CN109110739A - The horizontal continuous producing apparatus of phosphorus pentafluoride - Google Patents

The horizontal continuous producing apparatus of phosphorus pentafluoride Download PDF

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Publication number
CN109110739A
CN109110739A CN201811318536.2A CN201811318536A CN109110739A CN 109110739 A CN109110739 A CN 109110739A CN 201811318536 A CN201811318536 A CN 201811318536A CN 109110739 A CN109110739 A CN 109110739A
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CN
China
Prior art keywords
horizontal
liquid level
horizontal reacting
producing apparatus
phosphorus pentafluoride
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Pending
Application number
CN201811318536.2A
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Chinese (zh)
Inventor
孔行健
胡春波
杨林
张志业
王辛龙
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Sichuan University
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Sichuan University
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Priority to CN201811318536.2A priority Critical patent/CN109110739A/en
Publication of CN109110739A publication Critical patent/CN109110739A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/10Halides or oxyhalides of phosphorus

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)

Abstract

The invention discloses a kind of horizontal continuous producing apparatus of phosphorus pentafluoride, including horizontal reacting container, with the liquid level maintaining segment of certain altitude in the inner cavity of the horizontal reacting container, the area equation of the horizontal cross-section of the liquid level maintaining segment arbitrary height position, feed pathway is provided with below the liquid level maintaining segment, the horizontal reacting one end of top is provided with inlet channel, and the other end is provided with exhaust passage.The present invention can accurately, easily control the reaction rate of yellow phosphorus and fluorine gas, keep reaction process more stable, reduce and generate the security risk exploded because reaction rate is excessive.

Description

The horizontal continuous producing apparatus of phosphorus pentafluoride
Technical field
The present invention relates to phosphorus pentafluoride Preparation equipment fields, and in particular to a kind of horizontal continuous production of phosphorus pentafluoride is set It is standby.
Background technique
Phosphorus pentafluoride is a kind of important inorganic fluoride, can be used for electronics industry, high molecular material and organic conjunction At catalyst.Currently, can be realized there are mainly two types of the techniques of industrialized production high-purity phosphorus pentafluoride, one is utilize pentachloro- Change phosphorus and hydrogen fluoride reaction, generate phosphorus pentafluoride and hydrogen chloride, another kind is to be reacted using fluorine gas with yellow phosphorus, generates five fluorinations Phosphorus.
It is existing react the equipment for preparing phosphorus pentafluoride with yellow phosphorus using fluorine gas or technique can refer to application No. is 201210113224.4 patent of invention, or application No. is 201210557911.5 patent of invention, these existing preparations Technique or equipment are all using solid yellow phosphorus as raw material, and solid yellow phosphorus is the different particle of surface area, and different moments are passed through The yellow phosphorus of reactor and the contact area of fluorine gas cannot keep unanimously, and reaction rate is caused to have biggish fluctuation, be unfavorable for steady Determine, accurately control reaction rate, since yellow phosphorus can discharge a large amount of heat with reacting for fluorine gas, when reaction rate fluctuation is larger When, it is easy to there is runaway reaction and lead to explosion accident, security risk is larger.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of reaction rate for more easily controlling yellow phosphorus and fluorine gas, Keep reaction process more stable, reduces and generate the security risk exploded because reaction rate is excessive.
The technical proposal for solving the technical problem of the invention is: the horizontal continuous producing apparatus of phosphorus pentafluoride, including Horizontal reacting container, with the liquid level maintaining segment of certain altitude, the liquid level maintaining segment in the inner cavity of the horizontal reacting container The area equation of the horizontal cross-section of arbitrary height position, is provided with feed pathway below the liquid level maintaining segment, top it is sleeping Formula reaction vessel one end is provided with inlet channel, and the other end is provided with exhaust passage.
Further, the horizontal reacting external container is provided with collet, sets between the collet and horizontal reacting container It is equipped with cooling chamber, and one end of collet is provided with the cooling liquid inlet communicated with cooling chamber, the other end is provided with and cooling chamber phase Logical coolant liquid arranges mouth.
Further, temperature detector and pressure detector are provided in the horizontal reacting container.
Further, the bottom of the horizontal reacting container is provided with horizontal support base.
Further, the inlet channel is vertically arranged.
Compared with prior art, the beneficial effects of the present invention are: in use, being first passed through into horizontal reacting container enough lazy Property gas, by horizontal reacting container air be discharged, the liquid phosphor of thawing is then passed through horizontal reacting container, makes liquid The liquid level of yellow phosphorus is located in liquid level maintaining segment, is then passed through fluorine gas by inlet channel, and fluorine gas is contacted with the liquid level of liquid phosphor And react, phosphorus pentafluoride is generated, phosphorus pentafluoride is gas, is discharged from exhaust passage.During the reaction, it is constantly passed through new Liquid phosphor controls the liquid level of liquid phosphor in liquid level maintaining segment always, thus guarantee that the liquid level area of yellow phosphorus is constant, fluorine The contact area of gas and yellow phosphorus is constant, and reaction rate is avoided greatly to fluctuate, then is passed through flow by control fluorine gas, i.e., Comparable reaction rate that is accurate, easily controlling yellow phosphorus and fluorine gas, keeps reaction process more stable, reduces because of reaction rate mistake Security risk that is big and generating explosion.
Detailed description of the invention
Fig. 1 is schematic front view of the invention.
Fig. 2 is schematic top plan view of the invention.
Appended drawing reference: 1-horizontal reacting container;2-liquid level maintaining segment;3-feed pathways;4-inlet channels;5-rows Gas channel;6-collets;7-cooling chambers;8-cooling liquid inlets;9-coolant liquids arrange mouth;10-temperature detectors;11-pressure Detector;12-support bases.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples.
As depicted in figs. 1 and 2, the horizontal continuous producing apparatus of phosphorus pentafluoride of the invention, including horizontal reacting container 1, With the liquid level maintaining segment 2 of certain altitude, the 2 arbitrary height position of liquid level maintaining segment in the inner cavity of the horizontal reacting container 1 The area equation for the horizontal cross-section set, the lower section of the liquid level maintaining segment 2 are provided with feed pathway 3, and the horizontal reacting of top holds 1 one end of device is provided with inlet channel 4, and the other end is provided with exhaust passage 5.
Horizontal reacting container 1 uses high-temperature and high-presure resistent reactor, and feed pathway 3 is sleeping for liquid phosphor to be continuously passed through Formula reaction vessel 1, fluorine gas for being continuously passed through horizontal reacting container 1 by inlet channel 4, and exhaust passage 5 will be for that will react generation Phosphorus pentafluoride discharge.When due to the yellow phosphorus using solid powder as raw material, it is not easy to control contact of the yellow phosphorus with fluorine gas Area causes reaction to be not sufficiently stable, and control is not easy.And solid yellow phosphorus is heated as liquid first with heating equipment by the present invention Then liquid phosphor is passed through horizontal reacting container, then fluorine gas is passed through horizontal reacting container above yellow phosphorus liquid level by state, make Fluorine gas is merely able to contact with yellow phosphorus liquid level, and it is excessive with the contact area of yellow phosphorus and lead to react excessively violent to avoid fluorine gas.
With the progress of reaction, the yellow phosphorus in horizontal reacting container 1 is constantly consumed, and yellow phosphorus liquid level can reduce, liquid level It can change, in order to guarantee reacting balance, the liquid level area of liquid phosphor should be as constant as possible, to guarantee fluorine gas and Huang The contact area of phosphorus remains unchanged, therefore with the liquid level maintaining segment 2 of certain altitude, liquid in the inner cavity of horizontal reacting container 1 The area equation of the horizontal cross-section of 2 arbitrary height position of face maintaining segment.Liquid level maintaining segment 2 is the position required where yellow phosphorus liquid level Range, it is the liquid levels maintaining segment 2 such as 10mm, 20mm, 30mm that the liquid level maintaining segment 2 of certain altitude, which specifically can be height,.It is reacting In the process, it is continuously added to new liquid phosphor according to the depletion rate of yellow phosphorus, yellow phosphorus liquid level is made to be in liquid level maintaining segment 2 always In, it can guarantee that the contact area of fluorine gas and yellow phosphorus remains unchanged, reaction rate is avoided biggish fluctuation occur.
It is excessively violent to avoid reacting in order to react fluorine gas only with the liquid level of yellow phosphorus, and convenient for control reaction rate, fluorine Gas is merely able to be passed through from the top of liquid level maintaining segment 2, i.e., the horizontal reacting that 2 top of liquid level maintaining segment is arranged in feed pathway 3 holds In device 1.
In order to guarantee that reacting balance, the liquid level of liquid phosphor should also be steady, can not occur biggish fluctuation, liquid as far as possible State yellow phosphorus generally uses delivery pump as power-equipment, with certain stream when new liquid phosphor enters horizontal reacting container 1 Speed will necessarily cause to impact, and then lead to yellow phosphorus liquid fluctuating to existing liquid phosphor in horizontal reacting container 1, in order to subtract Feed pathway 3, is arranged in the lower section of liquid level maintaining segment 2 by small this percussion, it is desirable to is arranged in horizontal reacting container 1 Bottom, the liquid phosphor being newly added in this way from bottom enter and mix with original yellow phosphorus, can slow down to horizontal reacting appearance The impact of existing liquid phosphor in device 1, keeps yellow phosphorus liquid level steady.
Although existing conventional gas-liquid reactor also has feed inlet, discharge port etc., above-mentioned requirements are obviously unable to satisfy, Be not suitable for the present invention claims phosphorus pentafluoride preparation process, the present invention is the setting of making of preparation process for phosphorus pentafluoride Meter has the advantages that simple structure, reacting balance, reaction controllability are good.
In order to make reaction temperature keep stablizing, be provided with collet 6 outside the horizontal reacting container 1, the collet 6 with Cooling chamber 7 is provided between horizontal reacting container 1, and one end of collet 6 is provided with the cooling liquid inlet 8 communicated with cooling chamber 7, The other end is provided with the coolant liquid row's mouth 9 communicated with cooling chamber 7.
In use, being passed through coolant liquid into cooling chamber 7 by cooling liquid inlet 8, coolant liquid can be water, and coolant liquid enters The heat in horizontal reacting container 1 is absorbed after cooling chamber 7, temperature increases, and is then discharged from coolant liquid row's mouth 9, takes away reaction and produce Raw heat avoids the temperature in horizontal reacting container 1 excessively high, and pressure is excessive.
In order to more accurately control the temperature and pressure in horizontal reacting container 1, setting in the horizontal reacting container 1 There are temperature detector 10 and pressure detector 11, temperature detector 10 is used to detect the reaction temperature in horizontal reacting container 1, can Using thermocouple etc., pressure detector 11 is used to detect the reaction pressure in horizontal reacting container 1, and pressure sensor can be used, Staff controls reaction rate according to the charging rate of the temperature and pressure real-time monitoring fluorine gas and liquid phosphor that detect In the range of safety.Temperature detector 10 and pressure detector 11 can be connected with controller, and controller can use PLC Deng each pump for charging can also be controlled by controller, and controller is automatically controlled according to reaction temperature and pressure The feed rate and pressure of each raw material reduce manual labor amount.
The bottom of the horizontal reacting container 1 is provided with horizontal support base 12, and horizontal reacting container 1 is fixed on support base On 12, horizontal reacting container 1 is made to keep stablizing.
The inlet channel 4 is vertically arranged, and the flow direction of fluorine gas guarantees that fluorine gas and yellow phosphorus are abundant perpendicular to yellow phosphorus liquid level Reaction reduces the content of fluorine in phosphorus pentafluoride gas.

Claims (5)

1. the horizontal continuous producing apparatus of phosphorus pentafluoride, which is characterized in that including horizontal reacting container (1), the horizontal reacting With the liquid level maintaining segment (2) of certain altitude, the water of liquid level maintaining segment (2) the arbitrary height position in the inner cavity of container (1) The area equation of plane section is provided with feed pathway (3) below the liquid level maintaining segment (2), the horizontal reacting container of top (1) one end is provided with inlet channel (4), and the other end is provided with exhaust passage (5).
2. the horizontal continuous producing apparatus of phosphorus pentafluoride according to claim 1, which is characterized in that the horizontal reacting holds It is provided with collet (6), is provided with cooling chamber (7) between the collet (6) and horizontal reacting container (1), and collet outside device (1) (6) one end is provided with the cooling liquid inlet (8) communicated with cooling chamber (7), the other end be provided with communicated with cooling chamber (7) it is cold But liquid row mouth (9).
3. the horizontal continuous producing apparatus of phosphorus pentafluoride according to claim 1, which is characterized in that the horizontal reacting holds Temperature detector (10) and pressure detector (11) are provided in device (1).
4. the horizontal continuous producing apparatus of phosphorus pentafluoride according to claim 1, which is characterized in that the horizontal reacting holds The bottom of device (1) is provided with horizontal support base (12).
5. the horizontal continuous producing apparatus of phosphorus pentafluoride according to claim 1, which is characterized in that the inlet channel (4) it is vertically arranged.
CN201811318536.2A 2018-11-07 2018-11-07 The horizontal continuous producing apparatus of phosphorus pentafluoride Pending CN109110739A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811318536.2A CN109110739A (en) 2018-11-07 2018-11-07 The horizontal continuous producing apparatus of phosphorus pentafluoride

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811318536.2A CN109110739A (en) 2018-11-07 2018-11-07 The horizontal continuous producing apparatus of phosphorus pentafluoride

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CN109110739A true CN109110739A (en) 2019-01-01

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101417791A (en) * 2008-11-17 2009-04-29 袁翔云 Technique for preparing phosphorus pentafluoride
CN102421702A (en) * 2009-03-13 2012-04-18 霍尼韦尔国际公司 Methods and reactor designs for producing phosphorus pentafluoride
CN203513282U (en) * 2013-10-11 2014-04-02 浙江巨化凯蓝新材料有限公司 Phosphorus pentafluoride continuously-synthesizing device

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101417791A (en) * 2008-11-17 2009-04-29 袁翔云 Technique for preparing phosphorus pentafluoride
CN102421702A (en) * 2009-03-13 2012-04-18 霍尼韦尔国际公司 Methods and reactor designs for producing phosphorus pentafluoride
CN203513282U (en) * 2013-10-11 2014-04-02 浙江巨化凯蓝新材料有限公司 Phosphorus pentafluoride continuously-synthesizing device

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