipment of the production technology of 1,4-benzoquinone according to claim 2, it is characterised in that: described temporary storage kettle is two, is provided with stirring rod in temporary storage kettle.
9. the equipment of the production technology of 1,4-benzoquinone according to claim 2, it is characterised in that: described transfering material pump is two, and is set up in parallel, and the upper end of each transfering material pump is equipped with valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610051955.9A CN105712856A (en) | 2016-01-27 | 2016-01-27 | Production process and apparatus of p-benzoquinone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610051955.9A CN105712856A (en) | 2016-01-27 | 2016-01-27 | Production process and apparatus of p-benzoquinone |
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| Publication Number | Publication Date |
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| CN105712856A true CN105712856A (en) | 2016-06-29 |
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| CN201610051955.9A Pending CN105712856A (en) | 2016-01-27 | 2016-01-27 | Production process and apparatus of p-benzoquinone |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974519A (en) * | 2006-11-28 | 2007-06-06 | 湖北开元化工科技股份有限公司 | Decompression gas stripping process |
| CN101139271A (en) * | 2007-08-23 | 2008-03-12 | 盐城凤阳化工有限公司 | Novel process for producing p-benzoquinone |
| CN102976914A (en) * | 2012-12-17 | 2013-03-20 | 重庆优萃科技有限公司 | Method for preparing p-benzoquinone |
| CN205528527U (en) * | 2016-01-27 | 2016-08-31 | 潍坊泰兴生物化工有限责任公司 | 1, 4 -benzoquinone production facility |
-
2016
- 2016-01-27 CN CN201610051955.9A patent/CN105712856A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974519A (en) * | 2006-11-28 | 2007-06-06 | 湖北开元化工科技股份有限公司 | Decompression gas stripping process |
| CN101139271A (en) * | 2007-08-23 | 2008-03-12 | 盐城凤阳化工有限公司 | Novel process for producing p-benzoquinone |
| CN102976914A (en) * | 2012-12-17 | 2013-03-20 | 重庆优萃科技有限公司 | Method for preparing p-benzoquinone |
| CN205528527U (en) * | 2016-01-27 | 2016-08-31 | 潍坊泰兴生物化工有限责任公司 | 1, 4 -benzoquinone production facility |
Non-Patent Citations (2)
| Title |
|---|
| 管丰年等: "基于PLC的间歇式化学反应釜控制系统", 《潍坊学院学报》 * |
| 莫彬编: "《过程控制工程》", 31 October 1991, 化学工业出版社 * |
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Application publication date: 20160629 |
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