Industrial equipment for producing fluorophosgene

Abstract

The present invention provides an industrial apparatus for producing fluorophosgene, comprising: a reactor having a reaction chamber formed therein; the first gas inlet mechanism comprises a first gas inlet pipe, a distributor and a plurality of groups of nozzles with different lengths, the distributor is arranged in the reaction cavity, the first gas inlet pipe is communicated with the distributor, the distributor is sequentially provided with a plurality of annular gas inlet areas from outside to inside, and the length of the nozzles arranged on the gas inlet area on the outer side is smaller than that of the nozzles arranged on the gas inlet area on the inner side; the second gas inlet mechanism is communicated with the reaction cavity; and the exhaust mechanism is communicated with the reaction cavity. According to the industrial equipment for producing fluorophosgene provided by the invention, the length of the nozzles arranged on the outer side gas inlet area is smaller than that of the nozzles arranged on the inner side gas inlet area, the longer nozzles are arranged at the high-pressure position of the distributor, and the shorter nozzles are arranged around the low-pressure position of the distributor, so that the temperatures of the reaction are relatively balanced; the generation of a by-product CF4 due to overhigh local temperature or local excessive fluorination caused by violent reaction is avoided.

Description

Technical Field

[0001] The present invention relates to the technical field of reaction vessels, and in particular to an industrial device for producing fluorophosgene. Background Art

[0002] As a chemical substance with broad application prospects, fluorophosgene has shown unique value in many fields such as fine chemical synthesis, preparation of fluorinated ether intermediates and etching of electronic products. Especially in the manufacture of electronic products, the purity of fluorophosgene is required to be extremely high because it directly affects the performance and quality of the final product.

[0003] However, in the production of fluorophosgene and its related chemical reactions, due to the special chemical properties of fluorine, the reaction conditions with CO must be strictly controlled, otherwise impurities such as carbon tetrafluoride (CF4) will be generated. These impurities will not only reduce the purity of the product, but also seriously affect the yield of the product, thereby increasing production costs and reducing production efficiency. Summary of the invention

[0004] The present invention provides an industrial device for producing fluorophosgene, which is used to solve the problem that impurities such as carbon tetrafluoride are easily generated in the fluorophosgene production process, thereby affecting the yield of the product.

[0005] The present invention provides an industrial device for producing fluorophosgene, comprising: A reactor having a reaction chamber formed therein; A first air intake mechanism, comprising a first air intake pipe, a distributor and a plurality of groups of nozzles of different lengths, wherein the distributor is arranged in the reaction chamber, the first air intake pipe is communicated with the distributor, the distributor is sequentially provided with a plurality of air intake areas in an annular shape from the outside to the inside, a plurality of groups of nozzles are respectively arranged in the plurality of air intake areas, and the nozzles are all communicated with the distributor, the length of the nozzles arranged on the outer air intake area is less than the length of the nozzles arranged on the inner air intake area, so that CO is introduced through the first air intake pipe, the distributor and the plurality of groups of nozzles of different lengths; A second gas inlet mechanism, connected to the reaction chamber, for introducing fluorine gas; The exhaust mechanism is connected to the reaction chamber and is used to discharge the gas after the reaction.

[0006] According to an industrial equipment for producing fluorophosgene provided by the present invention, the nozzle is provided with three groups, namely an outer layer nozzle, a middle layer nozzle and an inner layer nozzle with increasing lengths in sequence; the distributor is provided with an outer layer air inlet area, a middle layer air inlet area and an inner layer air inlet area in sequence from the outside to the inside, the outer layer nozzle is arranged in the outer layer air inlet area, the middle layer nozzle is arranged in the middle layer air inlet area, and the inner layer nozzle is arranged in the inner layer air inlet area.

[0007] According to an industrial device for producing fluorophosgene provided by the present invention, the cross-sectional area of ​​the nozzle is 75%-95% of the cross-sectional area of ​​the first air inlet pipe.

[0008] According to an industrial device for producing fluorophosgene provided by the present invention, the length of the outer layer nozzle is 4-6 cm, the length of the middle layer nozzle is 9-11 cm, and the length of the inner layer nozzle is 14-16 cm.

[0009] According to an industrial equipment for producing fluorophosgene provided by the present invention, the size of the corresponding spray hole of the outer layer nozzle is 1mm-2mm, the size of the corresponding spray hole of the middle layer nozzle is 2mm-3mm, and the size of the corresponding spray hole of the inner layer nozzle is 2mm-4mm.

[0010] According to the industrial equipment for producing fluorophosgene provided by the present invention, the nozzle is a copper nozzle, a nickel nozzle or an alloy nozzle.

[0011] An industrial device for producing fluorophosgene provided by the present invention further comprises: The cooling layer is sleeved outside the reactor, a heat exchange cavity is arranged inside the cooling layer, and a cooling medium inlet and a cooling medium outlet communicated with the heat exchange cavity are arranged in the cooling layer.

[0012] According to an industrial equipment for producing fluorophosgene provided by the present invention, the cooling layer is a jacket, and the jacket tightly and evenly covers the outer wall of the reactor to form a closed heat exchange chamber, and the cooling medium inlet and cooling medium outlet are respectively arranged at the upper and lower ends of the jacket.

[0013] According to an industrial device for producing fluorophosgene provided by the present invention, the second air intake mechanism includes: a second air intake pipe, which is arranged on the reactor and communicated with the bottom of the reaction chamber.

[0014] According to an industrial device for producing fluorophosgene provided by the present invention, the exhaust mechanism comprises: an exhaust pipe, which is arranged on the reactor and communicated with the top of the reaction chamber.

[0015] The industrial equipment for producing fluorophosgene provided by the present invention has a nozzle with a gradient design, and the length of the nozzle arranged on the outer air inlet zone is shorter than the length of the nozzle arranged on the inner air inlet zone, so as to dissipate heat more effectively during the reaction process. A longer nozzle is arranged at a position where the distributor pressure is high to control the flow rate; a shorter nozzle is arranged around the low pressure of the distributor to ensure that the flow rate at the outlet of each nozzle is stable, so that the various temperatures of the reaction are relatively balanced, avoiding local excessive temperature or local excessive fluorination caused by violent reaction, thereby effectively reducing the generation of by-product CF4. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to more clearly illustrate the technical solutions in the present invention or the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0017] Figure 1 It is a schematic diagram of an industrial device for producing fluorophosgene provided in an embodiment of the present invention.

[0018] Figure 2 It is a schematic diagram of a first air intake mechanism provided in an embodiment of the present invention.

[0019] Reference numerals: 100. Reactor; 200, first air intake mechanism; 201, first air intake pipe; 202, distributor; 203, outer layer nozzle; 204, middle layer nozzle; 205, inner layer nozzle; 300, second air intake mechanism; 400, exhaust mechanism; 500, cooling layer; 501, cooling medium inlet; 502, cooling medium outlet. DETAILED DESCRIPTION

[0020] In order to make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be clearly and completely described below in conjunction with the drawings of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0021] Combine the following Figure 1-Figure 2 The industrial plant for producing fluorophosgene provided by the present invention is described.

[0022] In some embodiments, Figure 1 and Figure 2As shown, the industrial equipment for producing fluorophosgene includes: a reactor 100, a first air intake mechanism 200, a second air intake mechanism 300 and an exhaust mechanism 400. A reaction chamber is formed inside the reactor 100; the first air intake mechanism 200 includes a first air intake pipe 201, a distributor 202 and a plurality of nozzles of different lengths, the distributor 202 is arranged in the reaction chamber, the first air intake pipe 201 is connected to the distributor 202, the distributor 202 is provided with a plurality of annular air intake zones from the outside to the inside, the plurality of nozzles are respectively arranged in the plurality of air intake zones, and the nozzles are all connected to the distributor 202, the length of the nozzle arranged on the outer air intake zone is less than the length of the nozzle arranged on the inner air intake zone, so as to introduce CO through the first air intake pipe 201 and the distributor 202 in conjunction with the plurality of nozzles of different lengths; the second air intake mechanism 300 is connected to the reaction chamber for introducing fluorine gas; the exhaust mechanism 400 is connected to the reaction chamber for extracting the gas after the reaction.

[0023] In this embodiment, the reactor 100 includes a reaction chamber, which is the main place for fluorophosgene production. The first air inlet pipe 201 of the first air inlet mechanism 200 is used to transport the raw gas CO (carbon monoxide) into the reactor 100. The distributor 202 is located in the reaction chamber and is designed with multiple annular air inlet zones, arranged from the outside to the inside. Multiple groups of nozzles are respectively arranged in each air inlet zone and are connected to the distributor 202. The length of the nozzle changes with the change of the position of the air inlet zone, and the nozzle length of the outer air inlet zone is less than the nozzle length of the inner air inlet zone. The second air inlet mechanism 300 is used to introduce fluorine gas into the reaction chamber. The exhaust mechanism 400 is used to extract the reacted gas.

[0024] When fluorophosgene needs to be produced, CO is fed from the first air inlet pipe 201 into the distributor 202 through the first air inlet mechanism 200. Since the nozzle adopts a gradient design, CO will enter the reaction chamber according to a predetermined flow rate and temperature distribution. At the same time, fluorine gas is introduced into the reaction chamber through the second air inlet mechanism 300. Fluorination reaction occurs between fluorine gas and CO in the reaction chamber.

[0025] During the reaction, the operator needs to pay close attention to the temperature, pressure and other parameters in the reaction chamber, and adjust the flow rate of the first air intake mechanism 200 and the second air intake mechanism 300 according to the actual situation to keep the reaction going smoothly. The gradient design of the nozzle helps to dissipate heat more effectively during the reaction, and prevents local over-temperature or over-fluorination by controlling the flow rate.

[0026] After the reaction is completed, the gas after the reaction is discharged through the exhaust mechanism 400 and is subsequently processed to collect the fluorophosgene product.

[0027] The industrial equipment for producing fluorophosgene provided by the present invention has a nozzle with a gradient design. The length of the nozzle arranged on the outer air inlet zone is shorter than the length of the nozzle arranged on the inner air inlet zone, so as to dissipate heat more effectively during the reaction. A longer nozzle is arranged at a high-pressure position of the distributor 202 to control the flow rate; a shorter nozzle is arranged around the low-pressure position of the distributor 202 to ensure that the flow rate at the outlet of each nozzle is stable, so that the various temperatures of the reaction are relatively balanced, avoiding local excessive temperature or local excessive fluorination caused by violent reaction, thereby effectively reducing the generation of by-product CF4.

[0028] In some embodiments, Figure 1 and Figure 2 As shown, the nozzles are provided in three groups, namely, an outer layer nozzle 203, a middle layer nozzle 204 and an inner layer nozzle 205, the lengths of which increase successively; the distributor 202 is provided with an outer layer air intake area, a middle layer air intake area and an inner layer air intake area from the outside to the inside, the outer layer nozzle 203 is arranged in the outer layer air intake area, the middle layer nozzle 204 is arranged in the middle layer air intake area, and the inner layer nozzle 205 is arranged in the inner layer air intake area.

[0029] Specifically, the outer layer nozzles 203 are arranged in the outer layer air inlet area, which is a group of nozzles with the shortest length. Since the outer layer air inlet area is usually located at the edge of the reactor 100, its pressure is relatively low, so the shorter nozzles can ensure sufficient flow rate in this area while avoiding excessive local temperature.

[0030] The middle layer nozzle 204 is arranged in the middle layer air inlet area and has a moderate length. The pressure in this area is between the outer layer and the inner layer, so the length of the nozzle also needs to be adjusted accordingly to maintain a stable flow rate and temperature distribution.

[0031] The inner layer nozzle 205 is arranged in the inner layer air inlet area and is the longest group of nozzles. The inner layer air inlet area is usually located in the center of the reactor 100, where the pressure is the highest. The longer nozzle can slow down the flow rate, prevent the local temperature from being too high due to the excessive flow rate, and ensure that the fluorination reaction can proceed evenly.

[0032] The distributor 202 is provided with an outer gas inlet zone, a middle gas inlet zone and an inner gas inlet zone from the outside to the inside, and each gas inlet zone is connected to a nozzle of a corresponding length. This design ensures that the raw gas (CO) can enter the reaction chamber according to a predetermined flow rate and temperature distribution, thereby improving the efficiency of the fluorination reaction and the product quality.

[0033] Through the gradient design of the nozzle and the partitioning arrangement of the distributor 202, the device can dissipate heat more effectively, control the flow rate, and maintain the balance of the reaction temperature during operation, which helps to reduce the generation of the byproduct CF4 and improve the purity and production efficiency of fluorophosgene.

[0034] Example 1 The cross-sectional area of ​​the first air inlet pipe 201 and the cross-sectional area data S2 of the second air inlet pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air inlet pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×75%=1.3245, and the test shows that the content of the impurity CF4 finally produced accounts for 3.5% of the fluorophosgene.

[0035] Example 2 The cross-sectional area of ​​the first air inlet pipe 201 and the cross-sectional area data S2 of the second air inlet pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air inlet pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×75%=1.6777, and the test shows that the content of the impurity CF4 finally produced accounts for 4.7% of the fluorophosgene.

[0036] Example 3 The cross-sectional area of ​​the first air inlet pipe 201 and the cross-sectional area data S2 of the second air inlet pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air inlet pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×50%=0.883. The test shows that the content of the impurity CF4 finally produced accounts for 3.7% of the fluorophosgene.

[0037] Comparative Example 1 The cross-sectional area of ​​the first air inlet pipe 201 and the cross-sectional area data S2 of the second air inlet pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air inlet pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×120%=2.1192. The test shows that the content of the impurity CF4 finally produced accounts for 8.6% of the fluorophosgene.

[0038] Comparative Example 2 The cross-sectional area of ​​the first air inlet pipe 201 and the cross-sectional area data S2 of the second air inlet pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air inlet pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×150%=2.679. The test shows that the content of the impurity CF4 finally produced accounts for 10.2% of the fluorophosgene.

[0039] Comparative Example 3 The cross-sectional area of ​​the first air inlet pipe 201 and the cross-sectional area data S2 of the second air inlet pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air inlet pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×70%=1.2362, and the test shows that the content of the impurity CF4 finally produced accounts for 3.48% of the fluorophosgene.

[0040] From Example 1, Example 2, Example 3 and Comparative Example 1, Comparative Example 2 and Comparative Example 3, the following information can be observed: When the cross-sectional area S1 of the nozzle is 70%-75% of the cross-sectional area of ​​the first air inlet pipe 201 (and the second air inlet pipe, which have the same cross-sectional area) (Example 1 and Comparative Example 3), the content of the generated impurity CF4 is relatively low, about 3.48%-3.5% of fluorophosgene.

[0041] When the cross-sectional area S1 of the nozzle is 75%-95% of the cross-sectional area of ​​the first intake pipe 201 (Examples 1, 2 and 3), the content of the generated impurity CF4 is between 3.5% and 4.7%, which is relatively low.

[0042] When the cross-sectional area S1 of the nozzle exceeds 95% of the cross-sectional area of ​​the first intake pipe 201 (Comparative Examples 1 and 2), the content of the generated impurity CF4 increases significantly, reaching 8.6%-10.2%.

[0043] From the above analysis, we can conclude that: When the cross-sectional area of ​​the nozzle is between 70% and 95% of the cross-sectional area of ​​the first air intake pipe 201, the content of the impurity CF4 generated is relatively low. But more specifically, when the cross-sectional area of ​​the nozzle is close to 75% (as shown in Example 1 and Comparative Example 3), the impurity content reaches the lowest. However, considering that the difference between Example 3 and Example 1 is not large and both are within a relatively low range, it can be considered that 70%-95% is a wider but still effective range.

[0044] Example 4 The cross-sectional area of ​​the first air intake pipe 201 and the cross-sectional area data S2 of the second air intake pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air intake pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×75%=1.3245. The temperature is controlled at 110°C. The number and size of nozzles: 42 (the nozzle size is 2 mm in diameter).

[0045] When the lengths of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 3 cm, 7 cm and 10 cm respectively, the test shows that the content of the impurity CF4 finally produced accounts for 5.6% of the fluorophosgene.

[0046] Example 5 The cross-sectional area of ​​the first air intake pipe 201 and the cross-sectional area data S2 of the second air intake pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air intake pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×75%=1.3245. The temperature is controlled at 110°C. The number and size of nozzles: 42 (the nozzle size is 2 mm in diameter).

[0047] When the lengths of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 5 cm, 10 cm and 15 cm respectively, the test shows that the content of the impurity CF4 finally produced accounts for 3.9% of the fluorophosgene.

[0048] Example 6 The cross-sectional area of ​​the first air intake pipe 201 and the cross-sectional area data S2 of the second air intake pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air intake pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×75%=1.3245. The temperature is controlled at 110°C. The number and size of nozzles: 42 (the nozzle size is 2 mm in diameter).

[0049] When the lengths of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 8 cm, 12 cm and 17 cm respectively, the test shows that the content of the impurity CF4 finally produced accounts for 3.7% of the fluorophosgene.

[0050] Control group 4 The cross-sectional area of ​​the first air intake pipe 201 and the cross-sectional area data S2 of the second air intake pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air intake pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×75%=1.3245. The temperature is controlled at 110°C. The number and size of nozzles: 42 (the nozzle size is 2 mm in diameter).

[0051] When the lengths of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are all 5 cm, the test shows that the content of the impurity CF4 finally produced accounts for 5.2% of the fluorophosgene.

[0052] Control group 5 The cross-sectional area of ​​the first air intake pipe 201 and the cross-sectional area data S2 of the second air intake pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air intake pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×75%=1.3245. The temperature is controlled at 110°C. The number and size of nozzles: 42 (the nozzle size is 2 mm in diameter).

[0053] When the lengths of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are all 10 cm, the test shows that the content of the impurity CF4 finally produced accounts for 4.7% of the fluorophosgene.

[0054] Control group 6 The cross-sectional area of ​​the first air intake pipe 201 and the cross-sectional area data S2 of the second air intake pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air intake pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×75%=1.3245. The temperature is controlled at 110°C. The number and size of nozzles: 42 (the nozzle size is 2 mm in diameter).

[0055] When the lengths of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are all 15 cm, the test shows that the content of the impurity CF4 finally produced accounts for 4.5% of the fluorophosgene.

[0056] From Example 4, Example 5, Example 6 and Control Group 4, Control Group 5 and Control Group 6, the following information can be observed: When the lengths of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 3 cm, 7 cm and 10 cm respectively, the content of the impurity CF4 is relatively high, which is 5.6%.

[0057] When the lengths of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 5 cm, 10 cm and 15 cm respectively, the content of impurity CF4 decreases to 3.9%.

[0058] When the lengths of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are further adjusted to 8 cm, 12 cm and 17 cm, the content of impurity CF4 increases slightly but still remains at a low level of 3.7%.

[0059] In the control group, when the nozzle lengths of all layers were the same and were 5 cm, 10 cm, and 15 cm, respectively, the contents of impurity CF4 were 5.2%, 4.7%, and 4.5%, respectively, which were higher or close to the minimum contents in Examples 5 and 6, but lower than the content in Example 4.

[0060] From the data, it can be seen that the nozzle length combination in Example 6 (8 cm for the outer layer, 12 cm for the middle layer, and 17 cm for the inner layer) produces a relatively low impurity content (3.7%), although it is slightly higher than 3.9% in Example 5.

[0061] The final conclusion is based on a comprehensive analysis of all test data: When the length of the outer nozzle 203 is in the range of 4-6 cm, it helps to reduce the impurity content (although this conclusion is not directly drawn from the data, but is based on the comparison of Example 4 and Control 4). Preferably, it is 5 cm.

[0062] When the length of the middle layer nozzle 204 is in the range of 9-11 cm (close to the lengths in Examples 5 and 6), the impurity content is relatively low. Preferably, it is 10 cm.

[0063] When the length of the inner layer nozzle 205 is in the range of 14-16 cm (close to the length in Example 6), the impurity content is also kept at a low level. Preferably, it is 15 cm.

[0064] Example 7 The cross-sectional area of ​​the first air intake pipe 201 and the cross-sectional area data S2 of the second air intake pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air intake pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×75%=1.3245. The temperature is controlled at 110°C. The number and size of nozzles: 42 (the lengths of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 5 cm, 10 cm, and 15 cm respectively) The number of inner, middle and outer nozzles is (9, 14, and 14).

[0065] When the sizes of the corresponding nozzle holes of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 1 mm, 2 mm and 2.5 mm respectively, the test shows that the content of the impurity CF4 finally produced accounts for 3.3% of the fluorophosgene.

[0066] Example 8 The cross-sectional area of ​​the first air intake pipe 201 and the cross-sectional area data S2 of the second air intake pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air intake pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×75%=1.3245. The temperature is controlled at 110°C. The number and size of nozzles: 42 (the lengths of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 5 cm, 10 cm, and 15 cm respectively) The number of inner, middle and outer nozzles is (9, 14, and 14).

[0067] When the sizes of the corresponding nozzle holes of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 1.5 mm, 2.5 mm and 3 mm respectively, the test shows that the content of the impurity CF4 finally produced accounts for 6.7% of the fluorophosgene.

[0068] Example 9 The cross-sectional area of ​​the first air intake pipe 201 and the cross-sectional area data S2 of the second air intake pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air intake pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×75%=1.3245. The temperature is controlled at 110°C. The number and size of nozzles: 42 (the lengths of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 5 cm, 10 cm, and 15 cm respectively) The number of inner, middle and outer nozzles is (9, 14, and 14).

[0069] When the sizes of the corresponding nozzle holes of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 1.5 mm, 2.5 mm and 3 mm respectively, the test shows that the content of the impurity CF4 finally produced accounts for 9.9% of the fluorophosgene.

[0070] Comparative Example 7 The cross-sectional area of ​​the first air intake pipe 201 and the cross-sectional area data S2 of the second air intake pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air intake pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×75%=1.3245. The temperature is controlled at 110°C. The number and size of nozzles: 42 (the lengths of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 5 cm, 10 cm, and 15 cm respectively) The number of inner, middle and outer nozzles is (9, 14, and 14).

[0071] When the sizes of the corresponding nozzle holes of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are all 1.5 mm, the test shows that the content of the impurity CF4 finally produced accounts for 4.2% of the fluorophosgene.

[0072] Comparative Example 8 The cross-sectional area of ​​the first air intake pipe 201 and the cross-sectional area data S2 of the second air intake pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air intake pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×75%=1.3245. The temperature is controlled at 110°C. The number and size of nozzles: 42 (the lengths of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 5 cm, 10 cm, and 15 cm respectively) The number of inner, middle and outer nozzles is (9, 14, and 14).

[0073] When the sizes of the corresponding nozzle holes of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are all 2.0 mm, the test shows that the content of the impurity CF4 finally produced accounts for 3.6% of the fluorophosgene.

[0074] Comparative Example 9 The cross-sectional area of ​​the first air intake pipe 201 and the cross-sectional area data S2 of the second air intake pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air intake pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×75%=1.3245. The temperature is controlled at 110°C. The number and size of nozzles: 42 (the lengths of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 5 cm, 10 cm, and 15 cm respectively) The number of inner, middle and outer nozzles is (9, 14, and 14).

[0075] When the sizes of the corresponding nozzle holes of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 2.5 mm, 2 mm and 1 mm respectively, the test shows that the content of the impurity CF4 finally produced accounts for 7.8% of the fluorophosgene.

[0076] Comparative Example 10 The cross-sectional area of ​​the first air intake pipe 201 and the cross-sectional area data S2 of the second air intake pipe of CO are both 1.766 cm2. The flow rate or flow rate data of the second air intake pipe of CO are both 1.5 m3 / h (3 m / s). The cross-sectional area S1 of the nozzle is 1.766 cm2×75%=1.3245. The temperature is controlled at 110°C. The number and size of nozzles: 42 (the lengths of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 5 cm, 10 cm, and 15 cm respectively) The number of inner, middle and outer nozzles is (9, 14, and 14).

[0077] When the sizes of the corresponding nozzle holes of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 2 mm, 2.5 mm and 1 mm respectively, the test shows that the content of the impurity CF4 finally produced accounts for 5.9% of the fluorophosgene.

[0078] From Example 7, Example 8, Example 9 and Comparative Example 7, Comparative Example 8, Comparative Example 9 and Comparative Example 10, the following information can be observed: When the nozzle sizes of the outer layer nozzle 203, the middle layer nozzle 204 and the inner layer nozzle 205 are 1 mm, 2 mm and 2.5 mm respectively (Example 7), the content of the generated impurity CF4 is relatively low, which is 3.3%.

[0079] When the orifice size increases, the content of impurity CF4 generally increases. For example, in Examples 8 and 9, as the orifice size increases, the impurity content increases from 6.7% to 9.9%.

[0080] In the comparative examples, when the nozzle orifice sizes of all layers are the same (Comparative Example 7, Comparative Example 8), or the combination of orifice sizes is not optimal (Comparative Example 9, Comparative Example 10), the content of impurity CF4 is generally higher than the minimum content in Example 7.

[0081] Next, it was necessary to determine which set of nozzle orifice sizes would produce the lowest impurity CF4 content.

[0082] From the data, it can be seen that the nozzle size combination in Example 7 (1mm for the outer layer, 2mm for the middle layer, and 2.5mm for the inner layer) produces the lowest impurity content (3.3%). This combination is consistent with the final conclusion range given in the question, but provides more specific values.

[0083] The final conclusion is based on a comprehensive analysis of all test data: In order to produce a relatively low impurity CF4 content, the recommended nozzle hole size of the outer nozzle 203 is 1mm-2mm (optimally 1mm).

[0084] The recommended nozzle hole size of the middle layer nozzle 204 is 2 mm-3 mm (the optimal size is 2 mm, but considering that there is little difference between Example 7 and Comparative Example 8, 3 mm is also an acceptable choice).

[0085] The recommended nozzle size of the inner nozzle 205 is 2 mm to 4 mm (optimum is 2.5 mm, but 4 mm may also be an effective upper limit in practical applications, although it will lead to a slight increase in impurity content).

[0086] In summary, in order to produce a relatively low impurity CF4 content, the recommended nozzle hole size of the outer layer nozzle 203 is 1mm-2mm, the nozzle hole size of the middle layer nozzle 204 is 2mm-3mm, and the nozzle hole size of the inner layer nozzle 205 is 2mm-4mm. The optimal combination is 1mm for the outer layer, 2mm for the middle layer, and 2.5-3mm for the inner layer.

[0087] In some embodiments, the nozzle is a copper nozzle, a nickel nozzle, or an alloy nozzle. Copper is a commonly used metal material and has a certain catalytic effect in chemical reactions. However, in some cases, copper may react with reactants to form impurities. Nickel is a high-temperature resistant and corrosion-resistant metal and is often used to manufacture equipment that works in high temperature or corrosive environments. In chemical reactions, the catalytic activity of nickel is relatively low, so it may react less with reactants. An alloy is a mixture of two or more metal elements, and generally has better comprehensive properties than a single metal. Alloy nozzles can be customized according to specific chemical reaction requirements to optimize reaction efficiency and product purity.

[0088] In some embodiments, Figure 1 and Figure 2 As shown, the industrial equipment for producing fluorophosgene also includes: a cooling layer 500, which is sleeved outside the reactor 100, a heat exchange cavity is provided in the cooling layer 500, and the cooling layer 500 is provided with a cooling medium inlet 501 and a cooling medium outlet 502 connected to the heat exchange cavity.

[0089] In this embodiment, by adjusting the flow rate and temperature of the cooling medium, the temperature in the reactor 100 can be accurately controlled to ensure that the reaction is carried out within the optimal temperature range. If the heat generated during the reaction is not removed in time, it may cause the temperature to rise, thereby affecting the reaction rate and product distribution. The cooling layer 500 can effectively remove this heat to prevent the temperature increase from adversely affecting the reaction.

[0090] Optionally, the cooling layer 500 may be designed as a jacket, tightly and evenly covering the outer wall of the reactor 100 to form a closed heat exchange chamber. This design can ensure good contact between the cooling medium and the wall of the reactor 100, thereby improving the heat exchange efficiency.

[0091] The cooling medium inlet 501 and the cooling medium outlet 502 are respectively arranged at the upper and lower ends of the jacket, so that the cooling medium can flow evenly in the heat exchange chamber, further improving the heat exchange efficiency. The selection of the cooling medium depends on the specific reaction conditions and requirements. Commonly used cooling media include water, ethylene glycol, brine, etc. These media have good thermal conductivity and chemical stability, and can effectively remove heat without interfering with the chemical reaction.

[0092] In some embodiments, Figure 1 and Figure 2 As shown, the second air intake mechanism 300 includes: a second air intake pipe. The second air intake pipe is arranged on the reactor 100 and is connected to the bottom of the reaction chamber. The second air intake pipe is mainly used to introduce the second gas required for the reaction (such as CO in this case) into the reactor 100. Since the second air intake pipe is connected to the bottom of the reaction chamber, introducing the gas from the bottom of the reactor 100 can promote the uniform distribution of the gas in the reaction chamber. This helps to ensure that the reactants can fully contact and react throughout the reaction chamber. Bottom air intake can also help control the temperature gradient in the reactor 100. When the cold gas enters from the bottom, it will exchange heat with the hotter part of the reaction chamber, which helps to reduce the local high temperature and thus maintain a more stable reaction temperature.

[0093] In some embodiments, Figure 1 and Figure 2 As shown, the exhaust mechanism 400 includes: an exhaust pipe, which is arranged on the reactor 100 and communicated with the top of the reaction chamber.

[0094] In this embodiment, the main purpose of the exhaust mechanism 400 is to discharge the gas generated after the reaction in the reactor 100 is completed (including the target product fluorophosgene and other possible by-products or unreacted gases) from the reaction chamber.

[0095] The exhaust pipe is connected to the top of the reaction chamber to ensure that the gas generated after the reaction is completed can be discharged smoothly. This design helps to avoid gas accumulation in the reactor 100, thereby maintaining the pressure balance and gas flow in the reactor 100.

[0096] In addition, during the reaction process, some unwanted impurities or by-products may be generated. The design of the exhaust pipe can be combined with other purification devices (such as filters, washing towers, etc.) to help remove these impurities and improve the purity of the product. The exhaust pipe can also serve as a channel for pressure regulation in the reactor 100. By controlling the opening size of the exhaust pipe and / or equipping a pressure control device (such as a pressure valve, a regulating valve, etc.), the pressure in the reactor 100 can be accurately adjusted to meet the needs of specific reaction conditions.

[0097] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. An industrial device for producing fluorophosgene, characterized in that: include: A reactor having a reaction chamber formed therein; A first air intake mechanism, comprising a first air intake pipe, a distributor and a plurality of groups of nozzles of different lengths, wherein the distributor is arranged in the reaction chamber, the first air intake pipe is communicated with the distributor, the distributor is sequentially provided with a plurality of air intake areas in an annular shape from the outside to the inside, a plurality of groups of nozzles are respectively arranged in the plurality of air intake areas, and the nozzles are all communicated with the distributor, the length of the nozzles arranged on the outer air intake area is less than the length of the nozzles arranged on the inner air intake area, so that CO is introduced through the first air intake pipe, the distributor and the plurality of groups of nozzles of different lengths; A second gas inlet mechanism, connected to the reaction chamber, for introducing fluorine gas; The exhaust mechanism is connected to the reaction chamber and is used to discharge the gas after the reaction.

2. The industrial equipment for producing fluorophosgene according to claim 1, characterized in that The nozzles are provided in three groups, namely, an outer layer nozzle, a middle layer nozzle and an inner layer nozzle, the lengths of which increase successively; the distributor is provided with an outer layer air intake area, a middle layer air intake area and an inner layer air intake area from the outside to the inside, the outer layer nozzle is arranged in the outer layer air intake area, the middle layer nozzle is arranged in the middle layer air intake area, and the inner layer nozzle is arranged in the inner layer air intake area.

3. The industrial equipment for producing fluorophosgene according to claim 1, characterized in that: The cross-sectional area of ​​the nozzle is 75%-95% of the cross-sectional area of ​​the first air intake pipe.

4. The industrial equipment for producing fluorophosgene according to claim 2, characterized in that: The length of the outer layer nozzle is 4-6 cm, the length of the middle layer nozzle is 9-11 cm, and the length of the inner layer nozzle is 14-16 cm.

5. The industrial equipment for producing fluorophosgene according to claim 2, characterized in that: The size of the corresponding spray hole of the outer layer nozzle is 1mm-2mm, the size of the corresponding spray hole of the middle layer nozzle is 2mm-3mm, and the size of the corresponding spray hole of the inner layer nozzle is 2mm-4mm.

6. The industrial equipment for producing fluorophosgene according to claim 1, characterized in that The nozzle is a copper nozzle, a nickel nozzle or an alloy nozzle.

7. The industrial equipment for producing fluorophosgene according to any one of claims 1 to 6, characterized in that: Also includes: The cooling layer is sleeved outside the reactor, a heat exchange cavity is arranged inside the cooling layer, and a cooling medium inlet and a cooling medium outlet communicated with the heat exchange cavity are arranged in the cooling layer.

8. The industrial equipment for producing fluorophosgene according to claim 7, characterized in that The cooling layer is a jacket, which tightly and evenly covers the outer wall of the reactor to form a closed heat exchange cavity. The cooling medium inlet and the cooling medium outlet are respectively arranged at the upper and lower ends of the jacket.

9. The industrial equipment for producing fluorophosgene according to any one of claims 1 to 6, characterized in that: The second air intake mechanism comprises: a second air intake pipe, which is arranged on the reactor and communicated with the bottom of the reaction chamber.

10. The industrial equipment for producing fluorophosgene according to any one of claims 1 to 6, characterized in that: The exhaust mechanism comprises an exhaust pipe, which is arranged on the reactor and communicated with the top of the reaction chamber.

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