WO2003027010A1 - Method for producing nitrogen trifluoride - Google Patents

Abstract

The invention relates to inorganic chemistry, in particular to methods for producing nitrogen trifluoride. The inventive method consists in fluorating the solid phase of ammonium polyfluoride salt having the formula NH 4Fx HF, wherein x is higher than 0 to 1.3 and can be equal to 1.3. The initial salt is used mixed with a sorbing agent which is capable to sorb hydrogen fluoride formed by synthesis. Said sorbing agent is embodied in the form of metal fluorides having the formula MeF, wherein Me is a metal of the 1st group of the Periodic table, preferably NaF, KF and LiF. RbF and CsFF can be also used, but the use thereof being economically impractical. The production of nitrogen trifluoride is carried out at a temperature ranging from 20 to 125 °C. Said invention makes it possible to totally use the initial salt NH ¿4?Fx HF and to remove hydrogen fluoride thus produced.

Description

 SPECIAL PROBLEMS ΤΡandΦΤΟΡIDΑ ΑЗΟΤΑ

The invention relates to the field of inorganic chemistry, and specifically to the methods for the production of nitrogen nitrogen. 5 Nitrogen gas is used as a chemical agent and as an oxidizing agent for fuels. Мыш The electrical process is used in dry processes, such as gas, which does not leave a precipitate; its well-known application and in the equipment of chemical plants.

Known are the 3 basic technologies for the conversion of nitrogen from nitrogen:

1. The electrolysis of the alloy of a bifluoride of ammonium [part. SSH 3235474, κl. 204/63, οπ. 10/02/1961]. 15 2. Liquid phase separation of an alloy of ammonium bifluoride at 130-160 ° С and 0.2-0.4 ΜPa [part of the USA 4091091, class 423/406, οπ. 05/23/1978].

3. The formation of solid industrial compounds of ammonia and metals. This direction is subject to the 20 proposed invention.

Izvesτen sποsοb φτορiροvaniya τveρdyχ κοmπleκsnyχ φτορidοv ammοniya and meτallοv οbschey φορmuly (ΝΗ _{4) Χ} ΜΡ _Y and (ΝΗ ₄₎ χΜΜ py ¹ where χ = 1-3, y = 4-7, Μ = Ρe, ΑΙ, Τι ^'and dρ . metals, Μ ¹ = Ц Νа, Κ [pаt. USA 4543242, С 01 Β 21 / 83Β, 09/24/1985] 25 The process can be operated in a continuous mode, with the flow of gas, diluted with inert gas (nitrogen). Ample ammonia complex salts are used in particles of a selectable size, which ensures a stable reaction. The yield of the reaction reaches 80-85%.

A cheap method is the high cost of 5 original commercially available ammunition and metal fluids, and also is inadmissible to dispose of it.

The closest technical solution is the means [p. Japanese 3232710, cl. C 01 Β 21/083, application. 10/06/1990, οπ. 10.16.1991]. Because of this, the nitrogen compound is produced by reacting the reaction with a mixture of metal and ammonium salts in a mass ratio of 2: 1. The reaction is carried out at a temperature of 50-450 ° C, with the dilution of nitrogen being supplied to the reaction.

15 Β κachesτve φτορida meτalla in eτοm izοbρeτenii mοguτ isποlzοvaτsya, naπρimeρ, φτορidy Κ, Νa, Cu, Ca, Ζη, ΑΙ, δη, Ρ, Μη, Νϊ, Sο, Ρe and dρugie, οdnaκο best ρezulτaτ dοsτigaeτsya πρi isποlzοvanii ΝaΡ, SaΡ _{2 ,} ΡеΡ ₃ .

Аче For the most part, the inorganic ammonia salt in

20 of the present invention, you may use (ΝΗ) ₂ δ0 _4ι (ΝΗ ₄ ) ₂ С0 ₂ , ΝΗ ₄ Ν0 ₂₎ ΝΗ ₄ Ρ, ΝΗ ₄ СΙ, ΝΗ ₄ Βг, ΝΗ ₄ Ι and others.

Comparison of metal components and metal ammonia may be useful, but it is desirable that the reaction

25 There was an excess of metal fluoride, the weight ratio of metal fluoride and non-urban ammonia was 2: 1. The reaction unit may be close to or above the room. From the point of view, the speed of the reaction is desirable, so that the temperature is more than 50 ° C. For the sake of convenience, it was advisable to have ₃ more, so that 5 temperature was less than 450 ° С. Taken into account a number of industrial factors (speed of reaction, waste of energy and other), it is advisable that the temperature is 100 ° C.

The method of production is the production of liquid ammonia; Liquid phase treatment may result in clogging of the treatment and increased treatment. High

15 Processes for processing the process increase the contribution to the normal reactions that go with the conversion of nitrogen, which substantially reduces the output of the target process.

The challenge facing the invention is the processing

20 means of using the full use of the original salt ΝΗ ₄ Ρ ^”

Solving this problem allows you to speed up the process of production of nitrogen and nitrogen, to achieve high

25 its efficiency and, to a large extent, will facilitate the solution of the problems associated with the disposal of by-products. This problem is solved by means of the interaction of the acid salt, which is in the opposite phase of acid salt, with ammonium oxide ΝΗ ₄ Ρ ΗΡ, where χ is more than 0, more than 1, but less than 1. The original salt of 5 is used in a mixture with a binder that is capable of combining a product resulting from the synthesis. The product is a component of metal formulas, where it is the metal of the first group, preferably, it is. It is also possible to use both GSG and SΡΡ, but they are also used inappropriately.

Pροtsess ποlucheniya τρiφτορida azοτa προvοdyaτ πρi 20 - 125 ° C and massοvοm sοοτnοshenii sορbenτ: ΝΗ ₄ Ρ ^«χΗΡ οτ 2 dο 100.

15 In the case of solid saline, ammonia may be able to accept values greater than 0, less than or equal to 1, 3.

If you are in the game, you are in the opposite phase of the compounds of the formula ΝΗ Ρ ^« χΗΡ for 1 mole of target

20 reaction products ΝΡ ₃ ; (4 + χ) mol ΗΡ is produced.

Οbρazuyuschiysya φτοροvοdοροd sορbiρueτsya φτορidami meτallοv (πρeimuschesτvennο meτallami I gρuππy πeρiοdichesκοy τablitsy, naπρimeρ, YΡ, ΝaΡ, ΚΡ), and πρi eτοm οbρazuyuτsya ποligidροφτορidy sοοτveτsτvuyuschiχ meτallοv.

25 The collection is based on a large proportion of the output of the metal: metal grade from 1: 1 to 1: 100, using a specially prepared metal grade. Before submitting to the event The metal powder allows activation by heating to a temperature of about 350 ° C, removing from volatile impurities and moisture.

Metal detergents may be used in 5 convenient, portable or restricted forms. Particle size, granule or table are not essential for the implementation of the reaction.

Such a metal product allows for a wide range of production and distribution cycles of a metal product. For the purpose of desorption, the saturated mixture is placed in the dispenser and gradually increases the temperature at a temperature of 25-100 ° C / h, bringing it to 350 ° С. A very slow rise in temperature is unreasonable, and quicker may cause the destruction of 15 buildings or disruption. The product obtained through the desorption of fuels may be used in the synthesis of fused compounds.

It is possible to administer the reaction zone as diluted with 20 inert gas (for example, nitrogen, argon or helium), and without dilution.

The process is carried out on a installation depicted on the drawing.

The installation is made up of mixer 1, process 2, 25 of separator 3 and step 4.

Β mixer 1 delivers the original salt ΝΗ ₄ Ρ »χΗΡ, where χ is greater than 0 to 1, 3, but χ may be equal to 1.3, and Partially activated metal grade I group. The agents are mixed in a given ratio for a single mass, and from the mixer they are fed into the reactor 2 with a diameter of 40 mm, 500 mm long, made of nickel. This 5 process reacts with a gaseous mixture or a mixture of inert gas. The temperature is between 20 and 125 ° C. There is a process of passing through. From the reaction, the reaction mixture is sent to phase 3, where the separation of the gas and the reaction products is effected. Gaseous products are collected in the receiver, then there they are directed to the separation stage, where they share the target product (not shown).

Other products, mainly those metal products, which are ΗΡ, are 15 in section 4, where there is a dispensing of 350 units. The selected product is condensed and assembled in the receiver (not shown), and metal products are returned to the mixing stage.

The process can be arranged in both primary and secondary modes, and in continuous mode. The above examples illustrate, but do not limit the scope of this invention.

The invention is illustrated by the examples given in the table. 25 ПΡИΜΕΡ 1.

Β Mixer 1 delivers 70g ΝΗ ₄ Ρ ^” ΗΡΗΡ where Χ = 0.01, and 700g ΝaΡ. Before doing this, a drug that wasn’t used in In the process, it is pre-activated in step 4, raising the temperature by 25 ° С per hour. Dοvedya τemπeρaτuρu dο 350 ° C, vydeρzhivayuτ φτορid naτρiya πρi eτοy τemπeρaτuρe in τechenie 5 hours Β smesiτel uκazannye 5 ρeagenτy ποdayuτ in οτnοshenii ΝaΡ:. ΝΗ ₄ Ρ ^»χΗΡ = 10 and smeshivayuτ iχ dο οdnοροdnοy mass. The size of the particles of solid reagents was around 200 microns.

2 React 2 from the mixer gives solid reagents at a rate of 385 g / h, and a gas-phase feed at a speed of 110 g / h. The facility is located in the territory of the Republic of Belarus.

80 ° C. The resulting reaction mixture from the inlet is discharged to separator 3, where the separation of the gaseous products is carried out. Gaseous products are released through the trap of acidic impurities (not

15 is shown in the diagram) and assembled in the receiver.

The gas analysis of gas-based products showed the following composition of the device. %: ΝΡ ₃ - 87%, Ν ₂ -1 1, 0%, other products (СΡ ₄ , Ν ₂ Ρ ₂ , Ν ₂ Ρ ₄ ) - 2.0%.

I say the phase consisting of ΝΗ ₄ Ρ ^« ΧΗΡ, where χ is less

20 or equal to 1, is supplied to the desorption stage ΗΡ, which is supplied at 350 ° С. The desorption time is 30 hours. After the desorption, they are cooled down to 20-60 ° С and sent to the mixer 1. They are not condensed in the trap (as a result of which is not used).

25 neutralization.

The other steps (2-11) of the activation and desorption step were described as described in Example 1. Examples of implementation of arcs are shown in the table.

The use of the process in the stated conditions makes it possible to fully utilize the original salt - to dispose of ammonia, to disinfect

Table. EXAMPLES OF IMPLEMENTATION OF EXPERIENCES

¹ Β gρaφe «φτορ iηi mixture" πρimeρa 9 - mixture φτορa azοτa and 10.5 + 10,5gρ; in the “gas phase composition” section, the introduced nitrogen is not taken into account

² - a mixture of phantoms ΝаΝ, ϋΡ and ΚΡ in the same way

Claims

10ΦΟΡΜULΑ IZBΟIA

1. The method of production of nitrogen by the formation of solid ammonium salt, which is

5 τem, chτο φτορiρuyuτ κisluyu sοl ποliφτορida ammοniya φορmuly ΝΗ ₄ Ρ ^«χΗΡ, where χ πρevyshaeτ 0 nο not πρevyshaeτ 1, 3, πρichem προtsess veduτ in πρisuτsτvii sορbenτa φτοροvοdοροda πρi massοvοm sοοτnοshenii sορbenτ: ΝΗ ₄ ^Ρ« χΗΡ οτ 2 dο 100 and temperature 20-125 ° С. 2. The method is π.1, which is different from the fact that, as a result of the connection of the product, use the connection of the utility, where it is metal, it is mixed.

3. Method πο π. 1 or 2, differing in that, in the 15th part of the product, the preferential use of KAN, YN,

ΚΡ or χ mixture.

4. The method for any of steps 1 to 3, which is different from the fact that there is a recirculation of the substance after the despatch from it is neglected

20 temperature up to 350 ° С.

5. Goodbye to any of ππ. 1 - 4, characterized by the fact that before transferring to the reaction, activation of the medium by stepped heating up to 350 ° С is carried out.