CN103449389B - A kind of production method of phosphorus trichloride automatic inflating device and production unit - Google Patents
A kind of production method of phosphorus trichloride automatic inflating device and production unit Download PDFInfo
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- CN103449389B CN103449389B CN201310396546.9A CN201310396546A CN103449389B CN 103449389 B CN103449389 B CN 103449389B CN 201310396546 A CN201310396546 A CN 201310396546A CN 103449389 B CN103449389 B CN 103449389B
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Abstract
The invention provides a kind of production method and production unit of phosphorus trichloride automatic inflating device, adopt nitrogen air admission system and gas regulating valve, Controlling System pressure, to 0-1MPa, the production basis of Optimization Technology effectively decreases the generation that phosphorus trichloride and water vapour generate the side reactions such as phosphite.Specifically in phosphorus trichloride is produced chlorination system and pan tank system exhaust pipe on increase nitrogen air admission system and gas check valve.Adopt the method and equipment avoids water vapor in air to enter production system and phosphorus trichloride reacts, improve phosphorus trichloride yield, also phosphoric acid ester material blocking pipe is avoided to produce security incident, save production cost, reduce side reaction to produce, realize phosphorus trichloride yield and increase by 0.5%, can industrial production greatly.
Description
Technical field
The present invention relates to a kind of production method and equipment of phosphorus trichloride automatic inflating device, in production system, specifically 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 takes place frequently in many enterprises, and what accident was brought to enterprise is not only financial loss, or even the disability to bring to employee, death, what face for enterprise is social responsibility and existence.Therefore, production control cost, autonomous innovation, enhance productivity, keep the safety in production, and Cai Nengshi enterprise is more competitive.Phosphorus trichloride is the fuming liquid of achromaticity and clarification, and meet water and air and resolve into phosphorous acid and hydrogenchloride, adularescent irritating smog is emerged, and chemical equation is PCl
3+ 3H
2o=H
3pO
3+ 3HCl, generates complex acid H further
3pCl
6, there is white cigarette and go bad, sealing storage must be stored.
In phosphorus trichloride production process or in material transfer process, system internal pressure can change, and produces " breathing ", in equalizing system internal pressure.For phosphorus trichloride manufacturer, it is most that what adopt is the method for air natural tonifying Qi, namely be adopt the pressure in the next balanced reactive system of the air in air, but containing a large amount of moisture in air, these moisture enter to react with phosphorus trichloride in production system along with air, not only reduce phosphorus trichloride yield, also can produce phosphoric acid ester material blocking exhaust pipe and produce 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, the production basis of Optimization Technology effectively decreases the generation that phosphorus trichloride and water vapour generate the side reactions such as phosphite.
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 controls at 60 DEG C-100 DEG C, and wherein in reactor, liquid temperature is 80 DEG C-95 DEG C, and reactor outer wall vapor temperature is 75 DEG C-90 DEG C.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 phosphorus trichloride scale tank, through chemically examine qualified after put into pan tank.In phosphorus trichloride production process, the exhaust pipe of chlorination system, pan tank system all substitutes air tonifying Qi with nitrogen tonifying Qi, and being equipped with pneumatic adjusting valve varitrol pressure and tail gas vacuum breaker, pressure control range 0-1Mpa, priority acccess control pressure is 20Kpa-50Kpa.When system internal pressure (chlorination system and pan tank system) is higher than 50Kpa, phosphorus trichloride tail gas enters into tail gas absorbing system by vacuum breaker and carries out condensation, buffering, washing, alkali cleaning, emptying; When system internal pressure is lower than 20Kpa, automatic regulating valve starts, and nitrogen substitutes replenish air and enters into system and carry out equalizing system internal pressure; System pressure reaches 20Kpa automatic regulating valve and closes.
Another object of the present invention is to the production unit that a kind of phosphorus trichloride automatic inflating device is provided, specifically in phosphorus trichloride is produced chlorination system and pan tank system exhaust pipe on 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, flows into pan tank, the exhaust pipe of scale tank and pan tank increases nitrogen air admission system and gas check valve bottom condenser through scale tank.
Described scale tank and the exhaust pipe of pan tank adopt 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, vacuum breaker, water wash column, soda-wash tower, and 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 detection system internal pressure, and when system internal pressure is 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 reaches height and establishes during value and stop tonifying Qi.When system internal pressure establishes value higher than height, 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, water vapor in air is avoided to enter production system and phosphorus trichloride reacts, improve phosphorus trichloride yield, also avoid phosphoric acid ester material blocking pipe to produce security incident, save production cost, reduce side reaction and produce, realize phosphorus trichloride yield and increase by 0.5%, greatly reduce the generation of waste gas, optimize operating environment, cleaner production.
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 towers, 13-1,2,3. vacuum pump, 14-1,2 gas check valves.
Embodiment
Embodiment 1
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 controls at 60 DEG C-100 DEG C, and wherein in reactor, liquid temperature is 80 DEG C-95 DEG C, and reactor outer wall vapor temperature is 75 DEG C-90 DEG C.The phosphorus trichloride gas generated is after rectifying, part phosphorus trichloride gas is back to reactor after condenser condenses, a part enter phosphorus trichloride scale tank through chemically examine qualified after put into pan tank, in phosphorus trichloride is produced chlorination system and pan tank system exhaust pipe on increase nitrogen air admission system and gas check valve.Between nitrogen air admission system and gas check valve, be equipped with pneumatic adjusting valve automatically regulate chlorination system, pressure between pan tank system and tail gas vacuum breaker, pressure control range 0-1Mpa, priority acccess control pressure is 20Kpa-50Kpa.When system internal pressure (chlorination system and pan tank system) is higher than 50Kpa, phosphorus trichloride tail gas enters into tail gas absorbing system by vacuum breaker and carries out condensation, buffering, washing, alkali cleaning, emptying; When system internal pressure is lower than 20Kpa, automatic regulating valve starts, and nitrogen substitutes replenish air and enters into system and carry out equalizing system internal pressure; System pressure reaches 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, flow into pan tank 5 through scale tank 4 bottom condenser 3, described scale tank 4 and the exhaust pipe of 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 can flow backwards material naturally, and avoid line clogging, 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, water wash column 11, soda-wash tower 12, and wherein water wash column 11 and soda-wash tower 12 self are equipped with vacuum pump 12-2,3.
Described tail gas buffer 10 is connected with water wash column 11 through vacuum breaker 14-2.
The production basis of Optimization Technology effectively decreases the generation that phosphorus trichloride and water vapour generate the side reactions such as phosphite, chlorination system, pan tank system exhaust pipe adopt automatic air replenishing system to carry out regulation system internal pressure, greatly reduce the generation of side reaction, save production cost, achieve phosphorus trichloride yield and increase by 0.5%, reduce the generation of waste gas, optimize operating environment, cleaner production safety.
Claims (3)
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 enter phosphorus trichloride scale tank through chemically examine qualified after put into pan tank, it is characterized in that: in phosphorus trichloride is produced chlorination system and pan tank system exhaust pipe on increase nitrogen air admission system and gas check valve, wherein, between nitrogen air admission system and gas check valve, be equipped with pneumatic adjusting valve automatically regulate chlorination system, pressure between pan tank system and tail gas vacuum breaker, and control pressure is at 20-50KPa.
2. the production method of phosphorus trichloride automatic inflating device according to claim 1, is characterized in that: chlorination reaction temperature controls at 60 DEG C-100 DEG C, and wherein in reactor, liquid temperature is 80 DEG C-95 DEG C, and reactor outer wall vapor temperature is 75 DEG C-90 DEG C.
3. the production method of phosphorus trichloride automatic inflating device according to claim 1, 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.
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CN103449389A CN103449389A (en) | 2013-12-18 |
CN103449389B true CN103449389B (en) | 2015-11-25 |
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CN110538620B (en) * | 2018-11-14 | 2021-10-15 | 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 |
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