CN103449389A - Phosphorus trichloride production method and device capable of automatically supplementing gas - Google Patents
Phosphorus trichloride production method and device capable of automatically supplementing gas Download PDFInfo
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- CN103449389A CN103449389A CN2013103965469A CN201310396546A CN103449389A CN 103449389 A CN103449389 A CN 103449389A CN 2013103965469 A CN2013103965469 A CN 2013103965469A CN 201310396546 A CN201310396546 A CN 201310396546A CN 103449389 A CN103449389 A CN 103449389A
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Abstract
The invention provides a phosphorus trichloride production method and device capable of automatically supplementing gas. A nitrogen gas supplementing system and a gas regulating valve are adopted to control system pressure to 0-1 MPa, and the generation of such side reactions as phosphorus trichloride and water vapor react to generate phosphate is effectively reduced on the production basis of optimizing the process. Specifically, the nitrogen gas supplementing system and a gas check valve are additionally arranged on a tail gas pipeline of a chlorination reaction system and a finished product slot system in phosphorus trichloride production. The method and the device have the advantages that water vapor in air is prevented from entering a production system and reacting with the phosphorus trichloride, so that the yield of the phosphorus trichloride is improved, and a safety accident generated when a pipeline is blocked by phosphate substances is also avoided. Moreover, the production cost is reduced, the generation of side reactions is reduced, and the yield of the phosphorus trichloride is increased by0.5%, and therefore, the production method and the production device can be used for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of production method and equipment of phosphorus trichloride automatic inflating device, specifically in production system, adopt pneumatic adjusting valve and tail gas vacuum breaker, the pressure of Controlling System.
Background technology
In recent years, the industrial accident of domestic phosphorus trichloride enterprise is of common occurrence, and personnel burn and explosion hazard is taking place frequently in many enterprises, and what accident was brought to enterprise is not only financial loss, or even the disability of bringing to the employee, death, what for enterprise, face is social responsibility and existence.Therefore, production control cost, autonomous innovation, enhance productivity, keep the safety in production, and just can make enterprise more competitive.Phosphorus trichloride is the fuming liquid of achromaticity and clarification, meets water and air and resolves into phosphorous acid and hydrogenchloride, and the adularescent irritating smog is emerged, and chemical equation is PCl
3+ 3H
2o=H
3pO
3+ 3HCl, further generate complex acid H
3pCl
6, white cigarette occurs and go bad, must storage sealing storage.
In the phosphorus trichloride production process or in the material transfer process, the system internal pressure can change, and produces " breathing ", in the equalizing system internal pressure.For phosphorus trichloride manufacturer, what majority adopted is the method for air natural tonifying Qi, be to adopt the air in atmosphere to carry out the pressure in balanced reactive system, but contain a large amount of moisture in air, these moisture are along with air enters to react with phosphorus trichloride in production system, not only reduce the phosphorus trichloride yield, also can produce the phosphoric acid ester material and stop up exhaust pipe generation explosion hazard.
Summary of the invention
The object of the present invention is to provide a kind of production method of phosphorus trichloride automatic inflating device, adopt nitrogen air admission system and gas regulating valve, Controlling System pressure, to 0-1MPa, has effectively reduced the generation that phosphorus trichloride and water vapour generate the side reactions such as phosphite on the production basis of Optimization Technology.
The present invention realizes above-mentioned purpose like this, yellow phosphorus adopts to beat in phosphorus pump method or hydraulic pressure phosphorus method input chlorination tank and reacts with chlorine, temperature of reaction is controlled at 60 ℃-100 ℃, and wherein in reactor, liquid temperature is 80 ℃-95 ℃, and reactor outer wall vapor temperature is 75 ℃-90 ℃.The phosphorus trichloride gas that reaction generates enters packing tower and carries out rectifying, to remove free phosphorus.Part phosphorus trichloride gas is back to reactor after condenser condenses, and a part enters the phosphorus trichloride scale tank, through chemically examining after qualified, puts into pan tank.In the phosphorus trichloride production process, the exhaust pipe of chlorination system, pan tank system is all used the tonifying Qi of nitrogen tonifying Qi replaces air, and be equipped with pneumatic adjusting valve varitrol pressure and tail gas vacuum breaker, and pressure control range 0-1Mpa, preferential control pressure is 20Kpa-50Kpa.System internal pressure (chlorination system and pan tank system) is during higher than 50Kpa, and phosphorus trichloride tail gas enters into tail gas absorbing system by vacuum breaker and carries out condensation, buffering, washing, alkali cleaning, emptying; When the system internal pressure, during lower than 20Kpa, automatic regulating valve starts, and the nitrogen replaces air is supplemented and entered into system and carry out the equalizing system internal pressure; System pressure reaches the 20Kpa automatic regulating valve and closes.
Another object of the present invention is to provide a kind of production unit of phosphorus trichloride automatic inflating device, specifically in phosphorus trichloride is produced, on the exhaust pipe of chlorination system and pan tank system, increase nitrogen air admission system and gas check valve.
The present invention realizes above-mentioned purpose like this, and chlorination tank is connected with condenser by rectifying tower, and the condenser bottom flows into pan tank through scale tank, increases nitrogen air admission system and gas check valve on the exhaust pipe of scale tank and pan tank.
The exhaust pipe of described scale tank and pan tank adopts 30 ° of elevations angle, and described pan tank self is equipped with vacuum pump.
Described nitrogen air admission system comprises nitrogen and coupled nitrogen buffer tank, and wherein nitrogen buffer tank is connected with gas check valve by pneumatic adjusting valve.
Described vacuum breaker is connected with tail gas condenser in turn, tail gas buffer, and vacuum breaker, water wash column, soda-wash tower, wherein water wash column and soda-wash tower self are equipped with vacuum pump.
Tail gas buffer is connected with water wash column through vacuum breaker.
The pneumatic adjusting valve of nitrogen air admission system can the detection system internal pressure, and when the system internal pressure, during lower than low set(ting)value, gas check valve is closed, and automatic regulating valve starts nitrogen in surge tank and is injected in system, and pressure stops tonifying Qi while reaching the high value of establishing.When the system internal pressure, during higher than the high value of establishing, phosphorus trichloride gas arrives condensate buffering tank by gas check valve and reclaims tail gas, more emptying after washing, alkali cleaning after gas buffer tank buffering.
Advantage of the present invention: this phosphorus trichloride production method adopts cheap nitrogen to carry out balanced reactive system internal pressure, avoiding the water in air steam to enter production system reacts with phosphorus trichloride, improve the phosphorus trichloride yield, also avoid phosphoric acid ester material blocking pipe to produce security incident, save production cost, reduce side reaction and produce, realize that the phosphorus trichloride yield increases by 0.5%, greatly reduce the generation of waste gas, optimize operating environment, cleaner production.
The accompanying drawing explanation
The production unit of Fig. 1 phosphorus trichloride automatic inflating device.
Wherein, 1. chlorination tank, 2. rectifying tower, 3 condensers, 4. scale tank, 5. pan tank, 6 nitrogen buffer tanks, 7 nitrogengas cylinders, 8. pneumatic adjusting valve, 9. tail gas condenser, 10. tail gas buffer, 11. water wash columns, 12. soda-wash tower, 13-1,2,3. vacuum pump, 14-1,2 gas check valves.
Embodiment
The production method of phosphorus trichloride automatic inflating device, yellow phosphorus adopts to beat in phosphorus pump method or hydraulic pressure phosphorus method input chlorination tank and reacts with chlorine, described chlorination reaction temperature is controlled at 60 ℃-100 ℃, and wherein in reactor, liquid temperature is 80 ℃-95 ℃, and reactor outer wall vapor temperature is 75 ℃-90 ℃.The phosphorus trichloride gas generated is after rectifying, part phosphorus trichloride gas is back to reactor after condenser condenses, a part enters the phosphorus trichloride scale tank and puts into pan tank through chemically examining after qualified, increases nitrogen air admission system and gas check valve in phosphorus trichloride is produced on the exhaust pipe of chlorination system and pan tank system.Automatically regulate the pressure between chlorination system, pan tank system and tail gas vacuum breaker at outfit pneumatic adjusting valve between nitrogen air admission system and gas check valve, pressure control range 0-1Mpa, preferential control pressure is 20Kpa-50Kpa.System internal pressure (chlorination system and pan tank system) is during higher than 50Kpa, and phosphorus trichloride tail gas enters into tail gas absorbing system by vacuum breaker and carries out condensation, buffering, washing, alkali cleaning, emptying; When the system internal pressure, during lower than 20Kpa, automatic regulating valve starts, and the nitrogen replaces air is supplemented and entered into system and carry out the equalizing system internal pressure; System pressure reaches the 20Kpa automatic regulating valve and closes.
A kind of production unit of phosphorus trichloride automatic inflating device, chlorination tank 1 is connected with condenser 3 by rectifying tower 2, condenser 3 bottoms flow into pan tank 5 through scale tank 4, on the exhaust pipe of described scale tank 4 and pan tank 5, increase nitrogen air admission system and gas check valve 14-1.
Described scale tank 4 adopts 30 ° of elevations angle with the exhaust pipe of pan tank 5, and the material that can naturally flow backwards, avoid line clogging, and described pan tank self is equipped with vacuum pump 13-1.
Described nitrogen air admission system comprises nitrogengas cylinder 7 and coupled nitrogen buffer tank 6, and wherein nitrogen buffer tank 6 is connected with gas check valve 14-1 by the pneumatic adjusting valve 8 of two-in-parallel.
Described gas check valve 14-1 is connected with tail gas condenser 9 in turn, tail gas buffer 10, and water wash column 11, soda-wash tower 12, wherein water wash column 11 self is equipped with vacuum pump 12-2,3 with soda-wash tower 12.
Described tail gas buffer 10 is connected with water wash column 11 through vacuum breaker 14-2.
Effectively reduced the generation that phosphorus trichloride and water vapour generate the side reactions such as phosphite on the production basis of Optimization Technology, on chlorination system, pan tank system exhaust pipe, adopt automatic air replenishing system to carry out the regulation system internal pressure, greatly reduce the generation of side reaction, save production cost, realized that the phosphorus trichloride yield increases by 0.5%, reduce the generation of waste gas, optimize operating environment, cleaner production safety.
Claims (10)
1. the production method of a phosphorus trichloride automatic inflating device, yellow phosphorus adopts to beat in phosphorus pump method or hydraulic pressure phosphorus method input chlorination tank and reacts with chlorine, the phosphorus trichloride gas generated is after rectifying, part phosphorus trichloride gas is back to reactor after condenser condenses, a part enters the phosphorus trichloride scale tank and puts into pan tank through chemically examining after qualified, it is characterized in that: increase nitrogen air admission system and gas check valve in phosphorus trichloride is produced on the exhaust pipe of chlorination system and pan tank system.
2. the production method of phosphorus trichloride automatic inflating device according to claim 1, it is characterized in that: chlorination reaction temperature is controlled at 60 ℃-100 ℃, and wherein in reactor, liquid temperature is 80 ℃-95 ℃, and reactor outer wall vapor temperature is 75 ℃-90 ℃.
3. the production method of phosphorus trichloride automatic inflating device according to claim 1, it is characterized in that: automatically regulate the pressure between chlorination system, pan tank system and tail gas vacuum breaker at outfit pneumatic adjusting valve between nitrogen air admission system and gas check valve, and control pressure is at 0-1 MPa.
4. the production method of phosphorus trichloride automatic inflating device according to claim 1, it is characterized in that: automatically regulate the pressure between chlorination system, pan tank system and tail gas vacuum breaker at outfit pneumatic adjusting valve between nitrogen air admission system and gas check valve, and control pressure is at 20-50KPa.
5. the production method of phosphorus trichloride automatic inflating device according to claim 1, it is characterized in that: phosphorus trichloride tail gas enters into tail gas absorbing system by vacuum breaker and carries out condensation, buffering, washing, alkali cleaning, emptying.
6. the production unit of a phosphorus trichloride automatic inflating device, chlorination tank (1) is connected with condenser (3) by rectifying tower (2), condenser (3) bottom flows into pan tank (5) through scale tank (4), it is characterized in that: increase nitrogen air admission system and gas check valve (14-1) on the exhaust pipe of scale tank (4) and pan tank (5).
7. the production unit of phosphorus trichloride automatic inflating device according to claim 6 is characterized in that: scale tank (4) adopts 30 ° of elevations angle with the exhaust pipe of pan tank (5), and described pan tank self is equipped with vacuum pump (13-1).
8. the production unit of phosphorus trichloride automatic inflating device according to claim 6, it is characterized in that: the nitrogen air admission system comprises nitrogengas cylinder (7) and coupled nitrogen buffer tank (6), and wherein nitrogen buffer tank (6) is connected with gas check valve (14-1) by the pneumatic adjusting valve (8) of two-in-parallel.
9. the production unit of phosphorus trichloride automatic inflating device according to claim 6, it is characterized in that: gas check valve (14-1) is connected with tail gas condenser (9) in turn, tail gas buffer (10), water wash column (11), soda-wash tower (12), wherein water wash column (11) self is equipped with vacuum pump (12-2,3) with soda-wash tower (12).
10. the production unit of phosphorus trichloride automatic inflating device according to claim 9, it is characterized in that: tail gas buffer (10) is connected with water wash column (11) through vacuum breaker (14-2).
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|---|---|---|---|
| CN201310396546.9A CN103449389B (en) | 2013-09-04 | 2013-09-04 | A kind of production method of phosphorus trichloride automatic inflating device and production unit |
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| CN201310396546.9A CN103449389B (en) | 2013-09-04 | 2013-09-04 | A kind of production method of phosphorus trichloride automatic inflating device and production unit |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110538620A (en) * | 2018-11-14 | 2019-12-06 | 北京北方华创微电子装备有限公司 | Pressure control system and pressure control method of reaction chamber |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5252306A (en) * | 1992-03-02 | 1993-10-12 | Monsanto Company | Semi-continuous process for preparing phosphorus trichloride |
| CN101264870A (en) * | 2008-04-08 | 2008-09-17 | 常州市阳城化工有限公司 | Technique for preparing phosphorus trichloride |
| CN203440081U (en) * | 2013-09-04 | 2014-02-19 | 湖北泰盛化工有限公司 | Phosphorus trichloride automatic air supply production equipment |
-
2013
- 2013-09-04 CN CN201310396546.9A patent/CN103449389B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5252306A (en) * | 1992-03-02 | 1993-10-12 | Monsanto Company | Semi-continuous process for preparing phosphorus trichloride |
| CN101264870A (en) * | 2008-04-08 | 2008-09-17 | 常州市阳城化工有限公司 | Technique for preparing phosphorus trichloride |
| CN203440081U (en) * | 2013-09-04 | 2014-02-19 | 湖北泰盛化工有限公司 | Phosphorus trichloride automatic air supply production equipment |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110538620A (en) * | 2018-11-14 | 2019-12-06 | 北京北方华创微电子装备有限公司 | Pressure control system and pressure control method of reaction chamber |
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| CN103449389B (en) | 2015-11-25 |
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