CN202107526U - Circulation process system for producing phosphorus oxychloride by pure oxygen oxidation of phosphorus trichloride - Google Patents
Circulation process system for producing phosphorus oxychloride by pure oxygen oxidation of phosphorus trichloride Download PDFInfo
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- CN202107526U CN202107526U CN2011202040999U CN201120204099U CN202107526U CN 202107526 U CN202107526 U CN 202107526U CN 2011202040999 U CN2011202040999 U CN 2011202040999U CN 201120204099 U CN201120204099 U CN 201120204099U CN 202107526 U CN202107526 U CN 202107526U
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Abstract
The utility model belongs to the field of chemical equipment, which relates to a circulation process system for producing phosphorus oxychloride by the pure oxygen oxidation of phosphorus trichloride. The circulation process system comprises a circulation reactor, a jet reactor, a tubular heat exchanger and a circulation pump. The tubular heat exchanger comprises an upper end cover, a lower end cover, tube plates, a cylinder body and a heat exchange tube. The two ends of the cylinder body are respectively equipped with a through tube plate. The through tube plates are welded with the cylinder wall at the two ends of the cylinder body so as to seal the cylinder body. The length of the heat exchange tube is greater than the height of the cylinder body. The two ends of the heat exchange tube respectively passing through the through tube plates are welded with the tube plates. The heat exchange tube and the through tube plates are expanded and sealed through a tube expander. According to the utility model, safety hazards caused by the leakage of the welded part of a heat exchange tube in the circulation process system for producing phosphorus oxychloride by the pure oxygen oxidation of phosphorus trichloride in the prior art are effectively avoided. Meanwhile, the production process is optimized and the reliability and the security of the process system are greatly improved. The circulation process system is also low in investment, fast in effect, convenient in transformation, simple and practicable.
Description
Technical field
The utility model belongs to the chemical plant field, relates to a kind of phosphorus trichloride " pure oxygen oxidation style " and produces POCl3 circulation process system.
Background technology
Wurtz was by PCl in 1847
5Prepared POCl
3, developed many methods later on again, like PCl
3Oxidation style (oxygenant of research has air, oxygen, ozone, Potcrate, phosphorus thiochloride, tin anhydride, sulfuryl chloride, nitrogen trichloride etc.), PCl
3Chlorinolysis, trichlorine dibrominated phosphorus hydrolysis method, phosphorus oxide chlorination and PCl
5Hydrolysis method etc.
The reaction of the synthetic POCl3 of phosphorus trichloride " pure oxygen oxidation style " is strong heat release long response time.The factor that influences speed of response mainly contains two: the transmission of oxygen molecule and the formation of oxyradical
[1]Macro manifestations is the rate of heat transfer between the medium.Phosphorus trichloride " pure oxygen oxidation style " POCl3 circulation technology, as shown in Figure 1, its major equipment is: loop reactor, injection reactor, interchanger and recycle pump are formed.This technology is from improving speed of reaction and improving two aspects of conversion unit exchange capability of heat; In processing unit; Especially creationary the equipment----interchanger that independently has higher heat transfer efficiency that adopted; Significantly strengthen the exchange transmission of quality and heat, realized the efficient utilization of oxygen, avoided the discharging of tail gas.
But the interchanger in this technology has adopted traditional structure, and is as shown in Figure 2, that is: heat transfer tube two ends and cylindrical shell and tube sheet directly weld together; Weld seam is more, and simultaneously, the variation of heat exchange temperature will make the frequent generation of the heat transfer tube shrinkage phenomenon that expands; Long term operation causes weld leakage easily and heat exchange material (POCl3) contacts with quench liquid (water), and the composition of heat-transmission material is mainly POCl3 in this technology, and it is met water and then fiercely decomposes; Produce a large amount of heat and white cigarette, even blast.In case weld seam leaks, dangerous with causing POCl3 and water coolant in the interchanger directly to contact to produce, so there is serious potential safety hazard.
The utility model content
The purpose of the utility model is the above-mentioned deficiency to prior art, provides a kind of phosphorus trichloride " pure oxygen oxidation style " to produce POCl3 circulation process system.
A kind of phosphorus trichloride " pure oxygen oxidation style " is produced POCl3 circulation process system, comprises loop reactor, injection reactor, tubular heat exchange and recycle pump; The pneumatic outlet of injection reactor links to each other with the gas feed of loop reactor through pipeline; The discharge port of loop reactor is through the opening for feed of pipe connection recycle pump; The discharge port of recycle pump links to each other with the material inlet and the pan tank of tubular heat exchange respectively through pipeline; The material outlet of tubular heat exchange links to each other with the material inlet of injection reactor through pipeline, forms a round-robin system; Described tubular heat exchange comprises upper end cover, lower end cover, tube sheet, cylindrical shell, heat transfer tube; The upper end cover top is provided with material outlet; The lower end cover bottom is provided with material inlet; Two end caps are respectively equipped with a tube sheet with respect to cylindrical shell one end, and tube sheet is connected through flange with end cap, and the cylindrical shell bottom is provided with water-in, emergent water port, cylindrical shell top and is provided with water outlet, venting port; The cylindrical shell two ends respectively are provided with a poling plate, the barrel welded seal at poling plate and cylindrical shell two ends, and the length of heat transfer tube is greater than the height of cylindrical shell, and its two ends are passed poling plate and tube sheet welding respectively, and heat transfer tube and poling plate adopt electric tube expander swelling sealing.
The barrel of tubular heat exchange is provided with traverse baffle.
The barrel of tubular heat exchange is provided with the fixedly pull bar of traverse baffle.
Beneficial effect:
The utility model is from traditional tubular heat exchange, through the poling plate is set, and prolongs heat transfer tube length, and the welding portion that heat transfer tube is connected with tube sheet does not contact with cylindrical shell.Even welding portion occurs owing to work long hours take place to leak and the dangerous phenomenon that heat exchange material and interchanger internal cooling water directly contact also can not occur; In addition; The cylindrical shell downside is provided with emergent water port in case tubulation can in time be handled when taking place to leak, and has improved the safe reliability that equipment uses greatly.The utility model has effectively solved existing phosphorus trichloride " pure oxygen oxidation style " and has produced in the POCl3 circulation process system because the heat transfer tube weld part leaks the security hidden trouble that is produced; Both optimized technology; The safety and the security of process system have been improved again greatly, less investment, instant effect; And it is convenient, simple to transform.
Description of drawings
The synthetic POCl3 production system figure of the phosphorus trichloride " pure oxygen oxidation style " of Fig. 1, the traditional tubular heat exchange of use.
15 is loop reactor, and 16 is injection reactor, and 17 is tubular heat exchange, and 18 is recycle pump.
Fig. 2, traditional heat exchangers structural representation.
1 is tube sheet, and 2 is heat transfer tube, and 4 is cylindrical shell, and 5 is traverse baffle, and 6 is pull bar, and 7-1 is a upper end cover, and 7-2 is a lower end cover, and 8 is material outlet, and 9 is material inlet, and 10 is water-in, and 11 is water outlet, and 12 are emergent water port, and 13 is venting port, and 14 is flange.
Fig. 3, embodiment 1 heat exchanger structure synoptic diagram.
1 is tube sheet, and 2 is heat transfer tube, and 4 is cylindrical shell, and 3 is the poling plate, and 5 is traverse baffle; 6 is pull bar, and 7-1 is a upper end cover, and 7-2 is a lower end cover, and 8 is material outlet, and 9 is material inlet; 10 is water-in, and 11 is water outlet, and 12 are emergent water port, and 13 is venting port, and 14 is flange.
Fig. 4, embodiment 1 phosphorus trichloride " pure oxygen oxidation style " are produced POCl3 circulation process system synoptic diagram.
15 is loop reactor, and 16 is injection reactor, and 17 is tubular heat exchange, and 18 is recycle pump.
Embodiment
A kind of phosphorus trichloride " pure oxygen oxidation style " is produced POCl3 circulation process system (Fig. 4), comprises loop reactor 15, injection reactor 16, tubular heat exchange 17 and recycle pump 18; The pneumatic outlet of injection reactor 16 links to each other with the gas feed of loop reactor 15 through pipeline; The discharge port of loop reactor 15 is through the opening for feed of pipe connection recycle pump 18; The discharge port of recycle pump 18 links to each other with the material inlet 9 and the pan tank of tubular heat exchange 17 respectively through pipeline; The material outlet 8 of tubular heat exchange 17 links to each other with the material inlet of injection reactor 16 through pipeline, forms a round-robin system.Tubular heat exchange 17; Comprise upper end cover 7-1, lower end cover 7-2, tube sheet 1, cylindrical shell 4, heat transfer tube 2; Upper end cover 7-1 top is provided with material outlet 8, and lower end cover 7-2 bottom is provided with 9, two end caps of material inlet and is respectively equipped with a tube sheet 1 with respect to cylindrical shell 4 one ends; Tube sheet 1 is connected through flange 14 with end cap, and cylindrical shell 4 bottoms are provided with water-in 10, emergent water port 10, cylindrical shell 4 tops and are provided with water outlet 10, venting port 13; Cylindrical shell 4 two ends respectively are provided with a poling plate 1, and the length of heat transfer tube 2 is greater than the height of cylindrical shell 4, and its two ends are passed poling plate 1 and tube sheet 1 welding respectively, and heat transfer tube 2 adopts electric tube expander swelling sealing with poling plate 1.
Cylindrical shell 4 set inside traverse baffles 5.
Cylindrical shell 4 set inside are the pull bar 6 of traverse baffle 5 fixedly.
Working state of system:
1, opens loop reactor chuck water coolant and loop reactor phosphorus trichloride imported valve, put into loop reactor to the phosphorus trichloride that has measured, close the phosphorus trichloride feed valve.
2, open loop reactor bottom valve and pump inlet valve, start recycle pump, slow ON cycle pump discharge valve circulates material simultaneously, treat that the material circulation is normal after, open into injection reactor oxygen flow meter and valve, control oxygen flow 50～60m
3/ h after reaction in several minutes starts, when temperature of charge rises to 70 ℃, opens the interchanger water coolant, opens big loop reactor oxygen-supply quantity then, and its oxygen-supply quantity is looked and will be controlled according to loop reactor internal pressure and temperature.Make the loop reactor internal pressure be controlled at 0.15Mpa～0.20Mpa, temperature is controlled at 70 ℃～80 ℃.After keeping 5 hours reaction times, when the loop reactor internal pressure begins to rise, when temperature begins to descend, reduces oxygen-supply quantity, fall that to open be 20～50m
3/ h.After branch folding to the reaction of taking a sample per half a hour simultaneously reached terminal point, discharging was to pan tank.
POCl3 gets into heat transfer tube 2 by the material inlet 9 of lower end cover 7-2 bottom.Being full of in the cylindrical shell 4 is used to exchange heat pipe and carries out refrigerative water, and POCl3 and heat transfer tube tube wall carry out heat exchange, in the process through heat transfer tube, obtains cooling, discharges tubular heat exchange from the material outlet 8 at upper end cover 7-1 top.Cylindrical shell 4 is provided with water-in 10, water outlet 11; Can change or the water yield is regulated the intravital water of tube; The venting port 13 that is provided with on the cylindrical shell 4 is used for regularly discharging the waste gas that produces in the cylindrical shell; The cylindrical shell downside is provided with emergent water port 12 in case heat transfer tube 2 can in time be handled when taking place to leak, and has improved the safe reliability that equipment uses greatly.
Each parts of tubular heat exchange are made the material table
| Parts | Material |
| Heat transfer tube | 316L stainless steel or titanium pipe |
| Tube sheet | The 316L stainless steel |
| The poling plate | The Q235B carbon steel |
| Cylindrical shell | The Q235B carbon steel |
Claims (3)
1. a phosphorus trichloride " pure oxygen oxidation style " is produced POCl3 circulation process system, comprises loop reactor (15), injection reactor (16), tubular heat exchange (17) and recycle pump (18); The pneumatic outlet of injection reactor (16) links to each other with the gas feed of loop reactor (15) through pipeline; The discharge port of loop reactor (15) is through the opening for feed of pipe connection recycle pump (18); The discharge port of recycle pump (18) links to each other with the material inlet (9) and the pan tank of tubular heat exchange (17) respectively through pipeline; The material outlet (8) of tubular heat exchange (17) links to each other with the material inlet of injection reactor (16) through pipeline, forms a round-robin system; Described tubular heat exchange (17) comprises upper end cover (7-1), lower end cover (7-2), tube sheet (1), cylindrical shell (4), heat transfer tube (2); Upper end cover (7-1) top is provided with material outlet (8); Lower end cover (7-2) bottom is provided with material inlet (9); Two end caps (7-1,7-2) are respectively equipped with a tube sheet (1) with respect to cylindrical shell (4) one ends; Tube sheet (1) is connected through flange (14) with end cap, and cylindrical shell (4) bottom is provided with water-in (10), emergent water port (12), cylindrical shell (4) top and is provided with water outlet (11), venting port (13); It is characterized in that cylindrical shell (4) two ends respectively are provided with a poling plate (3); The barrel welded seal at poling plate (3) and cylindrical shell (4) two ends; The length of heat transfer tube (2) is greater than the height of cylindrical shell (4); Its two ends are passed poling plate (3) and tube sheet (1) welding respectively, and heat transfer tube (2) adopts electric tube expander swelling sealing with poling plate (3).
2. phosphorus trichloride according to claim 1 " pure oxygen oxidation style " is produced POCl3 circulation process system, it is characterized in that cylindrical shell (4) the set inside traverse baffle (5) of tubular heat exchange (17).
3. phosphorus trichloride according to claim 1 " pure oxygen oxidation style " is produced POCl3 circulation process system, and cylindrical shell (4) set inside that it is characterized in that tubular heat exchange (17) is the pull bar (6) of traverse baffle (5) fixedly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202040999U CN202107526U (en) | 2011-06-16 | 2011-06-16 | Circulation process system for producing phosphorus oxychloride by pure oxygen oxidation of phosphorus trichloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202040999U CN202107526U (en) | 2011-06-16 | 2011-06-16 | Circulation process system for producing phosphorus oxychloride by pure oxygen oxidation of phosphorus trichloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN202107526U true CN202107526U (en) | 2012-01-11 |
Family
ID=45432970
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011202040999U Expired - Fee Related CN202107526U (en) | 2011-06-16 | 2011-06-16 | Circulation process system for producing phosphorus oxychloride by pure oxygen oxidation of phosphorus trichloride |
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| Country | Link |
|---|---|
| CN (1) | CN202107526U (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106008142A (en) * | 2016-06-29 | 2016-10-12 | 山东道可化学有限公司 | Device and method for preparing 1,3-bromochloropropane |
| CN113694852A (en) * | 2021-09-30 | 2021-11-26 | 南京佳华工程技术有限公司 | Continuous synthesis process and equipment for phosphorus trichloride |
| CN116237006A (en) * | 2023-03-30 | 2023-06-09 | 徐州宏达新能源科技有限公司 | Energy-saving production device and production method for high-purity phosphorus pentachloride |
-
2011
- 2011-06-16 CN CN2011202040999U patent/CN202107526U/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106008142A (en) * | 2016-06-29 | 2016-10-12 | 山东道可化学有限公司 | Device and method for preparing 1,3-bromochloropropane |
| CN106008142B (en) * | 2016-06-29 | 2018-09-07 | 山东道可化学有限公司 | A kind of device and method preparing 1,3- bromo-chloropropanes |
| CN113694852A (en) * | 2021-09-30 | 2021-11-26 | 南京佳华工程技术有限公司 | Continuous synthesis process and equipment for phosphorus trichloride |
| CN116237006A (en) * | 2023-03-30 | 2023-06-09 | 徐州宏达新能源科技有限公司 | Energy-saving production device and production method for high-purity phosphorus pentachloride |
| CN116237006B (en) * | 2023-03-30 | 2024-05-24 | 徐州宏达新能源科技有限公司 | Energy-saving production device and production method for high-purity phosphorus pentachloride |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: YANCHENG DAMING CHEMICAL CO., LTD. Free format text: FORMER OWNER: JIANGSU DAMING TECHNOLOGY CO., LTD. Effective date: 20130826 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 214204 WUXI, JIANGSU PROVINCE TO: 224600 YANCHENG, JIANGSU PROVINCE |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20130826 Address after: 224600 Jiangsu province Yancheng City Xiangshui Chenjiagang chemical concentration area Patentee after: Yancheng Daming Chemical Co.,Ltd. Address before: 214204, Jiangsu, Wuxi Yixing Xinjie Street joint village Patentee before: Jiangsu Daming Technology Co., Ltd. |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120111 Termination date: 20160616 |