A catalyst for preparing 1,1,1,2,3-pentafluoropropane by hydrogenating 1,1,1,2,3-pentafluoropropene, a preparation method and application thereof
The catalyst prepared by hydrolysis coprecipitation method, using a catalyst composed of alumina, Cu, Mo and Nb, achieves efficient hydrogenation synthesis of 1,1,1,2,3-pentafluoropropylene in a fixed-bed reactor. This solves the problems of low catalytic activity and selectivity in existing technologies, achieving high conversion rate and selectivity, and is suitable for industrial production.
Patent Information
- Application Number
- CN202311737959.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-18
- Publication Date
- 2025-12-19
- Estimated Expiration
- 2043-12-18
AI Technical Summary
Existing technologies are difficult to use for efficient and continuous synthesis of 1,1,1,2,3-pentafluoropropane, and the catalysts have low activity and selectivity, which makes it difficult to meet the needs of industrial production.
The catalyst was prepared by hydrolysis coprecipitation method, using alumina as support, Cu as active component, and Mo and Nb as auxiliary components. The hydrogenation reaction of 1,1,1,2,3-pentafluoropropylene was carried out in a fixed-bed reactor. The active metal content of the catalyst and the type and concentration of the precipitant were controlled to achieve efficient synthesis of the catalyst.
The catalyst exhibits excellent catalytic activity and selectivity at low temperatures, with high conversion rates of 1,1,1,2,3-pentafluoropropene and high selectivity for 1,1,1,2,3-pentafluoropropane. It is suitable for various solvent systems, has a long catalyst lifetime, and is simple and safe to operate, making it suitable for industrial production.
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Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of 1,1,1,2,3-pentafluoropropane preparation, and particularly relates to a catalyst for preparing 1,1,1,2,3-pentafluoropropane by hydrogenation of 1,1,1,2,3-pentafluoropropene, and a preparation method and application thereof. BACKGROUND
[0002] 1,1,1,2,3-pentafluoropropane (HFC-245eb) is an ideal blowing agent, which has excellent physical properties, environmental protection performance, low boiling point and low thermal conductivity, is friendly to the environment compared with HCFC, has zero ozone depletion potential (ODP) and low greenhouse effect potential (GWP), has a molecular weight of 134.05 g / mol, a density of 1.267 g / m 3 3, a boiling point of 23 DEG C, and is a non-flammable, non-toxic and colorless gas, and becomes an important product for ODS replacement in the spraying field; compared with CFC-1 and HCFC-141b, HFC-245eb has a lower boiling point and a higher vapor pressure, can improve some properties of the foam, and will replace the gradually eliminated HCFC blowing agent in the spraying field, especially the performance at low temperature, so that the foam has strong mechanical properties within a certain temperature range.
[0003] Therefore, it is urgent to realize the continuous hydrogenation of 1,1,1,2,3-pentafluoropropene to synthesize 1,1,1,2,3-pentafluoropropane (HFC-245eb) by a simple process. SUMMARY
[0004] The application provides a catalyst for preparing 1,1,1,2,3-pentafluoropropane by hydrogenation of 1,1,1,2,3-pentafluoropropene, and a preparation method and application thereof, the catalyst has a simple preparation process, a large space for regulating the content of active metals, is suitable for different solvent systems, and has wide operation conditions, when 1,1,1,2,3-pentafluoropropane is continuously synthesized in a fixed bed reactor, the catalyst has high raw material conversion rate, high product yield, long service life, is safe and environmentally friendly, and is easy for industrial production.
[0005] An object of the application is to provide a catalyst for preparing 1,1,1,2,3-pentafluoropropane by hydrogenation of 1,1,1,2,3-pentafluoropropene, the catalyst is composed of a carrier, an active component supported on the carrier and an auxiliary component; wherein the carrier is alumina, the active component is Cu, and the auxiliary component is Mo and Nb; the content of Cu is 3-27%, the content of Mo is 2-6%, the content of Nb is 2-6%, and the balance is the carrier, based on 100% of the weight of the catalyst.
[0006] Another object of the present application is to provide a preparation method of the aforementioned catalyst for preparing 1,1,1,2,3-pentafluoropropane by hydrogenation of 1,1,1,2,3-pentafluoropropene, which is prepared by a hydrolytic co-precipitation method, and specifically comprises the following steps:
[0007] (1) preparing an aqueous solution with a concentration of 0.08-0.48 mol / L of aluminum by using pseudoboehmite, to obtain a carrier solution, and starting stirring at a kettle temperature of 50-80℃;
[0008] (2) preparing an aqueous solution with a total concentration of 0.08-0.48 mol / L of metals by using precursor salts of Cu, Mo and Nb, to obtain a mixed metal solution;
[0009] (3) dropping the mixed metal solution and a first precipitant solution into the carrier solution by a peristaltic pump in a concurrent manner to obtain a mixed slurry, and stirring at a constant temperature for 3-6.5 h after the dropping is completed; the first precipitant is a water-soluble amide;
[0010] (4) dropping a second precipitant solution into the mixed slurry obtained in step (3) to control the pH of the mixed slurry to be 7.2-9.2, stirring at a constant temperature for 3-6.5 h after the dropping is completed, then stopping the stirring, aging in a glass kettle at a constant temperature for 12-24 h, filtering, washing the filter cake with deionized water until the pH of the filtrate is less than 7.2, drying to constant weight to obtain a catalyst precursor;
[0011] (5) tabletting the catalyst precursor by a tablet press, calcining, cooling to room temperature, and then reducing and activating to obtain the catalyst.
[0012] Preferably, the dropping speed of the mixed metal solution is 2.5-15 mL / min, and the dropping time of the mixed metal solution and the first precipitant solution is the same; the dropping speed of the second precipitant solution is 2.5-15 mL / min.
[0013] Preferably, the molar ratio of the first precipitant to the active component Cu is (0.6-5.8):1, and the mass concentration of the first precipitant solution and the second precipitant solution is 3-16%.
[0014] Preferably, the first precipitant is any one or two or more of urea, iminodiacetic acid diamide, carbonic acid diamide, N,N-dimethylformamide, N-methylacetamide, N,N-dimethylpropionamide, cyanoacetamide, propionamide, isobutyramide, formamide and N,N-dimethylglycine amide.
[0015] Preferably, the second precipitant is any one or two or more of sodium hydroxide, sodium carbonate, potassium hydroxide, potassium carbonate, lithium hydroxide, sodium bicarbonate, potassium bicarbonate and ammonium carbonate.
[0016] Preferably, the precursor salt of Cu is any one or more of copper nitrate, copper chloride, copper acetate, and basic copper carbonate; the precursor salt of Mo is any one or more of molybdenum chlorate, molybdenum nitrate, ammonium molybdate, and dinitrosodiaminomolybdenum; and the precursor salt of Nb is any one or more of niobium nitrate, niobium oxalate, niobium acetate, and di-niobium pentoxide.
[0017] Preferably, the reduction activation treatment specifically comprises: activating at 1-3℃ / min to 250-350℃ for 2-6h under a reducing gas atmosphere, the space velocity of the reducing gas being 100-500h -1 ; and the reducing gas being any one of hydrogen, hydrogen / argon mixed gas, and carbon monoxide.
[0018] Preferably, the drying conditions are drying at 70-120℃ for 12-36h; and the calcination conditions are calcination treatment at 300-500℃ for 8-12h.
[0019] Another object of the present application is to provide a method for preparing 1,1,1,2,3-pentafluoropropane by hydrogenation of 1,1,1,2,3-pentafluoropropene, which comprises the following steps: loading the aforementioned catalyst into a fixed bed reactor, dissolving 1,1,1,2,3-pentafluoropropene in a solvent to obtain a uniform transparent soluble solution, and passing in the solution and hydrogen, the reaction temperature being 55-80℃, and the reaction pressure being 0.1-0.5MPa; wherein the volume space velocity of the solution is 0.85-6.4h -1 , the molar ratio of hydrogen to 1,1,1,2,3-pentafluoropropene is (2-20):1, the solvent is methanol, N,N-dimethylformamide, isopropyl alcohol, γ-butyrolactone, 1,4-dioxane, or ethylene glycol dimethyl ether, and the mass concentration of 1,1,1,2,3-pentafluoropropene in the solution is 25-50%.
[0020] The excellent effects of the present application are as follows:
[0021] 1. The catalyst of the present application introduces the assistant components Mo and Nb, promotes the synergistic effect among the carrier, the active metal, and the assistant components, and significantly improves the catalytic performance of the catalyst.
[0022] 2. In the preparation of 1,1,1,2,3-pentafluoropropane, the method of the present application is simple to operate, easy to control, safe, and has higher stability of product quality; 3. Two kinds of precipitants are used in the preparation process of the catalyst, and the first amide precipitant is added in parallel flow with the metal precursor, the hydrolysis and precipitation rate is controlled, and the metal precursor is completely precipitated by using a stronger alkaline precipitant later, the process is simple, the prepared catalyst has good metal dispersity, and has excellent catalytic activity and 1,1,1,2,3-pentafluoropropane selectivity at low temperature.
[0023] 4. The fixed bed continuous catalytic reaction is suitable for a variety of solvent systems with different types and concentrations, and ensures that the conversion rate of 1,1,1,2,3-pentafluoropropene is more than 99%, and the selectivity of 1,1,1,2,3-pentafluoropropane is more than 99.5%. Embodiment
[0024] The raw materials involved in the embodiments of the application, unless otherwise specified, can be obtained from commercial sources or synthesized by using commercially available starting materials and reagents through conventional methods in the art.
[0025] Preparation of catalyst 1 (Cat. 1) in example 1
[0026] Cat. 1 is composed of a carrier alumina, an active component Cu supported on the carrier, and an auxiliary component Mo and Nb, wherein the content of Cu is 15%, the content of Mo is 4%, the content of Nb is 4%, and the content of alumina is 77% based on the weight of the catalyst. It is prepared by a hydrolysis co-precipitation method, which specifically includes the following steps:
[0027] (1) According to the content of alumina in the catalyst, pseudo-boehmite is weighed to prepare an aqueous solution with an aluminum concentration of 0.35 mol / L, obtaining a carrier solution, which is added to a 60℃ reaction kettle and stirred;
[0028] (2) According to the content of Cu, Mo and Nb in the catalyst, the corresponding precursor salts copper nitrate, ammonium molybdate and di-niobium pentoxide are weighed to prepare an aqueous solution with a total concentration of Cu, Mo and Nb of 0.35 mol / L, obtaining a mixed metal solution;
[0029] (3) According to the molar ratio of the first precipitant urea to Cu of 4:1, a urea solution with a concentration of 8wt% is prepared as the first precipitant solution; the mixed metal solution and the urea solution are added to the carrier solution in parallel flow, obtaining a mixed slurry; the dropping speed of the mixed metal solution is 6mL / min, and the dropping time of the mixed metal solution and the urea solution is the same, and after dropping, it is stirred at 60℃ for 4h;
[0030] (4) The second precipitant solution is added to the mixed slurry obtained in step (3) at a flow rate of 6mL / min, and the pH of the mixed slurry is controlled at 8.2, after dropping, it is stirred at 60℃ for 4h, then the stirring is stopped, and it is aged at constant temperature for 15h, then it is filtered, the filter residue is washed with deionized water until the pH of the filtrate is less than 7.2, and then it is dried in an oven at 100℃ for 20h, obtaining a catalyst precursor; the second precipitant solution is an ammonium carbonate solution with a concentration of 8wt%;
[0031] (5) The catalyst precursor was pressed into a tablet, calcined at 450°C for 10 h under air atmosphere, cooled to room temperature, and then reduced and activated at 300°C under hydrogen atmosphere at a temperature increasing rate of 2°C / min for 3.5 h, hydrogen space velocity 250 h"1. -1 The catalyst, denoted as Cat. 1, was obtained.
[0032] Preparation of Catalyst 2 (Cat. 2) of Example 2
[0033] Cat. 2 consisted of a carrier alumina, an active component Cu supported on the carrier, and an auxiliary component Mo and Nb, the catalyst having a weight of 100%, a Cu content of 3%, a Mo content of 4%, a Nb content of 4%, and alumina of 89%.
[0034] Cat. 2 was prepared according to the component contents in Cat. 2, with reference to the method in Example 1.
[0035] Preparation of Catalyst 3 (Cat. 3) of Example 3
[0036] Cat. 3 consisted of a carrier alumina, an active component Cu supported on the carrier, and an auxiliary component Mo and Nb, the catalyst having a weight of 100%, a Cu content of 27%, a Mo content of 4%, a Nb content of 4%, and alumina of 65%;
[0037] Cat. 3 was prepared according to the component contents in Cat. 3, with reference to the method in Example 1.
[0038] Preparation of Catalyst 4 (Cat. 4) of Example 4
[0039] Cat. 4 consisted of a carrier alumina, an active component Cu supported on the carrier, and an auxiliary component Mo and Nb, the catalyst having a weight of 100%, a Cu content of 15%, a Mo content of 2%, a Nb content of 4%, and alumina of 79%;
[0040] Cat. 4 was prepared according to the component contents in Cat. 4, with reference to the method in Example 1.
[0041] Preparation of Catalyst 5 (Cat. 5) of Example 5
[0042] Cat. 5 consisted of a carrier alumina, an active component Cu supported on the carrier, and an auxiliary component Mo and Nb, the catalyst having a weight of 100%, a Cu content of 15%, a Mo content of 2%, a Nb content of 6%, and alumina of 77%;
[0043] Cat. 5 was prepared according to the component contents in Cat. 5, with reference to the method in Example 1.
[0044] Example 6 Preparation of catalyst 6 (Cat. 6)
[0045] The precursor salt of the catalytically active metal Cu in Cat. 6 is basic copper carbonate, and the other steps are the same as in Example 1. The obtained catalyst is denoted as Cat. 6.
[0046] Example 7 Preparation of catalyst 7 (Cat. 7)
[0047] The precursor salt of the catalytic promoter component Mo in Cat. 7 is molybdenum nitrate, and the other steps are the same as in Example 1. The obtained catalyst is denoted as Cat. 7.
[0048] Example 8 Preparation of catalyst 8 (Cat. 8)
[0049] The first precipitant amide in Cat. 8 is formamide, and the other steps are the same as in Example 1. The obtained catalyst is denoted as Cat. 8.
[0050] Example 9 Preparation of catalyst 9 (Cat. 9)
[0051] Cat. 9 is composed of a carrier alumina, an active component Cu supported on the carrier, a promoter component Mo and Nb, and the content of Cu, Mo and Nb is 15%, 6% and 2% respectively, and the content of alumina is 77% in the catalyst with a weight of 100%;
[0052] It is prepared by a hydrolytic co-precipitation method, specifically comprising the following steps:
[0053] (1) According to the content of alumina in the catalyst, pseudo-boehmite is weighed to prepare an aqueous solution with an aluminum concentration of 0.08 mol / L to obtain a carrier solution, which is added to a reaction kettle at 50°C and stirring is started;
[0054] (2) According to the content of Cu, Mo and Nb in the catalyst, the corresponding precursor salts copper chloride, molybdate and niobium oxalate are weighed to prepare an aqueous solution with a total concentration of Cu, Mo and Nb of 0.08 mol / L to obtain a mixed metal solution;
[0055] (3) According to the molar ratio of the first precipitant to Cu of 5.8:1, a solution of di-carboxylic amide with a concentration of 3wt% is prepared as the first precipitant solution; the mixed metal solution and the first precipitant solution are added to the carrier solution in parallel flow to obtain a mixed slurry; the dropping speed of the mixed metal solution is 2.5 mL / min, and the dropping time of the mixed metal solution and the first precipitant solution is the same, and after the dropping is completed, constant temperature stirring is carried out at 50°C for 6.5h;
[0056] (4) a second precipitant solution was added dropwise into the mixed slurry obtained in step (3) at a flow rate of 8 mL / min, the pH of the mixed slurry was controlled at 7.2, after the dropwise addition was completed, constant temperature stirring was carried out at 50°C for 6.5 h, then the stirring was stopped, constant temperature aging was carried out for 24 h, filtration was carried out, the filter residue was washed with deionized water until the pH of the filtrate was less than 7.2, and drying was carried out in an oven at 70°C for 36 h to obtain a catalyst precursor; the second precipitant solution was a 3wt% sodium hydroxide solution;
[0057] (5) the catalyst precursor was tablet-pressed into a shape, calcination treatment was carried out at 300°C for 12 h in an air atmosphere, cooling was carried out to room temperature, then reduction activation treatment was carried out at a temperature rising rate of 1°C / min to 250°C for 6 h in a carbon monoxide atmosphere, and the carbon monoxide gas space velocity was 100h -1 , to obtain the catalyst, recorded as Cat.9.
[0058] Preparation of catalyst 10 (Cat.10) in example 10
[0059] Cat.10 is composed of a carrier alumina, an active component Cu supported on the carrier, and an auxiliary component Mo and Nb, wherein the content of Cu is 18%, the content of Mo is 6%, the content of Nb is 2%, and the content of alumina is 74% in the catalyst, with the weight being 100%.
[0060] It is prepared by a hydrolysis co-precipitation method, specifically including the following steps:
[0061] (1) according to the content of alumina in the catalyst, a pseudo-boehmite was weighed to prepare an aqueous solution with an aluminum concentration of 0.48 mol / L to obtain a carrier solution, which was added to a reaction kettle at 80°C, and stirring was started;
[0062] (2) according to the content of Cu, Mo and Nb in the catalyst, corresponding precursor salts copper acetate, dinitrosodiaminomolybdenum and niobium acetate were weighed to prepare an aqueous solution with a total concentration of Cu, Mo and Nb of 0.48 mol / L to obtain a mixed metal solution;
[0063] (3) an iminodiacetic acid diamide solution with a concentration of 16wt% was prepared according to a first precipitant to Cu molar ratio of 0.6:1; the mixed metal solution and the first precipitant solution were added dropwise into the carrier solution in parallel flow to obtain a mixed slurry; the dropwise addition speed of the mixed metal solution was 15 mL / min, and the dropwise addition time of the mixed metal solution and the first precipitant solution was the same, and after the dropwise addition was completed, constant temperature stirring was carried out at 80°C for 3 h;
[0064] (4) drop the second precipitant solution into the mixed slurry obtained in step (3) at a flow rate of 15 mL / min, control the pH of the mixed slurry to be 9.2, after the dropping is completed, stir at 80℃ for 3h, then stop stirring, constant temperature aging for 12h, filter, wash the filter residue with deionized water until the pH of the filtrate is less than 7.2, dry in an oven at 120℃ for 12h, to obtain a catalyst precursor; the second precipitant solution is a 16wt% sodium carbonate solution;
[0065] (5) tablet the catalyst precursor, calcine at 500℃ for 8h under air atmosphere, cool to room temperature, then reduce and activate at 350℃ for 2h under hydrogen and argon mixed gas atmosphere at a temperature rising rate of 3℃ / min, hydrogen space velocity is 500h -1 , to obtain the catalyst, recorded as Cat.10.
[0066] Preparation of Comparative Catalyst 1 (Dcat.1)
[0067] On the basis of Example 1, without Mo, and the others are the same as Example 1, recorded as Dcat.1.
[0068] Preparation of Comparative Catalyst 2 (Dcat.2)
[0069] On the basis of Example 1, without Nb, and the others are the same as Example 1, recorded as Dcat.2.
[0070] Application and performance detection of the catalyst
[0071] The catalyst prepared by the method of the present application is used to test the method of preparing 1,1,1,2,3-pentafluoropropane by hydrogenating 1,1,1,2,3-pentafluoropropene: the catalyst is loaded in a fixed bed reactor, 1,1,1,2,3-pentafluoropropene is dissolved in a solvent to obtain a uniform transparent soluble solution, the solution and hydrogen are introduced, the reaction temperature is 55-80℃, and the reaction pressure is 0.1-0.5MPa; wherein the volume space velocity of the solution is 0.85-6.4h -1 , the molar ratio of hydrogen to 1,1,1,2,3-pentafluoropropene is (2-20):1, the solvent is methanol, N,N-dimethylformamide, isopropanol, γ-butyrolactone, 1,4-dioxane or ethylene glycol dimethyl ether, and the mass concentration of 1,1,1,2,3-pentafluoropropene in the solution is 25-50%; the specific reaction conditions and reaction results are shown in Table 1
[0072] Table 1 Hydrogenation reaction conditions and results
[0073]
[0074] Note: The above evaluation results are the average results in each running time.
[0075] The foregoing is considered as illustrative only of the principles of the application. Further, since numerous modifications and changes will readily occur to those skilled in the art, it is not desired to limit the application to the exact construction and practice described. Accordingly, all such variations and modifications are intended to be included within the scope of the application as defined in the following claims and the equivalents thereof.
Claims
1. Use of a catalyst for the production of 1,1,1,2,3-pentafluoropropane by hydrogenation of 1,1,1,2,3-pentafluoropropene, characterized in that: The catalyst is composed of a carrier, an active component supported on the carrier and an auxiliary component; wherein the carrier is alumina, the active component is Cu, and the auxiliary component is Mo and Nb; the Cu content is 3-27%, the Mo content is 2-6%, the Nb content is 2-6%, and the balance is the carrier, based on the weight of the catalyst as 100%; The catalyst is prepared by a hydrolysis co-precipitation method, specifically including the following steps: (1) an aqueous solution with an aluminum concentration of 0.08-0.48 mol / L is prepared by using pseudo-boehmite as a raw material to obtain a carrier solution, and the carrier solution is stirred at a kettle temperature of 50-80℃; (2) precursor salts of Cu, Mo and Nb are weighed and an aqueous solution with a total metal concentration of 0.08-0.48 mol / L is prepared to obtain a mixed metal solution; (3) the mixed metal solution and a first precipitant solution are dropped into the carrier solution through a peristaltic pump in a concurrent manner to obtain a mixed slurry, and constant temperature stirring is performed for 3-6.5 h after the dropping is completed; the first precipitant is a water-soluble amide; (4) a second precipitant solution is dropped into the mixed slurry obtained in step (3), the pH of the mixed slurry is controlled to be 7.2-9.2, constant temperature stirring is performed for 3-6.5 h after the dropping is completed, then the stirring is stopped, constant temperature aging is performed in a glass kettle for 12-24 h, filtration is performed, the filter cake is washed with deionized water until the pH of the filtrate is less than 7.2, and drying is performed until the weight is constant to obtain a catalyst precursor; (5) the catalyst precursor is tabletted by a tablet press, calcination is performed, cooling to room temperature is performed, and then reduction activation treatment is performed to obtain the catalyst.
2. Use according to claim 1, characterized in that: The dropping speed of the mixed metal solution is 2.5-15 mL / min, and the dropping time of the mixed metal solution and the first precipitant solution is the same; the dropping speed of the second precipitant solution is 2.5-15 mL / min.
3. Use according to claim 2, characterized in that: The molar ratio of the first precipitant to the active component Cu is 0.6-5.8:1, and the mass concentration of the first precipitant solution and the second precipitant solution is 3-16%.
4. Use according to claim 1, characterized in that: The first precipitant is any one or two or more of a carbonic acid diamide, N,N-dimethylformamide, N-methylacetamide, cyanoacetamide, formamide and N,N-dimethylglycine amide.
5. Use according to claim 1, characterized in that: The second precipitant is any one or two or more of sodium hydroxide, sodium carbonate, potassium hydroxide, potassium carbonate, lithium hydroxide, sodium bicarbonate, potassium bicarbonate and ammonium carbonate.
6. Use according to claim 1, characterized in that: The precursor salt of Cu is any one or two or more of copper nitrate, copper chloride, copper acetate and basic copper carbonate; the precursor salt of Mo is one or two of molybdenum nitrate and ammonium molybdate; and the precursor salt of Nb is any one or two or more of niobium nitrate, niobium oxalate and niobium acetate.
7. The use according to claim 1, characterized in that: The reduction activation treatment is specifically: activating at 1-3 ℃ / min to 250-350 ℃ for 2-6 h under a reducing gas atmosphere, the space velocity of the reducing gas is 100-500 h -1 ; the reducing gas is any one of hydrogen, hydrogen / argon mixed gas, carbon monoxide.
8. Use according to claim 1, characterized in that: The drying condition is drying at 70-120℃ for 12-36 h; and the calcination condition is calcination treatment at 300-500℃ for 8-12 h.
9. The use according to claim 1, characterized in that, The method for preparing 1,1,1,2,3-pentafluoropropane by hydrogenating 1,1,1,2,3-pentafluoropropene comprises the following steps: loading a catalyst into a fixed bed reactor, dissolving 1,1,1,2,3-pentafluoropropene in a solvent to obtain a uniform and transparent soluble solution, and introducing the solution and hydrogen into the reactor, wherein the reaction temperature is 55-80 DEG C, the reaction pressure is 0.1-0.5 MPa, the volume space velocity of the solution is 0.85-6.4 h-1, the molar ratio of hydrogen to 1,1,1,2,3-pentafluoropropene is 2-20:1, the solvent is methanol, N,N-dimethylformamide, isopropyl alcohol, gamma-butyrolactone, 1,4-dioxane or ethylene glycol dimethyl ether, and the mass concentration of 1,1,1,2,3-pentafluoropropene in the solution is 25-50%. -1 The method for preparing 1,1,1,2,3-pentafluoropropane by hydrogenating 1,1,1,2,3-pentafluoropropene comprises the following steps: loading a catalyst into a fixed bed reactor, dissolving 1,1,1,2,3-pentafluoropropene in a solvent to obtain a uniform and transparent soluble solution, and introducing the solution and hydrogen into the reactor, wherein the reaction temperature is 55-80 DEG C, the reaction pressure is 0.1-0.5 MPa, the volume space velocity of the solution is 0.85-6.4 h-1, the molar ratio of hydrogen to 1,1,1,2,3-pentafluoropropene is 2-20:1, the solvent is methanol, N,N-dimethylformamide, isopropyl alcohol, gamma-butyrolactone, 1,4-dioxane or ethylene glycol dimethyl ether, and the mass concentration of 1,1,1,2,3-pentafluoropropene in the solution is 25-50%.
Citation Information
Patent Citations
Method for preparing 1,1,1,2,3,3-hexafluoropropane from 1,1,1,2,3,3-hexafluoropropylene and hydrogen gas
CN101148395A