CN104477849B - A kind of preparation method of chlorine trifluoride - Google Patents
A kind of preparation method of chlorine trifluoride Download PDFInfo
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- CN104477849B CN104477849B CN201410719545.8A CN201410719545A CN104477849B CN 104477849 B CN104477849 B CN 104477849B CN 201410719545 A CN201410719545 A CN 201410719545A CN 104477849 B CN104477849 B CN 104477849B
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Abstract
The invention discloses the preparation method of a kind of chlorine trifluoride, belong to field of fine chemical.First being there is blistering reaction by described method in liquid phase chlorination thing and fluorine gas under uniform temperature, obtains product 1；Again product 1, diluent gas and fluorine gas are passed through synthesis reactor, react under uniform temperature, obtain product 2；After finally product 2 being liquefied, arranging light, vaporization process, obtain described chlorine trifluoride.Described preparation method cheaper starting materials, it is easy to get, it is to avoid employing highly corrosive, highly toxic chlorine, improves the security in production, transport and storing process；And the advantage such as structure of reactor is simple, input and output material is convenient, the conversion ratio of reaction is high, accessory substance can be easily separated, it is easy to accomplish industrialized production.
Description
Technical field
The present invention relates to the preparation method of a kind of chlorine trifluoride, be specifically related to one fluorine gas and carbon tetrachloride and/
Or silicon tetrachloride is the method that chlorine trifluoride prepared by raw material, belong to field of fine chemical.
Background technology
Chlorine trifluoride is the haloid fluoride that known chemical property is the most active, is a kind of very competent fluorization agent.
The boiling point of chlorine trifluoride is 11.5 DEG C, is easy to the gas of condensation under normal conditions, can select on demand
Air-liquid any state is reacted, and this is less than general fluorization agent.Many metal oxides and chlorination
React with chlorine trifluoride during thing heating and generate corresponding chloride, utilize this characteristic of chlorine trifluoride, can make
Obtain many important metal fluorides, especially can be used to separate and purify rare element.Along with semiconductor,
The fast development of liquid crystal, solar energy and LED industry, chlorine trifluoride obtains in its CVD chamber cleaning link
To being widely applied, and demand constantly gesture in rising, chlorine trifluoride has become as the key of IC industry
One of special gas.
Chlorine trifluoride is a kind of important fluorization agent, can carry out many reactions, at industrial circle by substitute element fluorine
May be used for following purposes: (1) chlorine trifluoride and uranium react the separation and Extraction for uranium；(2) as fluorination
Reagent is used for organic fluorination and the preparation of metal fluoride；(3) can conduct in space flight and military field
The oxidisability propellant of rocket or guided missile；(4) in semiconductor, liquid crystal, solar energy and LED industry, three
Chlorine fluoride can be used for the cleaning of CVD chamber.At present, the topmost purposes of chlorine trifluoride is for semiconductor, liquid
Crystalline substance, solar energy and LED industry, with other fluoro-gas (such as NF3、C2F6And CF4) different, trifluoro
Changing chlorine the most just to react with semi-conducting material, therefore it can clean the CVD chamber of cold wall,
It is carried out being a kind of chemical etching process with chlorine trifluoride, there is not energetic ion as plasma and bang
Hitting process, the damage to equipment can be preferably minimized limit, and chlorine trifluoride cleans and belongs to the most cleaned simultaneously
Journey, it is possible to reduce equipment downtime, it is also possible to reduce the quantity of granule foreign, and decrease operating personnel
Open-assembly time.Comparing the cleaning of plasma cracking fluorine, chlorine trifluoride cleaning is simple and efficient,
And cleaning performance is more preferable.There are not obvious greenhouse effects in chlorine trifluoride, therefore its semiconductor, liquid crystal,
Solar energy and LED industry have broad application prospects.
Owing to chlorine trifluoride chemical property is active, corrosivity is extremely strong, control and the equipment to manufacturing condition
The requirement of selection the harshest, significantly limit its production, application.The preparation method of chlorine trifluoride
Proposed by Ruff and Krug the earliest, fluorine gas and chlorine reaction firstly generate chlorine monofluoride (formula (1)),
Chlorine monofluoride further react with fluorine gas generation chlorine trifluoride (formula (2)), reaction is undertaken in two steps, need through
Cross the purification and separation process of twice.And raw material chlorine has deep-etching, the characteristic of high poison, in storage and transport
The security risk that middle existence is bigger.
Cl2+F2=2ClF (1)
ClF+F2=ClF3 (2)
Patent US2006006057 reports another kind and prepares the method (formula (3)～(6)) of chlorine trifluoride,
The method is with HCl and/or Cl2For raw material and F2、NF3Or SF6In plasma reactor, reaction generates trifluoro
Change chlorine, and on the spot for the cleaning of CVD chamber.The advantage of this patent is that raw material has more selection, and shortcoming is
Structure of reactor is complicated, and the temperature of plasma is the highest, and the cell materials of reactor is difficult to tolerate F2、ClF3
Corrosion, cause the damage of equipment, the method is difficult to industrialized production and use.
Cl2+2NF3=2ClF3+N2 (3)
3HCl+4NF3=3ClF3+3HF+2N2 (4)
Cl2+3SF6=2ClF3+3SF4 (5)
HCl+4SF6=2ClF3+2HF+4SF4 (6)
Patent RU2223908 reports another kind and prepares the method (formula (7)～(9)) of chlorine trifluoride,
The method is with solid metal chlorides (NaCl and/or CaCl2) it is that raw material reacts generation chlorine and one with fluorine gas
Chlorine fluoride, chlorine and chlorine monofluoride react generation chlorine trifluoride further with fluorine gas.The advantage of this patent is former
Material is easy to get, and shortcoming relates to gas-solid reaction, and reaction temperature is high, structure of reactor is complicated, the conversion ratio of reaction
Relatively low, and reaction need substep carry out, relate to twice separation, purification process, complex operation.
3NaCl+2F2=3NaF+ClF+Cl2 (7)
3CaCl2+4F2=3CaF2+2ClF+2Cl2 (8)
ClF+Cl2+4F2=3ClF3 (9)
In sum, chlorine trifluoride preparation method known today be primarily present equipment dependability low, produce work
There is the problems such as bigger security risk in skill complexity, the storage of raw material chlorine and transport.
Summary of the invention
In view of this, it is an object of the invention to the preparation method of a kind of chlorine trifluoride, described method is with liquid phase chlorine
Compound (CCl4And/or SiCl4) with fluorine gas be raw material, reaction generate chlorine trifluoride, there is raw material and be easy to get, instead
Answer the advantages such as device simple in construction, input and output material conversion ratio convenient, reaction is high, accessory substance can be easily separated, it is easy to
Realize industrialized production.
The preparation method of the present invention is broadly divided into 3 technical process:
(1) by liquid phase chlorination thing (CCl4And/or SiCl4) add in gas-liquid reactor, fluorine gas is by reacting
Being passed through bottom device, liquid phase chlorination thing and fluorine gas blistering reaction in liquid phase material generates Cl2、CF4And/or SiF4,
Gas liquid reaction liberated heat is taken away by being arranged on the heat exchanger within gas-liquid reactor, remains stable anti-
Answer temperature；Gas-liquid reactor is provided with fluid level controller, can supplement the liquid phase chlorination thing that reaction consumes in time
(CCl4And/or SiCl4), control liquid phase material liquid level during operation and maintain in certain region；
(2) by the product in gas-liquid reactor, (main component includes Cl2、CF4And/or SiF4The most anti-
Should fluorine gas completely) it is passed through synthesis reactor, meanwhile, it is passed through a certain amount of fluorine gas in the reactor, will
In the range of fluorine gas and chlorine are adjusted to predetermined stoichiometric proportion, reaction generates borontrifluoride at a predetermined temperature
Chlorine；
(3) by the product in synthesis reactor, (main component includes ClF3、ClF、CF4And/or SiF4
With unreacted Cl completely2And F2) it is passed through cold-trap, chlorine trifluoride liquefaction is collected, meanwhile, in product
ClF、Cl2、F2、CF4And/or SiF4Discharge after harmless treatment Deng light impurity, the trifluoro in income cold-trap
Change chlorine and enter in storage tank or steel cylinder by turning stockline.
The purpose of the present invention is realized by techniques below scheme:
The preparation method of a kind of chlorine trifluoride, described method specifically comprises the following steps that
(1) the liquid phase chlorination thing of excess is added in gas-liquid reactor, bottom gas-liquid reactor, be passed through fluorine
There is blistering reaction in gas, liquid phase chlorination thing and fluorine gas at-20～50 DEG C, obtains product 1；
(2) product 1, inert gas and fluorine gas are passed through synthesis reactor, react at 100～400 DEG C,
Obtain product 2；
(3), after product 2 being liquefied, arranging light, vaporization process, chlorine trifluoride of the present invention is obtained；
Wherein, step (1) the described liquid phase chlorination preferred CCl of thing4And SiCl4In more than one；
The flow velocity of described fluorine gas preferably 0.1～1L/min；
Described blistering reaction temperature is-20～50 DEG C, preferably 10～30 DEG C, and reaction pressure is-0.09～0.6MPa,
Preferably-0.07～0.2MPa；
Step (2) described inert gas is more than one in nitrogen, argon gas, helium and carbon tetrafluoride；
The flow velocity preferably 0.1～1L/min of described product 1；The flow velocity of fluorine gas preferably 0.3～4L/min；Indifferent gas
The flow velocity of body preferably 0.51～40L/min；
Described synthesis reactor is tubular reactor, and the material of tubular reactor is nickel or monel metal,
Preferably nickel；
Reaction temperature preferably 200～300 DEG C, reaction pressure is-0.09～0.6MPa, preferably-0.04～0.3MPa.
Step (3) described liquefaction and row are gently carried out in cold-trap；Synthesis reactor and cold-trap are connected by pipeline,
The material of pipeline is stainless steel, carbon steel, copper, nickel or monel metal, preferably carbon steel or stainless steel；
Described liquefaction parameter: temperature is-100～0 DEG C, preferably-60～-30 DEG C, pressure is-0.09～0.6MPa,
It is preferably 0～0.2MPa；
Described vapourizing temperature preferably 20～40 DEG C.
Beneficial effect
(1) preparation method cheaper starting materials of the present invention, be easy to get, it is to avoid employing highly corrosive, high toxicity
Chlorine, improve production, transport and storing process in security, accessory substance CF4And/or SiF4Can divide
From, reclaim, can use as industrial goods, technical process uses gas phase and liquid phase material, operability
Good, it is possible to realize the industrial operation of serialization.And structure of reactor is simple, input and output material is convenient, the turning of reaction
The advantages such as rate is high, accessory substance can be easily separated, it is easy to accomplish industrialized production.
(2) high purity 98.1% of the chlorine trifluoride gas prepared by preparation method of the present invention, fluorination
The content of hydrogen is less than 0.2%, and this gas can use directly as industrial gasses, it is also possible to purifies essence further
Make high-purity chlorine trifluoride.
Accompanying drawing explanation
The process chart of Fig. 1 chlorine trifluoride of the present invention preparation method；
Wherein, 1-inert gas pipeline one, 2-fluorine gas pipeline one, 3-inert gas pipeline two, 4-fluorine gas pipeline
Two, 5-gas-liquid reactor, 6-chlorine pipeline, 7-synthesis reactor, 8-crude product chlorine trifluoride pipeline, 9-cold-trap,
10-fine work chlorine trifluoride pipeline, 11-vent line, 12-chlorine trifluoride storage tank, 13-vavuum pump, 14-vavuum pump
Outlet, 15-purges offgas outlet.
Detailed description of the invention
With specific embodiment in detail the present invention is described in detail below, but is not limited to this.
Following example are under normal temperature and pressure, and fluorine gas is passed through liquid phase chlorination thing (CCl4And/or SiCl4In),
Displacing the chlorine atom in reactant and generate chlorine, then fluorine gas generates chlorine trifluoride with chlorine reaction.Reaction
Shown in equation such as formula (10)～(12), raw material and product physical property are as shown in table 1:
CCl4+2F2=CF4+2Cl2 (10)
SiCl4+2F2=SiF4+2Cl2 (11)
Cl2+3F2=2ClF3 (12)
Table 1 raw material and product physical property list
In following example, the process chart of chlorine trifluoride preparation method is as it is shown in figure 1, described preparation method
The device used mainly includes gas-liquid reactor 5, synthesis reactor 7, cold-trap 9, chlorine trifluoride storage tank 12,
With vavuum pump 13；Gas-liquid reactor 5, synthesis reactor 7, logical between cold-trap 9 and chlorine trifluoride storage tank 12
Piping is sequentially connected with.Wherein, gas-liquid reactor 5 is connected by chlorine pipeline 6 with synthesis reactor 7；
Synthesis reactor 7 is connected by crude product chlorine trifluoride pipeline 8 with cold-trap 9；Cold-trap 9 and chlorine trifluoride storage tank
12 are connected by fine work chlorine trifluoride pipeline 10.
Before system starts, first carry out vacuumizing pretreatment with vavuum pump 13, then use inert gas tube
Line 1,3 purging, the air of displacement residual and moisture.After having carried out pretreatment work, will by fluorine gas pipeline 4
Fluorine gas is passed through in gas-liquid reactor 5, fluorine gas and the CCl in gas-liquid reactor 54And/or SiCl4Reaction generates
Cl2、CF4And/or SiF4, this product is passed through in synthesis reactor 7 via chlorine pipeline 6, meanwhile,
Fluorine gas and diluent gas are entered synthesis reactor 7 by inert gas pipeline 1 and fluorine gas pipeline 2 the most respectively
Middle reaction, the temperature of reactor controls at 100～400 DEG C, and fluorine gas and chlorine react raw in synthesis reactor 7
Become chlorine trifluoride.Process gas in synthesis reactor 7 enters cold-trap 9 via crude product chlorine trifluoride pipeline 8,
Being liquefied by chlorine trifluoride at low temperatures, be collected in cold-trap 9 with liquid phase state, low-boiling point gas impurity passes through
Vent line 11 drains into vacuum pump outlet 14 and/or purging offgas outlet 15 delivers to exhaust treatment system, through nothing
Evilization is vented after processing.The chlorine trifluoride of the collection in cold-trap 9 proceeds to three by fine work chlorine trifluoride pipeline 10
In chlorine fluoride storage tank.
Embodiment 1
(1) first by vavuum pump, each parts of device are vacuumized pretreatment；Again with fluorine gas purging, put
The air remained in changing system and moisture；Again by the CCl of excess4Add in gas-liquid reactor, and with 0.1
The flow velocity of L/min for be passed through fluorine gas bottom gas-liquid reactor, CCl4With fluorine gas in 0.6MPa, at 50 DEG C
There is blistering reaction, obtain product 1；
(2) it is passed through product 1, fluorine gas with the flow velocity of 0.1L/min, 0.3L/min and 1.2L/min respectively
Being passed through synthesis reactor with nitrogen, the operation pressure arranging synthesis reactor is 0.6MPa, anti-at 100 DEG C
Should, obtain product 2；
(3) product 2 being passed through cold-trap, the operation pressure arranging cold-trap is 0.6MPa, to product at 0 DEG C
2 liquefy, and low-boiling point gas impurity is delivered to exhaust treatment system, through harmless treatment by emptying pipeline
Rear emptying.After 20h, stop being passed through unstrpped gas, stop the heating of reactor.Close the import and export of cold-trap
Valve, with nitrogen and application of vacuum reaction system, reduces corrosive gas to equipment, pipeline, valve instrument
Corrosion.Cold-trap is warming up to 40 DEG C, after chlorine trifluoride gas vaporization, is pressed into chlorine trifluoride storage tank by pipeline
Middle preservation.
The yield of chlorine trifluoride is 81.3%, and purity is 98.1%, wherein, the content of hydrogen fluoride is 1000 ×
10-6mg/m3, nitrogen content is 500 × 10-6mg/m3。
Wherein, the constituent material of described synthesis reactor is monel metal, a diameter of 100mm of reactor,
A height of 1500mm, the internal coil pipe equipped with Monel heats.
The purity of described fluorine gas is 99%, and wherein the content of hydrogen is 500 × 10-6mg/m3；Carbon tetrachloride purity
Being 99%, moisture is 500 × 10-6mg/m3。
Embodiment 2
(1) first by vavuum pump, each parts of device are vacuumized pretreatment；Again with nitrogen purging, put
The air remained in changing system and moisture；Again by the SiCl of excess4Add in gas-liquid reactor, and with 1
The flow velocity of L/min for be passed through fluorine gas bottom gas-liquid reactor, SiCl4With fluorine gas in 0.03MPa, at 25 DEG C
There is blistering reaction, obtain product 1；
(2) it is passed through product 1, fluorine gas and nitrogen with the flow velocity of 1L/min, 4L/min and 40L/min respectively
Gas is passed through synthesis reactor, and the operation pressure arranging synthesis reactor is 0.32MPa, reacts at 380 DEG C,
Obtain product 2；
(3) product 2 being passed through cold-trap, the operation pressure arranging cold-trap is 0.05MPa, right at-95 DEG C
Product 2 liquefies, and low-boiling point gas impurity is delivered to exhaust treatment system, through harmless by emptying pipeline
Change is vented after processing.After 3h, stop being passed through unstrpped gas, stop the heating of reactor.Close entering of cold-trap
Outlet valve, with nitrogen and application of vacuum reaction system, reduces corrosive gas to equipment, pipeline, valve
The corrosion of instrument.Cold-trap is warming up to 20 DEG C, after chlorine trifluoride gas vaporization, is pressed into chlorine trifluoride by pipeline
Storage tank preserves.
The yield of chlorine trifluoride is 84.6%, and purity is 95.3%, wherein, the content of hydrogen fluoride is 1900 ×
10-6mg/m3, nitrogen content is 830 × 10-6mg/m3。
Wherein, the constituent material of described synthesis reactor is nickel, and a diameter of 100mm of reactor is a height of
1500mm, the internal coil pipe equipped with Monel heats.
The purity of described fluorine gas is 99%, and wherein the content of hydrogen is 500 × 10-6mg/m3；SiCl4Purity is
99%, moisture is 1 × 10-6mg/m3。
Embodiment 3
(1) first by vavuum pump, each parts of device are vacuumized pretreatment；Again with nitrogen purging, put
The air remained in changing system and moisture；Again by the CCl of excess4And SiCl4Mixed liquor (CCl4With SiCl4
Volume ratio be 2:1) add in gas-liquid reactor, and with the flow velocity of 0.5L/min from the bottom of gas-liquid reactor
Portion is passed through fluorine gas, CCl4、SiCl4With fluorine gas in-0.09MPa, there is blistering reaction at-20 DEG C, obtain product
1；
(2) it is passed through product 1, fluorine gas with the flow velocity of 0.5L/min, 1L/min and 0.51L/min respectively
Being passed through synthesis reactor with nitrogen, the operation pressure arranging synthesis reactor is-0.09MPa, anti-at 400 DEG C
Should, obtain product 2；
(3) product 2 being passed through cold-trap, the operation pressure arranging cold-trap is-0.09MPa, right at-100 DEG C
Product 2 liquefies, and low-boiling point gas impurity is delivered to exhaust treatment system, through harmless by emptying pipeline
Change is vented after processing.After 10h, stop being passed through unstrpped gas, stop the heating of reactor.Close cold-trap
Terminal valve, with nitrogen and application of vacuum reaction system, reduces corrosive gas to equipment, pipeline, valve
The corrosion of door instrument.Cold-trap is warming up to 30 DEG C, is pressed into by pipeline borontrifluoride after chlorine trifluoride gas vaporization
Chlorine storage tank preserves.
The yield of chlorine trifluoride is 75.8%, and purity is 97.5%, wherein, the content of hydrogen fluoride is 1300 ×
10-6mg/m3, nitrogen content is 50 × 10-6mg/m3。
Wherein, the constituent material of described synthesis reactor is monel metal, the internal dish equipped with Monel
Pipe heats；A diameter of 100mm of reactor, a height of 1500mm.
The purity of described fluorine gas is 98%, and wherein hydrogen fluoride content is 600 × 10-6mg/m3；CCl4's
Purity is 99%, moisture 500 × 10-6mg/m3；SiCl4Purity be 99.9%, moisture
It is 2 × 10-6mg/m3；
The present invention includes but not limited to above example, every carry out under the principle of spirit of the present invention appoint
What equivalent or local improvement, all will be regarded as within protection scope of the present invention.
Claims (7)
1. the preparation method of a chlorine trifluoride, it is characterised in that: described method specifically comprises the following steps that
(1) the liquid phase chlorination thing of excess is added in gas-liquid reactor, bottom gas-liquid reactor, be passed through fluorine
There is blistering reaction in gas, liquid phase chlorination thing and fluorine gas at-20～50 DEG C, obtains product 1；
(2) product 1, diluent gas and fluorine gas are passed through synthesis reactor, react at 100～400 DEG C,
Obtain product 2；
(3), after product 2 being liquefied, arranging light, vaporization process, described chlorine trifluoride is obtained；
Wherein, described in step (1), liquid phase chlorination thing is CCl4And SiCl4In more than one.
The preparation method of a kind of chlorine trifluoride the most according to claim 1, it is characterised in that: step (1)
The flow velocity of described fluorine gas is 0.1～1L/min；Described blistering reaction pressure is-0.09～0.6MPa.
The preparation method of a kind of chlorine trifluoride the most according to claim 1 and 2, it is characterised in that: institute
Stating blistering reaction parameter: temperature is 10～30 DEG C, pressure is-0.07～0.2MPa.
The preparation method of a kind of chlorine trifluoride the most according to claim 1, it is characterised in that: step (2)
Described diluent gas is more than one in nitrogen, argon gas, helium and carbon tetrafluoride；The stream of described product 1
Speed is 0.1～1L/min；The flow velocity of fluorine gas is 0.3～4L/min；The flow velocity of diluent gas is 0.51～40L/min；
The pressure of described reaction is-0.09～0.6MPa；Described synthesis reactor is tubular reactor；Tubular reactor
Constituent material be the one in nickel and monel metal.
5. according to the preparation method of a kind of chlorine trifluoride described in claim 1 or 4, it is characterised in that: step
Suddenly (2) described reaction temperature is 200～300 DEG C, and reaction pressure is-0.04～0.3MPa.
The preparation method of a kind of chlorine trifluoride the most according to claim 1, it is characterised in that: step (3)
Described liquefaction and row are gently carried out in cold-trap；Synthesis reactor and cold-trap are connected by pipeline, and the material of pipeline is
One in stainless steel, carbon steel, copper, nickel and monel metal；
Described liquefaction parameter: temperature is-100～0 DEG C；Pressure is-0.09～0.6MPa；
Described vapourizing temperature is 20～40 DEG C.
7. according to the preparation method of a kind of chlorine trifluoride described in claim 1 or 6, it is characterised in that: institute
State liquefaction parameter: temperature is-60～-30 DEG C；Pressure is 0～0.2MPa.
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| KR102314586B1 (en) * | 2016-04-05 | 2021-10-18 | 칸토 덴카 코교 가부시키가이샤 | How to supply chlorine fluoride |
| CN114538381B (en) * | 2021-01-29 | 2022-10-11 | 福建德尔科技股份有限公司 | Separation device and separation method for electronic-grade chlorine trifluoride |
| CN113912013B (en) * | 2021-10-13 | 2022-12-27 | 中船(邯郸)派瑞特种气体股份有限公司 | High-purity chlorine trifluoride reaction preparation device with high safety |
| CN113958869B (en) * | 2021-10-19 | 2023-11-21 | 国网安徽省电力有限公司电力科学研究院 | Zero-emission insulating gas purifying treatment device and method |
| CN113856233B (en) * | 2021-10-22 | 2022-11-25 | 中船(邯郸)派瑞特种气体股份有限公司 | Efficient chlorine trifluoride rectifier unit |
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| JP2788102B2 (en) * | 1990-07-26 | 1998-08-20 | セントラル硝子株式会社 | Arsenic cleaning method using fluorine or chlorine fluoride gas |
| US20070039924A1 (en) * | 2005-08-18 | 2007-02-22 | Tokyo Electron Limited | Low-temperature oxide removal using fluorine |
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|---|---|---|---|---|
| RU2223908C1 (en) * | 2002-06-05 | 2004-02-20 | Федеральное государственное унитарное предприятие "Сибирский химический комбинат" | Chlorine trifluoride preparation process |
| CN102143793A (en) * | 2008-12-11 | 2011-08-03 | 中央硝子株式会社 | Detoxifying method of chlorine trifluoride |
| CN102502503A (en) * | 2011-10-08 | 2012-06-20 | 核工业理化工程研究院华核新技术开发公司 | Method for preparing bromine trifluoride |
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