CN218609428U - For FNO 2 Reactor for preparation - Google Patents
For FNO 2 Reactor for preparation Download PDFInfo
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- CN218609428U CN218609428U CN202222855122.1U CN202222855122U CN218609428U CN 218609428 U CN218609428 U CN 218609428U CN 202222855122 U CN202222855122 U CN 202222855122U CN 218609428 U CN218609428 U CN 218609428U
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Abstract
The utility model provides a be used for FNO 2 The reactor is a straight tube type and is sequentially divided into a feeding section, a heating section and a cooling section; one end of the feeding section is symmetrically provided with a fluorine gas inlet and a nitrogen dioxide inlet; heating units are arranged around the heating section in a surrounding manner; the middle part of the heating section is further provided with a temperature sensor; be provided with cooling coil around the cooling zone, just the cooling zone is kept away from the one end of heating section is provided with the product gas export, cooling coil includes cooling water discharge port and cooling water import.
Description
Technical Field
The utility model relates to a be used for FNO 2 Preparation of reactors, especially for the direct reaction of fluorine and nitrogen dioxide to FNO 2 The reactor of (1).
Background
FNO 2 Gases, namely nitroxyl fluorides, also known as fluorinated nitroxyl fluorides, are colorless gases, liquids or white solids with pungent odor, often used as oxidizers in rocket propellants.
At present, no FNO is found in China 2 The report of the preparation method of (2) is only FNO 2 The laboratory preparation methods of (1) mainly use fluorine gas and nitrate (or CoF) 3 Etc. fluoride and nitrogen oxide) under specific conditions, the method is only suitable for trace preparation, and most importantly, the method has high danger and cannot be applied industrially. At present, no FNO is found 2 Reports on the prepared reactor.
SUMMERY OF THE UTILITY MODEL
The utility model provides a be used for FNO 2 The prepared reactor can effectively solve the problems.
The utility model discloses a realize like this:
the utility model provides a be used for FNO 2 The reactor is a straight tube type and is sequentially divided into a feeding section, a heating section and a cooling section; one end of the feeding section is symmetrically provided with a fluorine inlet and a nitrogen dioxide inlet; heating units are arranged around the heating section in a surrounding manner; the middle part of the heating section is further provided with a temperature sensor; be provided with cooling coil around the cooling zone, just the cooling zone is kept away from the one end of heating section is provided with the product gas export, cooling coil includes cooling water discharge port and cooling water import.
The beneficial effects of the utility model are that: the utility model provides a be used for FNO 2 The prepared reactor can be suitable for preparing FNO by direct reaction of fluorine gas and nitrogen dioxide 2 The technical process solves the problem of preparing FNO by fluoride and nitrate in a laboratory 2 Thereby making FNO 2 The industrial preparation of the compound becomes possible.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention, and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a flow chart of a FNO2 gas production method according to an embodiment of the present invention.
FIG. 2 is a schematic diagram of an embodiment of the present invention for FNO 2 The structure of the prepared reactor is shown schematically.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the drawings of the embodiments of the present invention are combined to clearly and completely describe the technical solutions of the embodiments of the present invention, and obviously, the described embodiments are some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
Referring to FIG. 1, an embodiment of the present invention provides an FNO 2 A method for producing a gas, comprising the steps of:
s1, fluorine gas and NO 2 Introducing gas into the reactor, controlling the reaction temperature at 300-500 ℃ to obtain a product FNO 2 And (4) crude gas.
Referring to fig. 2, the reactor is a straight tube type, and is sequentially divided into a feeding section 10, a heating section 12 and a cooling section 14, wherein the length of each section is 100 mm-2000 mm, and the temperature of the heating section 12 is 300-500 ℃. Preferably, each segment has a length of 500mm to 1800mm, and in one embodiment, each segment has a length of about 1500mm. It can be understood that by controlling the length of each segment, the raw materials can be fully mixed and reacted, and the conversion efficiency can be improved. The length-diameter ratio of the straight tube reactor can be 10:1 to 1.5.
Specifically, one end of the feeding section 10 is symmetrically provided with a fluorine gas inlet 101 and a nitrogen dioxide inlet 102. The fluorine inlet 101 and the nitrogen dioxide inlet 102 are elbow type, and extend along the other end of the feeding section 10. The length of the feeding section 10 is 100 mm-2000 mm. Preferably, the length of the feeding section 10 is 500mm to 1000mm. In one embodiment, the feed section 10 has a length of 600mm and a diameter of 60mm. The other end of the feeding section 10 is hermetically connected with the heating section 12 through a first connecting flange 11. In particular, the first connecting flange 11 may be a convex connecting flange, so that the feeding section 10 and the heating section 12 can form a good sealing connection. The use of flange can make the utility model discloses a reactor, the maintenance is conveniently dismantled.
The length of the heating section 12 is 100 mm-2000 mm. Preferably, the length of the heating section 12 is 1000mm to 1500mm. In one embodiment, the heating section 12 has a length of 1200mm and a diameter of about 180 mm. Heating units 121 are disposed around the heating section 12 for heating the heating section 12 to a reaction temperature. The middle part of the heating section 12 is further provided with a temperature sensor 122, so that stable temperature control of the heating section 12 can be realized. The other end of the heating section 12, which is far away from the feeding section 10, is also provided with a second connecting flange 13, and the second connecting flange 13 is used for being connected with the cooling section 14 in a sealing manner. The second connecting flange 13 may also be a convex connecting flange.
The length of the cooling section 14 is 100 mm-2000 mm. Preferably, the length of the cooling section 14 is 1500mm to 1800mm. In one embodiment, the cooling section 14 has a length of 1700mm and a diameter of about 200 mm. A cooling coil 141 is arranged around the cooling section 14, and a product gas outlet 144 is arranged at one end of the cooling section 14 far away from the heating section 12. The cooling coil 141 includes a cooling water discharge port 142 and a cooling water inlet port 143.
As a further improvement, the reactor preferably employs a nickel-containing alloy. More preferably, a nickel-copper alloy is selected. The nickel base in the nickel-containing alloy can generate passivation reaction with fluorine gas, so that the reactor can be operated efficiently for a long time without being corroded. Therefore, as a further improvement, in other embodiments, before step S1, the method may further include:
s11, introducing a fluorine-nitrogen mixed gas and a pure fluorine gas into the reactor in sequence for pretreatment. The ratio of fluorine gas to nitrogen gas in the fluorine-nitrogen mixed gas is 1. The pretreatment is carried out by using the fluorine-nitrogen mixed gas with lower activity, so that the excessive corrosion of the reactor in the early stage can be prevented; then, the passivation treatment is carried out by pure fluorine gas, so that a fluorine gas passivation film is formed in the reactor.
As a further improvement, it is preferable that the reaction temperature is 300 to 450 ℃; more preferably, the reaction temperature is 350 to 400 ℃. In one embodiment, the reaction temperature is controlled in the range of 360-400 ℃.
As a further improvement, the fluorine gas and NO 2 The gas is mixed according to a molar ratio of 1:1.0 to 3.5. Proved by a large number of experiments, the fluorine gas and NO 2 Ratio of gas to FNO 2 The gas yield of the raw gas has a major impact. Preferably, the fluorine gas and NO 2 The gas is mixed according to a molar ratio of 1:2.0 to 2.5. More preferably, the fluorine gas and NO 2 The gas is mixed according to a molar ratio of 1:2.0 to 2.3.
As a further improvement, the NO 2 The gas is obtained by the following method:
mixing industrial liquid N 2 O 4 Heating and gasifying to obtain gas NO 2 Then the gasified gas NO 2 After passing through a calcium fluoride molecular sieve, the temperature is raised to 70-110 ℃. After being treated by calcium fluoride molecular sieve, the gas NO can be treated 2 The content of (A) is not less than 90% by volume. Preferably, the gasified gas NO 2 After passing through a calcium fluoride molecular sieve, the temperature is raised to 85-105 ℃. More preferably, the gasified gas NO 2 Passing through calcium fluoride molecular sieve, and heating to 90-100 deg.C. In one embodiment, the gasified gas NO is 2 After passing through calcium fluoride molecular sieve, the temperature is raised to about 95 ℃, thereby leading the NO gas to be 2 The volume content of the calcium fluoride can reach about 98 percent, and the calcium fluoride molecular sieve is shown in the table 1 (the length of the calcium fluoride molecular sieve is about 0.5 meter, the pressure is standard atmospheric pressure, about 0.1 MPa), and the NO can be seen from the table 1 along with the increase of the temperature 2 Is significantly increased, probably due to the calcium fluoride molecular pair N with increasing temperature 2 O 4 The adsorption performance of (3) is increased. However, when the temperature reached 95 ℃, there was some decrease in the volume concentration with increasing temperature, probably due to the increase in temperature N 2 O 4 Is desorbed by calcium fluoride molecular sieve.
TABLE 1
As a further improvement, the fluorine gas is obtained by the following method:
f prepared by electrolytic cell 2 The gas is treated by a cold trap at-60 to-70 ℃ to remove hydrogen fluoride impurities, thus obtaining fluorine gas with volume content of about 95 to 97 percent. The fluorine gas raw material can be anode gas (fluorine gas volume content is about 90%) obtained by electrolyzing industrial HF by using a medium-temperature electrolytic cell. Further, the fluorine gas having a volume content of about 95 to 97% may be further purified by using an adsorbent so that the content becomes 99% or more. The adsorbent is specifically: a granular form having a plurality of micropores, and comprising: 35 to 50 parts of sodium fluoride powder, 20 to 30 parts of potassium fluoride powder and 3 to 5 parts of binder.
The preparation method of the adsorbent comprises the following steps:
s11, weighing 35-50 parts of sodium fluoride powder, 20-30 parts of potassium fluoride powder, 3-6 parts of binder and 3-8 parts of diluent according to mass fraction, adding into an oil bath pan at 180-200 ℃, uniformly mixing, and melting to form a mixed solution;
s12, placing the mixed solution into a spherical mold, carrying out mold pressing in a press at 180-200 ℃, and cooling at room temperature to obtain a spherical fluoride salt mixture, wherein the mold pressing pressure is 0.2-1 Mpa;
s13, putting the spherical fluoride salt mixture into a solvent to extract a diluent, wherein the solvent is a volatile organic solvent;
s14, taking out the extracted spherical fluoride salt, volatilizing the solvent, and finally blowing the surface of the product with nitrogen to obtain the fluoride salt adsorbent with high porosity.
As a further improvement, in step S11, the binder is selected from binders capable of forming sodium fluoride powder and potassium fluoride powder into good binding performance, such as polyvinylidene fluoride, styrene-butadiene rubber emulsion, carboxymethyl cellulose, and the like. In one embodiment, the binder is selected from polyvinylidene fluoride, which can form good binding performance for sodium fluoride powder and potassium fluoride powder. The content of the binder is not too high, and although the binding effect is good, the binder is easy to block channels and is difficult to form high porosity.
The diluent is selected from materials capable of infiltrating the three materials, such as benzophenone, or other ketone compounds containing benzene rings.
For further improvement, preferably, 36 to 40 parts of sodium fluoride powder, 22 to 25 parts of potassium fluoride powder, 3 to 6 parts of binder and 5 to 8 parts of diluent are weighed. In one embodiment, 36 parts of sodium fluoride powder, 24 parts of potassium fluoride powder, 5 parts of binder and 5 parts of diluent are weighed.
As a further improvement, the temperature of the oil bath pan is preferably 185 to 195 ℃, and in one embodiment the temperature of the oil bath pan is about 190 ℃.
Generally, to increase the filling rate, it is generally pressed to form a spherical fluoride salt mixture. As a further modification, in step S12, the mixed solution is placed in a spherical mold having a diameter of 5 to 15 mm. The pressure of the die pressing needs to be strictly controlled, if the pressure is too high, the formed spherical fluoride salt mixture is too dense, and the later-stage diluent needs a long time to finish the extraction or is difficult to completely extract; in addition, if the pressure is too small, the resulting spherical fluoride salt mixture does not have sufficient strength, and the column of the clogged adsorbent is easily crushed. Therefore, it is preferable that the pressure for molding is 0.4 to 0.6MPa. In one embodiment, the pressure of the molding is about 0.55MPa.
As a further modification, in step S13, the volatile organic solvent includes ethanol, diethyl ether and a mixture thereof. The extraction time is 10-20 hours, which can be selected according to actual needs and is limited by completely extracting the diluent. In one example, the spherical fluoride salt mixture was placed in ethanol for 18 hours to completely extract benzophenone.
As a further improvement, the ratio of the volatile organic solvent to the spherical fluoride salt mixture in the extraction process can be controlled to be 10-50ml. Preferably, the ratio of the volatile organic solvent to the spherical fluoride salt mixture can be controlled to be 20-30ml.
In step S14, the spherical fluoride salt after extraction is taken out, and then left at room temperature to naturally volatilize the solvent.
The embodiment of the utility model provides a further provide a fluorine is adsorbent for purification, fluorine is adsorbent for purification for the preparation according to above-mentioned method and obtains. The moisture content of the final product of the adsorbent for fluorine gas purification is less than or equal to 0.2%, and the internal porosity can reach more than 50%.
Example A-1
Taking 36 g of sodium fluoride powder, 24 g of potassium fluoride powder, 5 g of polyvinylidene fluoride and 5 g of benzophenone, sequentially adding the materials into an oil bath kettle at 190 ℃, uniformly stirring, melting for 1.5 hours to form a mixed solution, and putting the mixed solution into the oil bath kettle
The spherical mold is pressed in a press at 190 ℃ under the pressure of 0.55Mpa, cooled at 25 ℃ for 20 hours for molding, and the product is put into ethanol for extraction for 18 hours after molding, and the extraction is finishedAnd then placing the extract in the air for 36 hours to volatilize the ethanol, blowing the surface with nitrogen after the ethanol is volatilized, and measuring the moisture content of the final product to be 0.14 percent and the internal porosity to be 57.6 percent.
Example A-2
The same as example 1 except that: 30 g of sodium fluoride powder and 20 g of potassium fluoride powder are taken, and the moisture content of the final product is measured to be 0.13 percent, and the internal porosity is measured to be 55.4 percent.
Examples A to 3
The same as example 1 except that: 50 g of sodium fluoride powder and 30 g of potassium fluoride powder are taken, and the moisture content of the final product is measured to be 0.16 percent, and the internal porosity is measured to be 58.9 percent.
Comparative examples A to 4
The same as example 1 except that: 25 g of sodium fluoride powder and 15 g of potassium fluoride powder are taken, and the moisture content of the final product is measured to be 0.11 percent, and the internal porosity is measured to be 48.5 percent.
Comparative examples A to 5
The same as example 1 except that: 55 g of sodium fluoride powder and 35 g of potassium fluoride powder are taken, and the moisture content of the final product is measured to be 0.20 percent, and the internal porosity is measured to be 59.2 percent.
Comparative examples A to 6
The same as example 1 except that: 25 g of sodium fluoride powder and 35 g of potassium fluoride powder are taken, and the moisture content of the final product is measured to be 0.11 percent, and the internal porosity is measured to be 48.5 percent.
Comparative examples A to 7
The same as example 1 except that: 55 g of sodium fluoride powder and 15 g of potassium fluoride powder are taken, and the moisture content of the final product is measured to be 0.20 percent, and the internal porosity is measured to be 59.2 percent.
The examples A-1 to A-3 and the comparative examples A-4 to A-7 were subjected to the following adsorption tests:
the product is placed in a stainless steel adsorption tower, the temperature is controlled at 20 ℃, 95 percent of fluorine gas is introduced, and the flow velocity of the fluorine gas is 1m/s. The fluorine gas content and the hydrogen fluoride content (volume content) of the outlet gas component were measured as shown in table 2 below:
table 2 shows the gas contents of examples A-1 to A-3 and comparative examples A-4 to A-7 (wherein the balance is impurity gas)
From the above data, it can be seen that the adsorption performance of the adsorbent for hydrogen fluoride is greatly changed as the ratio of sodium fluoride powder to potassium fluoride powder is changed.
As a further improvement, the preparation method further comprises the following steps:
s2, mixing FNO 2 Introducing the crude gas into a condenser at the temperature of-30 to-50 ℃ to remove impurities such as nitrogen dioxide and the like;
s3, and then FNO in the step S2 2 Introducing the gas into a rectifying tower, and further removing FNO and oxygen and nitrogen impurities under the pressure of 0.1-0.3 MPa.
Example B-1
The fluorine gas flow rate is 0.3kg/h; NO 2 Flow rate 0.72kg/h (molar ratio 1;
the purification temperature of fluorine gas is-80 ℃; the fluorine gas purification pressure was 0.1MPa;
NO 2 the purification temperature is 95 ℃; NO 2 The purification pressure is 0.1MPa;
the reaction temperature is 360-400 ℃; the reaction pressure is 0.1MPa
FNO in crude gas 2 The output is 0.9kg/h; FNO in crude gas 2 The content was 88% (v/v).
Example B-2
The fluorine gas flow rate is 0.3kg/h; NO (nitric oxide) 2 The flow rate was 0.90kg/h (molar ratio 1;
the purification temperature of fluorine gas is-80 ℃; the fluorine gas purification pressure was 0.1MPa;
NO 2 the purification temperature is 95 ℃; NO 2 The purification pressure is 0.1MPa;
the reaction temperature is 360-400 ℃; the reaction pressure is 0.1MPa
FNO in crude gas 2 The output is 0.93kg/h; FNO in crude gas 2 The content was 93% (v/v).
Further, FNO 2 Introducing the crude gas into a condenser at the temperature of minus 45 ℃ to remove impurities such as nitrogen dioxide and the like; then controlThe working temperature of the rectifying tower is-30 ℃; the working pressure of the rectifying tower is 0.2MPa, and high-purity FNO with the purity of more than 99 percent can be obtained 2 A gas.
Example B-3
The flow rate of fluorine gas was 0.3kg/h; NO (nitric oxide) 2 Flow rate 0.60kg/h (molar ratio 1;
the purification temperature of fluorine gas is-80 ℃; the fluorine gas purification pressure was 0.1MPa;
NO 2 the purification temperature is 95 ℃; NO 2 The purification pressure is 0.1MPa;
the reaction temperature is 360-400 ℃; the reaction pressure is 0.1MPa
FNO in crude gas 2 The output is 0.7kg/h; FNO in crude gas 2 The content was 78% (v/v).
Example B-4
The flow rate of fluorine gas was 0.3kg/h; NO 2 Flow rate 0.37kg/h (molar ratio 1;
the purification temperature of fluorine gas is-80 ℃; the fluorine gas purification pressure was 0.1MPa;
NO 2 the purification temperature is 95 ℃; NO 2 The purification pressure is 0.1MPa;
the reaction temperature is 360-400 ℃; the reaction pressure is 0.1MPa
FNO in crude gas 2 The output is 0.4kg/h; FNO in crude gas 2 The content was 60% (v/v).
Example B-5
The fluorine gas flow rate is 0.3kg/h; NO (nitric oxide) 2 The flow rate is 1.29kg/h (molar ratio is 1;
the purification temperature of fluorine gas is-80 ℃; the fluorine gas purification pressure was 0.1MPa;
NO 2 the purification temperature is 95 ℃; NO 2 The purification pressure is 0.1MPa;
the reaction temperature is 360-400 ℃; reaction pressure 0.1MPa
FNO in crude gas 2 The output is 0.52kg/h; FNO in crude gas 2 The content was 33% (v/v).
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. For FNO 2 The prepared reactor is characterized in that the reactor is in a straight pipe type and is sequentially divided into a feeding section, a heating section and a cooling section;
one end of the feeding section is symmetrically provided with a fluorine inlet and a nitrogen dioxide inlet;
heating units are arranged around the heating section in a surrounding manner; the middle part of the heating section is further provided with a temperature sensor;
be provided with cooling coil around the cooling zone, just the cooling zone is kept away from the one end of heating section is provided with the product gas export, cooling coil includes cooling water discharge port and cooling water import.
2. The FNO of claim 1 2 The prepared reactor is characterized in that the length of each section is 100-2000 mm, and the length-diameter ratio of the straight tube type reactor is 10:1 to 1.5.
3. The FNO of claim 1 2 The prepared reactor is characterized in that the material of the reactor adopts nickel-containing alloy.
4. The FNO of claim 1 2 The prepared reactor is characterized in that the material of the reactor adopts nickel-copper alloy.
5. The FNO of claim 1 2 The prepared reactor is characterized in that the length of the feeding section is 500 mm-1000 mm; the length of the feeding section is 1000 mm-1500 mm; the length of the cooling section is 1500 mm-1800 mm.
6. The FNO of claim 1 2 The prepared reactor is characterized in that the interior of the reactor is provided with fluorine gas passivationAnd (3) a film.
7. The FNO of claim 1 2 The reactor is characterized in that the fluorine gas inlet and the nitrogen dioxide inlet are bent pipes and extend along the other end of the feeding section.
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| CN202222855122.1U CN218609428U (en) | 2022-10-28 | 2022-10-28 | For FNO 2 Reactor for preparation |
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