CN202754804U - Loop reaction device for producing phosphorus oxychloride in oxidation style with oxygen - Google Patents
Loop reaction device for producing phosphorus oxychloride in oxidation style with oxygen Download PDFInfo
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- CN202754804U CN202754804U CN201220430404.0U CN201220430404U CN202754804U CN 202754804 U CN202754804 U CN 202754804U CN 201220430404 U CN201220430404 U CN 201220430404U CN 202754804 U CN202754804 U CN 202754804U
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- phosphorus oxychloride
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Abstract
Disclosed is a loop reaction device for producing phosphorus oxychloride in an oxidation style with oxygen. The loop reaction device for producing the phosphorus oxychloride in the oxidation style with the oxygen comprises a reaction still, a circulating pump and a heat exchanger. The left side of the upper end of the reaction still is provided with a feed inlet and the bottom of the reaction still is provided with a discharge hole. A connecting pipeline is arranged on the discharge hole and is connected with the bottom of the heat exchanger. The circulating pump is arranged on the connecting pipeline between the discharge hole of the bottom of the reaction still and the bottom of the heat exchanger. The upper portion of the heat exchanger is provided with the connecting pipeline which is stretched into a feed inlet of the right side of the upper end of the reaction still and is connected with a material spray distributor arranged in the reaction still. The center of the upper end of the reaction still is provided with a gas inlet which is provided with a vertical pipeline which is almost stretched into the bottom of the reaction still and is connected with an oxygen distributor. Because the reaction still is provided with the material spray distributor and the oxygen distributor, oxygen molecules can fully contact phosphorus trichloride molecules, ratios of reactions are improved, reaction time is shorten, yield is increased and rate of equipment utilization is increased.
Description
Technical field
The utility model relates to a kind of device of producing phosphorus oxychloride, relates in particular to a kind of circulation reaction unit with dioxygen oxidation method production phosphorus oxychloride.
Background technology
Phosphorus oxychloride is widely used in chemical industry, is the important source material of agricultural chemicals, fire retardant, dyestuff intermediate, and a lot of application are also arranged in electronic industry and solar industry.
At home, great majority progressively developed the phosphorus trichloride dioxygen oxidation method of using last century with phosphorus trichloride chlorinolysis production phosphorus oxychloride after the nineties in the past.The characteristics of dioxygen oxidation method production phosphorus oxychloride are directly to pass into oxygen to react in phosphorus trichloride, and 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 form of many still series connection, oxygen is absorbed by phosphorus trichloride generate phosphorus oxychloride.But this reaction time consumption very long (just needing to finish in 40-48 hour), and some loose consumption of oxygen, utilization ratio is on the low side, in order to improve these shortcomings, proposes to raise the efficiency with circulation technique.The characteristics of circulation technique are with recycle pump the Matter Transfer in the reactor reciprocally to be extracted out and inputted, and material and oxygen are fully contacted produce reaction, and by the outer interchanger of still reaction heat is removed, and reaction is carried out at a lower temperature.
Install generally only respond still, interchanger, recycle pump in the circulation technique of prior art, only simply be provided with opening for feed and discharge port in its reactor, material and oxygen mix reaction are insufficient, and the reaction probability is lower, production time is longer, and production efficiency has much room for improvement.
Summary of the invention
The utility model provides the circulation reaction unit with dioxygen oxidation method production phosphorus oxychloride that a kind of material and oxygen reaction are abundant, the reaction times is short, production efficiency is high for the deficiencies in the prior art.
The utility model is for solving the problems of the technologies described above, provide following technical scheme: a kind of circulation reaction unit with dioxygen oxidation method production phosphorus oxychloride, comprise reactor, recycle pump, interchanger, described reactor top left hand is provided with opening for feed, the bottom is provided with discharge port, being provided with connecting pipeline on the discharge port is connected with the interchanger bottom, be provided with recycle pump on the connecting pipeline between described Polycondensation Reactor and Esterification Reactor end discharge port and interchanger bottom, it is characterized in that the interchanger top is provided with the cycle stock mouth that a connecting pipeline stretches into right side, reactor top, be connected with the material spray sparger in being arranged at reactor, center, reactor top offers inlet mouth, be provided with a vertical pipeline in the inlet mouth and stretch into the nearly bottom of reactor, be connected with oxygen distribution ware.
Described material spray sparger is comprised of vertical pipe and circular coil pipe, be evenly equipped with through hole on the described circular coil pipe, as preferably, described 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 altogether 130 groups, be distributed on the circular coil pipe, every group of hole of opening 3 φ 5mm.
Described oxygen distribution ware is circular coil pipe, be evenly equipped with through hole on the described 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 open altogether 39 groups, be distributed on the circular coil pipe every group of hole of opening 4 φ 4mm.
As further improvement of the utility model, two recycle pumps have been arranged in parallel on the connecting pipeline between described Polycondensation Reactor and Esterification Reactor end discharge port and interchanger bottom.Arrange by this kind and effectively to prevent from effectively shortening the device maintenance intervals because any recycle pump damages the situation that causes whole device to shut down, improve integral production efficient.
As further improvement of the utility model, interchanger is graphite heat exchanger.
As of the present utility model preferred, described material spray sparger, oxygen distribution ware material are metal titanium.Can make over a long time steady running of device and be not corroded by this kind setting, increase the service life.
The beneficial effects of the utility model: the utility model is by arranging the material spray sparger in reactor, oxygen distribution ware, oxygen molecule can be contacted with the phosphorus trichloride molecule, improve the reaction probability, Reaction time shorten, make the reaction that originally needed just can finish in 40-48 hour, shortening to 8-10 hour finishes, improved output, also improved plant factor, owing to having accelerated speed of response, the temperature of reaction that originally was controlled at 80-90 ℃ can be reduced to 70-75 ℃, increased the security of reaction, because circulating reaction can take full advantage of oxygen, make the oxygen depletion amount of producing phosphorus oxychloride 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 having used graphite heat exchanger, heat exchange performance is better, the thermal conductivity ratio stainless steel of graphite, carbon steel is many greatly.The interchanger of general steel often forms with many steel-pipe weldings, can produce many weld seams, and phosphorus trichloride, phosphorus oxychloride have strong corrodibility, be not suitable for using, and graphite material chemical stability strong (inert), machining property is good, is highly suitable in this project to use.
Description of drawings
Fig. 1 is structural representation of the present utility model.
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 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 phosphorus oxychloride, comprise reactor 001, recycle pump 002, interchanger 003, described reactor 001 top left hand is provided with opening for feed 011, the bottom is provided with discharge port 012, being provided with connecting pipeline 004 on the discharge port 012 is connected with interchanger 003 bottom, be provided with recycle pump 002 on the connecting pipeline 004 between described reactor 001 bottom discharge port 012 and interchanger 003 bottom, interchanger 003 top is provided with the cycle stock mouth 013 that a connecting pipeline 004 stretches into right side, reactor 001 top, be connected with the material spray sparger 005 in being arranged at reactor 001, center, reactor 001 top offers inlet mouth 014, be provided with a vertical pipeline 015 in the inlet mouth 014 and stretch into reactor 001 nearly bottom, be connected with oxygen distribution ware 006, two recycle pumps 002 have been arranged in parallel on the connecting pipeline 004 between described reactor 001 bottom discharge port 012 and interchanger 003 bottom, material spray sparger 005 is comprised of vertical pipe 051 and circular coil pipe 052,052 is evenly equipped with through hole 053 on the described circular coil pipe, described circular coil pipe 052 offers one group of through hole 053 along per 2.7 degree on the center of circle, one group of through hole 053 number is 3, 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 described circular coil pipe, described circular coil pipe offers one group of through hole 061 along per 9.2 degree on the center of circle, one group of through hole 061 number is 4, preferably open 39 groups, be distributed on the circular coil pipe every group of hole of opening 4 φ 4mm.
Interchanger 003 is graphite heat exchanger, and described material spray sparger 005, oxygen distribution ware 006 material are metal titanium.
The present embodiment is specifically realized by the following method: add the phosphorus trichloride measure in reactor, 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 liquid oxygen converts gaseous oxygen to through vaporizer, also from oxygen distribution ware 006 interior ejection, generate phosphorus oxychloride and emit heat with the phosphorus trichloride reaction.Control oxygen flow 14-15m3/h between the reaction period.When recycle stock passes through graphite heat exchanger, the refrigerant in the heat transferred graphite heat exchanger, control reactor 001 interior temperature is at 70-75 ℃, react after 8 hours, when temperature in the kettle begins to descend, reduce gradually oxygen-supply quantity, by sampling analysis, when analyzing boiling range＞97.5%, determine that reaction finishes.
Claims (8)
1. circulation reaction unit with dioxygen oxidation method production phosphorus oxychloride, comprise reactor, recycle pump, interchanger, described reactor top left hand is provided with opening for feed, the bottom is provided with discharge port, being provided with connecting pipeline on the discharge port is connected with the interchanger bottom, be provided with recycle pump on the connecting pipeline between described Polycondensation Reactor and Esterification Reactor end discharge port and interchanger bottom, it is characterized in that the interchanger top is provided with the cycle stock mouth that a connecting pipeline stretches into right side, reactor top, be connected with the material spray sparger in being arranged at reactor, center, reactor top offers inlet mouth, be provided with a vertical pipeline in the inlet mouth and stretch into the nearly bottom of reactor, be connected with oxygen distribution ware.
2. a kind of circulation reaction unit with dioxygen oxidation method production phosphorus oxychloride according to claim 1 is characterized in that being arranged in parallel on the connecting pipeline between described Polycondensation Reactor and Esterification Reactor end discharge port and interchanger bottom two recycle pumps.
3. a kind of circulation reaction unit with dioxygen oxidation method production phosphorus oxychloride according to claim 1 is characterized in that the material spray sparger is comprised of vertical pipe and circular coil pipe, is evenly equipped with through hole on the described circular coil pipe.
4. a kind of circulation reaction unit with dioxygen oxidation method production phosphorus oxychloride according to claim 3 is characterized in that described 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 phosphorus oxychloride according to claim 1 is characterized in that oxygen distribution ware is circular coil pipe, is evenly equipped with through hole on the described circular coil pipe.
6. a kind of circulation reaction unit with dioxygen oxidation method production phosphorus oxychloride according to claim 5 is characterized in that described 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 phosphorus oxychloride according to claim 1 is characterized in that interchanger is graphite heat exchanger.
8. a kind of circulation reaction unit with dioxygen oxidation method production phosphorus oxychloride 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 |
|---|---|---|---|
| CN201220430404.0U CN202754804U (en) | 2012-08-28 | 2012-08-28 | Loop reaction device for producing phosphorus oxychloride in oxidation style with oxygen |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201220430404.0U CN202754804U (en) | 2012-08-28 | 2012-08-28 | Loop reaction device for producing phosphorus oxychloride in oxidation style with oxygen |
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| Publication Number | Publication Date |
|---|---|
| CN202754804U true CN202754804U (en) | 2013-02-27 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201220430404.0U Expired - Lifetime CN202754804U (en) | 2012-08-28 | 2012-08-28 | Loop reaction device for producing phosphorus oxychloride in oxidation style with oxygen |
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| CN (1) | CN202754804U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826522A (en) * | 2012-08-28 | 2012-12-19 | 滨海雅克化工有限公司 | Circulation flow reaction device for producing phosphorus oxychloride by oxygen oxidation process |
| CN103303883A (en) * | 2013-05-08 | 2013-09-18 | 湖北泰盛化工有限公司 | Production process of phosphorus oxychloride |
-
2012
- 2012-08-28 CN CN201220430404.0U patent/CN202754804U/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826522A (en) * | 2012-08-28 | 2012-12-19 | 滨海雅克化工有限公司 | Circulation flow reaction device for producing phosphorus oxychloride by oxygen oxidation process |
| 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 |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term |
Granted publication date: 20130227 |
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| CX01 | Expiry of patent term |