CN102826522A - Circulation flow reaction device for producing phosphorus oxychloride by oxygen oxidation process - Google Patents
Circulation flow reaction device for producing phosphorus oxychloride by oxygen oxidation process Download PDFInfo
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- CN102826522A CN102826522A CN2012103095894A CN201210309589A CN102826522A CN 102826522 A CN102826522 A CN 102826522A CN 2012103095894 A CN2012103095894 A CN 2012103095894A CN 201210309589 A CN201210309589 A CN 201210309589A CN 102826522 A CN102826522 A CN 102826522A
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- reaction kettle
- pocl3
- oxidation method
- interchanger
- coil pipe
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Abstract
The invention relates to a circulation flow reaction device for producing phosphorus oxychloride by an oxygen oxidation process. The circulation flow reaction device comprises a reaction kettle, a circulating pump and a heat exchanger, wherein a feed port is arranged in the left side of the top of the reaction kettle and a discharge port is arranged in the bottom end of the reaction kettle; the discharge port is provided with a connecting pipeline which is connected with the bottom end of the heat exchanger; the connecting pipeline, which is positioned between the discharge port in the bottom end of the reaction kettle and the bottom end of the heat exchanger, is provided with the circulating pump; the top of the heat exchanger is provided with a connecting pipeline which extends into a feed port arranged in the right side of the top of the reaction kettle and is connected with a material spray distributor arranged in the reaction kettle; and an air inlet is drilled in the center of the top of the reaction kettle and is internally provided with a vertical pipeline which extends into the near bottom of the reaction kettle and is connected with an oxygen distributor. According to the circulation flow reaction device, as the material spray distributor and the oxygen distributor are arranged in the reaction kettle, oxygen molecules can be effectively and fully in contact with phosphorus oxychloride molecules, therefore, the reaction probability is increased, the reaction time is shortened, and the yield and the device availability are increased.
Description
Technical field
The present invention relates to a kind of device of producing POCl3, relate in particular to a kind of circulation reaction unit of producing POCl3 with the dioxygen oxidation method.
Background technology
POCl3 is widely used in chemical industry, is the important source material of agricultural chemicals, fire retardant, dyestuff intermediate, and plurality of applications is also arranged in electronic industry and solar industry.
At home, great majority are produced POCl3 with the phosphorus trichloride chlorinolysis in the past, and progressively develop with phosphorus trichloride dioxygen oxidation method after the nineties last century.The characteristics that the dioxygen oxidation method is produced POCl3 be in phosphorus trichloride directly aerating oxygen react, this is a thermopositive reaction, because reaction is simple, can not produce by product, so easy to control and yield is higher.What use in the production is the placed in-line forms of many stills, oxygen is absorbed by phosphorus trichloride generate POCl3.But this reaction time consumption very long (needing 40-48 hour ability to accomplish), and some consumption of loosing of oxygen, utilization ratio is on the low side, in order to improve these shortcomings, proposes to raise the efficiency with circulation technology.The characteristics of circulation technology are to extract the material in the reaction kettle circularly out and import with recycle pump, material and oxygen are fully contacted produce reaction, and remove reaction heat through the outer interchanger of still, and reaction is carried out at a lower temperature.
Install generally only respond still, interchanger, recycle pump in the circulation technology of prior art; Only simply be provided with opening for feed and discharge port in its reaction kettle, material and oxygen mix reaction are insufficient, and the reaction probability is lower; PT is longer, and production efficiency has much room for improvement.
Summary of the invention
The present invention is directed to the deficiency of prior art, the circulation reaction unit with dioxygen oxidation method production POCl3 that a kind of material and oxygen reaction are abundant, the reaction times is short, production efficiency is high is provided.
The present invention is for solving the problems of the technologies described above; Following technical scheme is provided: a kind of circulation reaction unit with dioxygen oxidation method production POCl3, comprise reaction kettle, recycle pump, interchanger, described reaction kettle top left hand is provided with opening for feed; The bottom is provided with discharge port; Discharge port is provided with connecting pipeline and is connected with the interchanger bottom, and the connecting pipeline between said Polycondensation Reactor and Esterification Reactor end discharge port and interchanger bottom is provided with recycle pump, it is characterized in that the interchanger top is provided with the cycle stock mouth that a connecting pipeline stretches into right side, reaction kettle top; Be connected with the material spray sparger in being arranged at reaction kettle; Center, reaction kettle top offers inlet mouth, is provided with a vertical pipeline in the inlet mouth and stretches into the nearly bottom of reaction kettle, is connected with oxygen distribution ware.
Said material spray sparger is made up of vertical pipe and circular coil pipe; Be evenly equipped with through hole on the said circular coil pipe, as preferably, said circular coil pipe offers one group of per 2.7 degree in hole along per 2.7 degree on the center of circle and offers one group of through hole; One group of via count is 3; Preferably open 130 groups altogether, be distributed on the circular coil pipe, every group of hole of opening 3 φ 5mm.
Said oxygen distribution ware is circular coil pipe; Be evenly equipped with through hole on the said circular coil pipe; Offer one group of per 9.2 degree in hole as preferred circular coil pipe along per 9.2 degree on the center of circle and offer one group of through hole, one group of via count is 4, preferably opens 39 groups altogether; Be distributed on the circular coil pipe every group of hole of opening 4 φ 4mm.
As further improvement of the present invention, parallelly connectedly on the connecting pipeline between said Polycondensation Reactor and Esterification Reactor end discharge port and interchanger bottom be provided with two recycle pumps.Be provided with through this kind and effectively prevent effectively to shorten the device maintenance intervals, improve production efficient because of any recycle pump damages the situation that causes whole device to shut down.
As further improvement of the present invention, interchanger is a graphite heat exchanger.
As of the present invention preferred, described material spray sparger, oxygen distribution ware material are metal titanium.Can make device steady running over a long time and be not corroded through this kind setting, increase the service life.
Beneficial effect of the present invention: the present invention effectively fully makes oxygen molecule contact with the phosphorus trichloride molecule through material spray sparger, oxygen distribution ware are set in reaction kettle, improves the reaction probability; Shorten the reaction times, make the reaction that originally needs ability completion in 40-48 hour, shorten to completion in 8-10 hour; Improved output, also improved plant factor, owing to accelerated speed of response; The temperature of reaction that originally was controlled at 80-90 ℃ can be reduced to 70-75 ℃, has increased reaction safety, because circulating reaction can make full use of oxygen; Make the oxygen depletion amount of producing POCl3 per ton drop to consumption 105 kg per ton from the 110-113 kilogram; Near 104 kilograms of levels of theoretical value, improved oxygen utilization rate, owing to used graphite heat exchanger; Heat exchange performance is better, and thermal conductivity ratio stainless steel, the carbon steel of graphite are many greatly.The interchanger of general steel often is welded with many steel pipes, can produce many weld seams, and phosphorus trichloride, POCl3 all have strong corrodibility; Be not suitable for using; And graphite material chemicalstability strong (inert), machining property is good, is highly suitable in this project to use.
Description of drawings
Fig. 1 is a structural representation of the present invention.
Fig. 2 is the oxygen distribution ware front view.
Fig. 3 is the vertical view of Fig. 2.
Fig. 4 is the A-A sectional view of Fig. 3.
Fig. 5 is a material spray sparger front view.
Fig. 6 is the vertical view of Fig. 5.
Fig. 7 is the B-B sectional view of Fig. 6.
Embodiment
A kind of circulation reaction unit with dioxygen oxidation method production POCl3 comprises reaction kettle 001, recycle pump 002, interchanger 003, and described reaction kettle 001 top left hand is provided with opening for feed 011; The bottom is provided with discharge port 012, and discharge port 012 is provided with connecting pipeline 004 and is connected with interchanger 003 bottom, and the connecting pipeline 004 between said reaction kettle 001 bottom discharge port 012 and interchanger 003 bottom is provided with recycle pump 002; Interchanger 003 top is provided with the cycle stock mouth 013 that a connecting pipeline 004 stretches into right side, reaction kettle 001 top, is connected with material spray sparger 005 in being arranged at reaction kettle 001, and center, reaction kettle 001 top offers inlet mouth 014; Be provided with a vertical pipeline 015 in the inlet mouth 014 and stretch into the nearly bottom of reaction kettle 001, be connected, parallelly connectedly on the connecting pipeline 004 between said reaction kettle 001 bottom discharge port 012 and interchanger 003 bottom be provided with two recycle pumps 002 with oxygen distribution ware 006; Material spray sparger 005 is made up of vertical pipe 051 and circular coil pipe 052; 052 is evenly equipped with through hole 053 on the said circular coil pipe, and it is 3 that said circular coil pipe 052 offers 053, one group of through hole of one group of through hole, 053 number along per 2.7 degree on the center of circle; Preferably open 130 groups; Be distributed on the circular coil pipe, every group of hole of opening 3 φ 5mm, oxygen distribution ware 006 is circular coil pipe; Be evenly equipped with through hole 061 on the said circular coil pipe; It is 4 that said circular coil pipe offers 061, one group of through hole of one group of through hole, 061 number along per 9.2 degree on the center of circle, preferably opens 39 groups; Be distributed on the circular coil pipe every group of hole of opening 4 φ 4mm.
Interchanger 003 is a graphite heat exchanger, and described material spray sparger 005, oxygen distribution ware 006 material are metal titanium.
Present embodiment is specifically realized through following method: in reaction kettle, add the phosphorus trichloride measure, open recycle pump 002 and be preferably two recycle pumps 002 and be used alternatingly, material is sprayed from material spray sparger 005.In addition, after LOX converts gox to through vaporizer, also in oxygen distribution ware 006, spray, generate POCl3 and emit heat with the phosphorus trichloride reaction.Control oxygen flow 14-15m3/h between the reaction period.When recycle stock passed through graphite heat exchanger, the refrigerant in the heat transferred graphite heat exchanger, temperature was at 70-75 ℃ in the control reaction kettle 001; React after 8 hours; When temperature in the kettle begins to descend, reduce oxygen-supply quantity gradually, through sampling analysis; When analyzing boiling range＞97.5%, confirm that reaction finishes.
Claims (8)
1. circulation reaction unit of producing POCl3 with the dioxygen oxidation method; Comprise reaction kettle, recycle pump, interchanger; Described reaction kettle top left hand is provided with opening for feed, and the bottom is provided with discharge port, and discharge port is provided with connecting pipeline and is connected with the interchanger bottom; Connecting pipeline between said Polycondensation Reactor and Esterification Reactor end discharge port and interchanger bottom is provided with recycle pump; It is characterized in that the interchanger top is provided with the cycle stock mouth that a connecting pipeline stretches into right side, reaction kettle top, be connected that center, reaction kettle top offers inlet mouth with material spray sparger in being arranged at reaction kettle; Be provided with a vertical pipeline in the inlet mouth and stretch into the nearly bottom of reaction kettle, be connected with oxygen distribution ware.
2. according to claim 1ly a kind ofly produce the circulation reaction unit of POCl3, it is characterized in that parallelly connectedly on the connecting pipeline between said Polycondensation Reactor and Esterification Reactor end discharge port and interchanger bottom being provided with two recycle pumps with the dioxygen oxidation method.
3. according to claim 1ly a kind ofly produce the circulation reaction unit of POCl3, it is characterized in that the material spray sparger is made up of vertical pipe and circular coil pipe, be evenly equipped with through hole on the said circular coil pipe with the dioxygen oxidation method.
4. a kind of circulation reaction unit with dioxygen oxidation method production POCl3 according to claim 3 is characterized in that said circular coil pipe offers one group of through hole along per 2.7 degree on the center of circle, and one group of via count is 3.
5. a kind of circulation reaction unit with dioxygen oxidation method production POCl3 according to claim 1 is characterized in that oxygen distribution ware is circular coil pipe, is evenly equipped with through hole on the said circular coil pipe.
6. a kind of circulation reaction unit with dioxygen oxidation method production POCl3 according to claim 5 is characterized in that said circular coil pipe offers one group of through hole along per 9.2 degree on the center of circle, and one group of via count is 4.
7. a kind of circulation reaction unit with dioxygen oxidation method production POCl3 according to claim 1 is characterized in that interchanger is a graphite heat exchanger.
8. a kind of circulation reaction unit with dioxygen oxidation method production POCl3 according to claim 1 is characterized in that described material spray sparger, oxygen distribution ware material are metal titanium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103095894A CN102826522A (en) | 2012-08-28 | 2012-08-28 | Circulation flow reaction device for producing phosphorus oxychloride by oxygen oxidation process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103095894A CN102826522A (en) | 2012-08-28 | 2012-08-28 | Circulation flow reaction device for producing phosphorus oxychloride by oxygen oxidation process |
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| CN102826522A true CN102826522A (en) | 2012-12-19 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012103095894A Pending CN102826522A (en) | 2012-08-28 | 2012-08-28 | Circulation flow reaction device for producing phosphorus oxychloride by oxygen oxidation process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103303883A (en) * | 2013-05-08 | 2013-09-18 | 湖北泰盛化工有限公司 | Production process of phosphorus oxychloride |
| CN107827781A (en) * | 2017-11-15 | 2018-03-23 | 山东尚舜化工有限公司 | The production technology and equipments of continuous production diphenylguanidine |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3052520A (en) * | 1957-11-21 | 1962-09-04 | Fmc Corp | Manufacture of phosphorus oxychloride |
| CN101010134A (en) * | 2004-09-02 | 2007-08-01 | 伊斯曼化学公司 | Optimized liquid-phase oxidation |
| CN202754804U (en) * | 2012-08-28 | 2013-02-27 | 滨海雅克化工有限公司 | Loop reaction device for producing phosphorus oxychloride in oxidation style with oxygen |
-
2012
- 2012-08-28 CN CN2012103095894A patent/CN102826522A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3052520A (en) * | 1957-11-21 | 1962-09-04 | Fmc Corp | Manufacture of phosphorus oxychloride |
| CN101010134A (en) * | 2004-09-02 | 2007-08-01 | 伊斯曼化学公司 | Optimized liquid-phase oxidation |
| CN202754804U (en) * | 2012-08-28 | 2013-02-27 | 滨海雅克化工有限公司 | Loop reaction device for producing phosphorus oxychloride in oxidation style with oxygen |
Non-Patent Citations (1)
| Title |
|---|
| 周明昊等: "液体喷射环流反应器的研究（III）-三氯氧磷合成中氧化过程的应用", 《农药》, vol. 47, no. 8, 31 August 2008 (2008-08-31), pages 566 - 568 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103303883A (en) * | 2013-05-08 | 2013-09-18 | 湖北泰盛化工有限公司 | Production process of phosphorus oxychloride |
| CN103303883B (en) * | 2013-05-08 | 2015-12-02 | 湖北泰盛化工有限公司 | A kind of production technique of phosphorus oxychloride |
| CN107827781A (en) * | 2017-11-15 | 2018-03-23 | 山东尚舜化工有限公司 | The production technology and equipments of continuous production diphenylguanidine |
| CN107827781B (en) * | 2017-11-15 | 2020-08-21 | 山东尚舜化工有限公司 | Production process and equipment for continuously producing diphenylguanidine |
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Application publication date: 20121219 |