CN112371110B - Catalyst for synthesizing gas fire extinguishing agent trifluoroiodomethane by gas phase method and preparation method and application thereof - Google Patents
Catalyst for synthesizing gas fire extinguishing agent trifluoroiodomethane by gas phase method and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a catalyst for synthesizing gas fire extinguishing agent trifluoroiodomethane by a gas phase method, and a preparation method and application thereof, belonging to the field of organic chemical synthesis. Firstly, mixing a chloride solution, a nitrate solution and a metal salt solution, regulating the pH value by ammonia water, precipitating and filtering, washing by deionized water, drying, and compacting to obtain a catalyst precursor; and then the catalyst precursor is put into a fixed bed reactor for drying, and finally the catalyst is obtained after the catalyst precursor is activated by different activating gases. The catalyst provided by the invention can be used for preparing high-yield trifluoroiodomethane through a simple reaction system and under proper reaction conditions, the maximum yield of trifluoroiodomethane can reach 84.4%, and the catalyst has the advantages of low raw materials and convenient sources; the catalyst has good stability, can be recycled and has long service life; the solvent can be recycled; the product is simple to separate and purify; the synthesis process is safe and suitable for industrial production.
Description
Technical Field
The invention belongs to the field of organic chemical synthesis, and relates to a catalyst for synthesizing gas fire extinguishing agent trifluoroiodomethane by a gas phase method, and a preparation method and application thereof.
Background
Fire protection issues with energy storage power stations have attracted considerable attention in the industry. Currently, heptafluoropropane is widely used to suppress lithium ion battery fires. However, heptafluoropropane is a high temperature greenhouse gas. In recent years, the call for the reduction of the use of fire extinguishing gases with the high temperature chamber effect has become increasingly large. Trifluoroiodomethane (CAS Number: 2314-97-8) is a very good heptafluoropropane fire extinguishing agent substitute, and has the characteristics of high fire extinguishing efficiency and low greenhouse effect. Ozone Depletion Potential (ODP) is almost 0, and photodissociation reaction is easy to occur under ultraviolet irradiation, the atmospheric lifetime is short, the greenhouse effect potential (GWP) is also very low, and the Ozone Depletion Potential (ODP) is considered as one of ideal substitutes of fluorohydrocarbons (HFCs, HCFCs) and halon fire extinguishing agents. The trifluoroiodomethane has good environmental performance, is nontoxic, flame retardant, oil-soluble and material-compatible, and has incomparable advantages with other substitutes. Thus, the market demand for trifluoroiodomethane is great.
At present, many reports are made on the synthesis of trifluoroiodomethane. Patent (US 7132578) reports a route to trifluoroiodomethane in 20% yield from trifluorobromomethane, hydrogen, fluorine iodide in a solvent of dimethyl sulfoxide or dimethylformamide at 100 ℃ with 3% pd/C catalyst. The use of fluorine iodide increases the production cost and limits the industrialized popularization. Patent (JP-52-068110) reports CHF 3 And I 2 Preparation of CF by gas phase catalytic iodination reaction using active carbon supported alkaline earth metal salt as catalyst 3 I, a process of I. The catalyst shows better activity, but the catalyst has serious carbon deposit and shorter service life due to high reaction temperature, and the byproduct polymer leads I to 2 And the recycling of the (c) is difficult. Literature (NOGASAKI N. A novel catalytic technology for the manufacture of CF) 3 I. Speciality Chemical Magazine, 2002, 22 (5): 31-31. ) Adding proper amount of O in the reaction 2 The catalyst carbon deposit is reduced, the service life of the catalyst is prolonged, the AC carrier is prevented from being oxidized, and the CF is synthesized by a continuous one-step gas phase catalytic process 3 I. However, the use of oxygen increases the industrial safety risk, creating new impurities. Patent (JP 2005008543) describes a process for reacting CHF in the presence of a solid catalyst 3 And I 2 Reaction in gas phase to produce CF 3 I, a process of I. Characterized in that the catalyst is moved in the reactor, which is advantageous in suppressing the local heat release in the reactor, and the unreacted I can be recovered in a high purity form without adding an oxygen-containing gas 2 Thereby simplifying the equipment and reducing the production cost. Patent (101219925A) reports a simultaneous preparation of CF suitable for industrialization 3 I and C 2 F 5 I, a process of I. It uses porous metal fluoride or oxyfluoride as carrier, makes alkaline earth metal or Cu salt load and make into catalyst, then makes the catalyst produce reaction in O 2 N 2 In the presence of co-gas, for catalyzing CHF 3 Or C 2 HF 5 And I 2 The gas phase reaction is carried out at high temperature. The invention improves the yield of the trifluoroiodomethane from different degrees as soon as possible, however, the problems of complex process and safety of the process limit industrialized popularization and application. In addition, the reaction uses industrial raw materials which are not easy to prepare, and the possibility of industrial popularization is greatly limited.
From the above, it can be seen that the existing routes of trifluoroiodomethane have the characteristics of long routes, harsh conditions, very expensive raw materials, toxic fluorine iodide, high equipment requirements and more three wastes, and these limit the industrial production of trifluoroiodomethane.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a catalyst for synthesizing gas fire extinguishing agent trifluoroiodomethane by a gas phase method, a preparation method and application thereof, and the catalyst can prepare high-yield trifluoroiodomethane by utilizing a simple reaction system and suitable reaction conditions, and has the advantages of low cost and convenient sources of raw materials; the catalyst has good stability and long service life; the product is simple to separate and purify; the synthesis process is safe and suitable for industrial production.
In order to solve the technical problems, the invention adopts the following technical scheme: the preparation method of the catalyst for synthesizing the gas extinguishing agent trifluoroiodomethane by a gas phase method comprises the following steps of:
(1) Preparation of a catalyst precursor: mixing a chloride solution, a nitrate solution and a metal salt solution, wherein the chloride is magnesium chloride, chromium chloride or aluminum chloride; the nitrate is magnesium nitrate, chromium nitrate or aluminum nitrate; the metal salt is bismuth salt, titanium salt or nickel salt, and the mol ratio of the chloride to the sum of the chloride, the nitrate and the metal salt is 0.15-0.3:1, the mol ratio of the nitrate to the sum of the chloride, the nitrate and the metal salt is 0.1-0.35:1, a step of; dropwise adding ammonia water into the mixed solution, adjusting the pH value of the mixed solution to be 11.0, precipitating and filtering, washing with deionized water, drying, and pressing to form to obtain a catalyst precursor;
(2) Drying of the catalyst precursor: the catalyst precursor is put into a fixed bed reactor, the fixed bed reactor is heated by an open type pipe heating furnace, the catalyst precursor is firstly heated to 400 ℃ at 1-20 ℃/min under the protection of nitrogen gas at 100-500ml/min and then dried for 10 hours, and then the temperature is reduced to 200 ℃, so that the drying of the catalyst precursor is completed;
(3) Activation of the catalyst: heating the fixed bed reactor to 150-200 ℃, and activating the catalyst with 100ml/min nitrogen and 10ml/min hydrogen fluoride for 10 hours; then activating the catalyst with 100ml/min nitrogen and 20ml/min hydrogen fluoride for 10 hours; activating the catalyst with 50ml/min nitrogen and 100ml/min hydrogen fluoride for 10 hours; then activating the catalyst with 100ml/min of pure hydrogen fluoride for 10 hours; and then the temperature of the fixed bed reactor is increased to 300-400 ℃,100ml/min of pure hydrogen fluoride is used for activating the catalyst for 10 hours, and finally, the catalyst is naturally cooled to room temperature, thus obtaining the catalyst for synthesizing the gas fire extinguishing agent trifluoroiodomethane by a gas phase method.
The mol ratio of the chloride, the nitrate and the metal salt is 30:10:60.
the chloride is CrCl 3 Nitrate is Al (NO) 3 ) 3 The metal salt is Ti (NO) 3 ) 4 。
The invention also provides the catalyst for synthesizing the gas extinguishing agent trifluoroiodomethane by the gas phase method.
The synthesis gas for the gas phase methodThe application of the catalyst of the bulk fire extinguishing agent trifluoroiodomethane, and the method for synthesizing the gas fire extinguishing agent trifluoroiodomethane by a gas phase method comprises the following steps of: to trifluoro methane CF 3 H and CCl dissolved in carbon tetrachloride 4 Iodine simple substance I of (2) 2 Gas phase catalysis under the action of catalyst to generate trifluoroiodomethane CF 3 I。
The molar ratio of the trifluoromethane, the carbon tetrachloride and the iodine simple substance is 1:1-30:0.1-3.
The reaction temperature is 150-300 ℃, and the contact time of the gas phase material and the catalyst is 0.1-20s.
The beneficial effects are that: the catalyst provided by the invention can be used for preparing high-yield trifluoroiodomethane through a simple reaction system and under proper reaction conditions, the maximum yield of trifluoroiodomethane can reach 84.4%, and the catalyst has the advantages of low raw materials and convenient sources; the catalyst has good stability, can be recycled and has long service life; the solvent can be recycled; the product is simple to separate and purify; the synthesis process is safe and suitable for industrial production.
Detailed Description
The invention is further illustrated by the following description of specific embodiments, which are not intended to be limiting, and various modifications or improvements can be made by those skilled in the art in light of the basic idea of the invention, but are within the scope of the invention without departing from the basic idea of the invention.
Example 1
And (3) preparing a catalyst: crCl with the molar ratio of 30:10:60 is prepared 3 、Mg(NO 3 ) 2 、Bi(NO 3 ) 3 The solutions were mixed and 30wt.% aqueous ammonia was added dropwise to the mixed solution, adjusting ph=11.0. Filtering the precipitate, washing with deionized water, drying, and compression molding to obtain a catalyst precursor Cr-Mg-Bi;
the prepared catalyst precursor Cr-Mg-Bi is added into a fixed bed reactor, and the fixed bed reactor is heated by an open type tube heating furnace. The catalyst precursor is firstly heated to 400 ℃ at 1 ℃/min under the protection of 100ml/min nitrogen, then dried for 10 hours, and then the temperature is reduced to 200 ℃. This completes the drying process of the catalyst precursor.
The reactor was heated to 200℃and the catalyst was activated with 100ml/min nitrogen and 10ml/min hydrogen fluoride for 10 hours; then activating the catalyst with 100ml/min nitrogen and 20ml/min hydrogen fluoride for 10 hours; activating the catalyst with 50ml/min nitrogen and 100ml/min hydrogen fluoride for 10 hours; then activating the catalyst with 100ml/min of pure hydrogen fluoride for 10 hours; the fixed bed reactor was then heated to 400℃and 100ml/min of pure hydrogen fluoride was used to activate the catalyst for 10 hours. Thus completing the activation process of the catalyst, and finally naturally cooling to room temperature to obtain the catalyst Cr-Mg-Bi.
The reactor was heated to 230℃and 50ml of Cr-Mg-Bi was used as the reaction catalyst, 407.8g of carbon tetrachloride CCl was fed by peristaltic pump at a rate of 0.1g/min 4 And iodine I 2 Is a mixture (CCl) 4 And I 2 The molar ratio is 15: 1) 49.0g of trifluoromethane CF with a flow rate of 67.2ml/min 3 H enters the mixing cavity together and is uniformly mixed. Then, the mixture was passed through a reactor to a buffer bottle, a water washing bottle, a concentrated alkali absorber and a cooling collector. After the end of the experiment, 163g of organic material was received in total. Wherein trifluoroiodomethane CF 3 The weight of I was 102.2g. The yield calculated as trifluoromethane was 74.4%.
Example 2
And (3) preparing a catalyst: crCl with the molar ratio of 30:10:60 is prepared 3 、Al(NO 3 ) 3 、Ti(NO 3 ) 4 The solutions were mixed and 30wt.% aqueous ammonia was added dropwise to the mixed solution, adjusting ph=11.0. Filtering the precipitate, washing with deionized water, drying, and compression molding to obtain a catalyst precursor Cr-Al-Ti;
the prepared catalyst precursor Cr-Al-Ti is added into a fixed bed reactor, and the fixed bed reactor is heated by an open type tube heating furnace. The catalyst was dried for 10 hours at 1 c/min to 400 c under the protection of 100ml/min nitrogen, and then the temperature was reduced to 200 c. This completes the drying process of the catalyst.
The reactor was heated to 150℃and the catalyst was activated with 100ml/min nitrogen and 10ml/min hydrogen fluoride for 10 hours; then activating the catalyst with 100ml/min nitrogen and 20ml/min hydrogen fluoride for 10 hours; activating the catalyst with 50ml/min nitrogen and 100ml/min hydrogen fluoride for 10 hours; then activating the catalyst with 100ml/min of pure hydrogen fluoride for 10 hours; the fixed bed reactor was then heated to 300℃and 100ml/min of pure hydrogen fluoride was used to activate the catalyst for 10 hours. Thus completing the activation process of the catalyst, and finally naturally cooling to room temperature to obtain the catalyst Cr-Al-Ti.
The reactor was heated to 200deg.C and 50ml of Cr-Al-Ti was used as the reaction catalyst, 407.8g of a mixture of carbon tetrachloride and iodine (CCl) was pumped by peristaltic pump at a rate of 0.1g/min 4 And I 2 The molar ratio is 15: 1) Enters a mixing cavity together with 49.0g of trifluoromethane with the flow rate of 67.2ml/min and is uniformly mixed. Then, the mixture was passed through a reactor to a buffer bottle, a water washing bottle, a concentrated alkali absorber and a cooling collector. After the end of the experiment, 184g of organic material was received in total. Wherein the trifluoroiodomethane is 115.8g. The yield was 84.4% calculated as trifluoromethane.
Example 3
And (3) preparing a catalyst: mgCl with the mol ratio of 30:10:60 2 、Cr(NO 3 ) 3 、Bi(NO 3 ) 3 The solutions were mixed and 30wt.% aqueous ammonia was added dropwise to the mixed solution, adjusting ph=11.0. Filtering the precipitate, washing with deionized water, drying, and compression molding to obtain catalyst precursor Mg-Cr-Bi;
and adding the prepared catalyst precursor Mg-Cr-Bi into a fixed bed reactor, and heating the fixed bed reactor by using an open type tube heating furnace. The catalyst was dried for 10 hours at 5 c/min to 400 c under nitrogen protection at 300ml/min, and then the temperature was reduced to 200 c. This completes the drying process of the catalyst.
The reactor was heated to 150℃and the catalyst was activated with 100ml/min nitrogen and 10ml/min hydrogen fluoride for 10 hours; then activating the catalyst with 100ml/min nitrogen and 20ml/min hydrogen fluoride for 10 hours; activating the catalyst with 50ml/min nitrogen and 100ml/min hydrogen fluoride for 10 hours; then activating the catalyst with 100ml/min of pure hydrogen fluoride for 10 hours; the fixed bed reactor was then heated to 300℃and 100ml/min of pure hydrogen fluoride was used to activate the catalyst for 10 hours. Thus completing the activation process of the catalyst, and finally naturally cooling to room temperature to obtain the catalyst Mg-Cr-Bi.
The reactor was heated to 170℃and 50ml of Mg-Cr-Bi was used as the reaction catalyst, 407.8g of a mixture of carbon tetrachloride and iodine (CCl) was fed at a rate of 0.1g/min using a peristaltic pump 4 And I 2 The molar ratio is 15: 1) Enters a mixing cavity together with 49.0g of trifluoromethane with the flow rate of 67.2ml/min and is uniformly mixed. Then, the mixture was passed through a reactor to a buffer bottle, a water washing bottle, a concentrated alkali absorber and a cooling collector. After the end of the experiment, 124g of organics were received in total. Wherein the trifluoroiodomethane is 65.3g. The yield calculated as trifluoromethane was 47.6%.
Example 4
And (3) preparing a catalyst: crCl with the molar ratio of 30:30:40 is prepared 3 、Mg(NO 3 ) 2 、Bi(NO 3 ) 3 The solutions were mixed and 30wt.% aqueous ammonia was added dropwise to the mixed solution, adjusting ph=11.0. Filtering the precipitate, washing with deionized water, drying, and compression molding to obtain a catalyst precursor Cr-Mg-Bi;
the prepared catalyst precursor Cr-Mg-Bi is added into a fixed bed reactor, and the fixed bed reactor is heated by an open type tube heating furnace. The catalyst precursor is firstly heated to 400 ℃ at 1 ℃/min under the protection of 100ml/min nitrogen, then dried for 10 hours, and then the temperature is reduced to 200 ℃. This completes the drying process of the catalyst precursor.
The reactor was heated to 200℃and the catalyst was activated with 100ml/min nitrogen and 10ml/min hydrogen fluoride for 10 hours; then activating the catalyst with 100ml/min nitrogen and 20ml/min hydrogen fluoride for 10 hours; activating the catalyst with 50ml/min nitrogen and 100ml/min hydrogen fluoride for 10 hours; then activating the catalyst with 100ml/min of pure hydrogen fluoride for 10 hours; the fixed bed reactor was then heated to 400℃and 100ml/min of pure hydrogen fluoride was used to activate the catalyst for 10 hours. Thus completing the activation process of the catalyst, and finally naturally cooling to room temperature to obtain the catalyst Cr-Mg-Bi.
Example 5
And (3) preparing a catalyst: alCl with the mol ratio of 15:35:50 is added 3 、Cr(NO 3 ) 3 、Ni(NO 3 ) 3 The solutions were mixed and 30wt.% aqueous ammonia was added dropwise to the mixed solution, adjusting ph=11.0. Filtering the precipitate, washing with deionized water, drying,compression molding to obtain a catalyst precursor Al-Cr-Ni;
the prepared catalyst precursor Al-Cr-Ni is added into a fixed bed reactor, and the fixed bed reactor is heated by an open type tube heating furnace. The catalyst was dried for 10 hours at 1 c/min to 400 c under the protection of 100ml/min nitrogen, and then the temperature was reduced to 200 c. This completes the drying process of the catalyst.
The reactor was heated to 150℃and the catalyst was activated with 100ml/min nitrogen and 10ml/min hydrogen fluoride for 10 hours; then activating the catalyst with 100ml/min nitrogen and 20ml/min hydrogen fluoride for 10 hours; activating the catalyst with 50ml/min nitrogen and 100ml/min hydrogen fluoride for 10 hours; then activating the catalyst with 100ml/min of pure hydrogen fluoride for 10 hours; the fixed bed reactor was then heated to 300℃and 100ml/min of pure hydrogen fluoride was used to activate the catalyst for 10 hours. Thus completing the activation process of the catalyst, and finally naturally cooling to room temperature to obtain the catalyst Al-Cr-Ni.
Comparative example 1
And (3) preparing a catalyst: caCl with the mol ratio of 30:10:60 is used for preparing the catalyst 2 、Cu(NO 3 ) 2 、Ni(NO 3 ) 3 The solutions were mixed and 30wt.% aqueous ammonia was added dropwise to the mixed solution, adjusting ph=11.0. Filtering the precipitate, washing with deionized water, drying, and compression molding to obtain a catalyst precursor Ca-Cu-Ni;
the prepared catalyst precursor Ca-Cu-Ni is added into a fixed bed reactor, and the fixed bed reactor is heated by an open tube heating furnace. The catalyst was dried for 10 hours at 5 c/min to 400 c under nitrogen protection at 300ml/min, and then the temperature was reduced to 200 c. This completes the drying process of the catalyst.
The reactor was heated to 150 ℃,100ml/min nitrogen and 10ml/min hydrogen fluoride to activate the catalyst for 10 hours; activating the catalyst with 100ml/min nitrogen and 20ml/min hydrogen fluoride for 10 hours; activating the catalyst with 50ml/min nitrogen and 100ml/min hydrogen fluoride for 10 hours; activating the catalyst with 100ml/min pure hydrogen fluoride for 10 hours; the temperature was raised to 300℃and 100ml/min of pure hydrogen fluoride activated the catalyst for 10 hours. This completes the activation process of the Ca-Cu-Ni catalyst.
The reactor was heated to 190℃and 50ml of Ca-Cu-Ni was used as the reaction catalyst, 407.8g of a mixture of carbon tetrachloride and iodine (CCl) was fed at a rate of 0.1g/min using a peristaltic pump 4 And I 2 The molar ratio is 15: 1) Enters a mixing cavity together with 49.0g of trifluoromethane with the flow rate of 67.2ml/min and is uniformly mixed. Then, the mixture was passed through a reactor to a buffer bottle, a water washing bottle, a concentrated alkali absorber and a cooling collector. After the end of the experiment, 108g of organics were received in total. Wherein the trifluoroiodomethane is 26.3g. The yield was 19.2% calculated as trifluoromethane.
Claims (6)
1. The preparation method of the catalyst for synthesizing the gas extinguishing agent trifluoroiodomethane by a gas phase method is characterized by comprising the following steps of:
(1) Preparation of a catalyst precursor: mixing a chloride solution, a nitrate solution and a metal salt solution, wherein the chloride is CrCl 3 The method comprises the steps of carrying out a first treatment on the surface of the The nitrate is Al (NO) 3 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The metal salt is Ti (NO) 3 ) 4 The mol ratio of the chloride to the sum of the chloride, the nitrate and the metal salt is 0.15-0.3:1, the mol ratio of the nitrate to the sum of the chloride, the nitrate and the metal salt is 0.1-0.35:1, a step of; dropwise adding ammonia water into the mixed solution, adjusting the pH value of the mixed solution to be 11.0, precipitating and filtering, washing with deionized water, drying, and pressing to form to obtain a catalyst precursor;
(2) Drying of the catalyst precursor: the catalyst precursor is put into a fixed bed reactor, the fixed bed reactor is heated by an open type pipe heating furnace, the catalyst precursor is firstly heated to 400 ℃ at 1-20 ℃/min under the protection of nitrogen gas at 100-500ml/min and then dried for 10 hours, and then the temperature is reduced to 200 ℃, so that the drying of the catalyst precursor is completed;
(3) Activation of the catalyst: heating the fixed bed reactor to 150-200 ℃, and activating the catalyst with 100ml/min nitrogen and 10ml/min hydrogen fluoride for 10 hours; then activating the catalyst with 100ml/min nitrogen and 20ml/min hydrogen fluoride for 10 hours; activating the catalyst with 50ml/min nitrogen and 100ml/min hydrogen fluoride for 10 hours; then activating the catalyst with 100ml/min of pure hydrogen fluoride for 10 hours; and then the temperature of the fixed bed reactor is increased to 300-400 ℃,100ml/min of pure hydrogen fluoride is used for activating the catalyst for 10 hours, and finally, the catalyst is naturally cooled to room temperature, thus obtaining the catalyst for synthesizing the gas fire extinguishing agent trifluoroiodomethane by a gas phase method.
2. The method for preparing the catalyst for synthesizing gas fire extinguishing agent trifluoroiodomethane by gas phase method according to claim 1, wherein the molar ratio of chloride, nitrate and metal salt is 30:10:60.
3. a catalyst for gas phase synthesis of gas fire extinguishing agent trifluoroiodomethane prepared according to the method of claim 1 or 2.
4. Use of a catalyst for gas phase synthesis of gas fire extinguishing agent trifluoroiodomethane as claimed in claim 3, wherein the gas phase synthesis of gas fire extinguishing agent trifluoroiodomethane comprises the steps of: the gas phase catalysis of the trifluoro methane and the iodine simple substance dissolved in the carbon tetrachloride is carried out under the action of the catalyst to generate trifluoro methyl iodide.
5. The application of the catalyst for synthesizing gas fire extinguishing agent trifluoroiodomethane by gas phase method according to claim 4, wherein the mole ratio of the trifluoromethane, carbon tetrachloride and iodine elementary substance is 1:1-30:0.1-3.
6. The use of a catalyst for gas phase synthesis of a gaseous extinguishing agent trifluoroiodomethane according to claim 4, wherein the reaction temperature is 150-300 ℃ and the contact time of the gaseous material with the catalyst is 0.1-20s.
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| CN112371110A (en) | 2021-02-19 |
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