Method for preparing 1, 5-pentanediol by catalyzing conversion of furfural
By using the hydrogenation catalyst composed of FE, CU, CO, and LA, the problem of unsatisfactory opening performance of precious metal catalysts when converting brachytal formation, realizing the effect of high-efficiency conversion to 1,5-pentaol, and reducing it. cost.
Patent Information
- Application Number
- CN202411492759.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-24
- Publication Date
- 2025-01-24
AI Technical Summary
In the prior art, when the noble metal catalyst converts furfural to 1,5-pentanediol, the ring opening performance is not ideal, and it is easy to generate the by-product tetrahydrofurfurfurol. The precious metal resources are rare and costly.
A hydrogenation catalyst including Fe, Cu, Co and La is used to improve the selectivity and yield of furfural into 1,5-pentanediol by adjusting the synergistic effect of metals.
It achieves efficient and highly selective conversion of furfural into 1,5-pentanediol, reduces the generation of by-products, and uses non-precious metal raw materials with low cost.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of biomass conversion, and in particular to a method for preparing 1,5-pentanediol by catalytic conversion of furfural. Background Art
[0002] The depletion of fossil fuels and petrochemicals has brought challenges of energy crisis and environmental pollution to mankind. For these reasons, biomass and its derivatives have received increasing attention in the production of renewable biofuels and value-added compounds. In terms of using biomass to replace fossil resources, the concept of "biomass-derived platform" has been proposed, and a series of biomass-derived chemicals have been listed as key intermediates. This type of biomass-derived chemicals contains a variety of cyclic ethers, such as furfural, 5-hydroxymethylfurfural, etc.
[0003] Furfural is usually synthesized from hemicellulose by hydrolysis and dehydration of xylose. Xylose is a hemicellulose-derived pentose found in agricultural wastes such as corn stover, corn cobs and peanut shells. Furfural as a raw material can be catalytically converted into a series of high value-added chemicals such as furfuryl alcohol (FOL), tetrahydrofurfuryl alcohol (THFOL), pentanediol (PeD), 2-methylfuran (MeF), 2-methyltetrahydrofuran (MTHF), cyclopentanone (CPO), etc. Among these products, 1,5-pentanediol is of great significance in the chemical industry. It can be used as a major component in the manufacture of polyester and polyurethane. At present, the industry mainly uses fossil fuels to synthesize 1,5-pentanediol, but due to the limited availability of C5 petroleum raw materials, it is not enough to meet production needs.
[0004] At present, there are few studies on the direct one-pot synthesis of 1,5-pentanediol from biomass-derived furfural. Some researchers have used precious metal catalysts such as Pt, Pd, Ir and Re to achieve the purpose of converting furfural into 1,5-pentanediol. Although the hydrogenation activity of precious metals is higher, their ring-opening performance is not ideal, which will promote the complete hydrogenation of furfural to form tetrahydrofurfuryl alcohol by-product. In addition, precious metals are a rare and expensive resource with a high cost of use. Summary of the invention
[0005] The purpose of the present invention is to provide a method for catalyzing the conversion of furfural to prepare 1,5-pentanediol, so as to solve the problems existing in the above-mentioned prior art. The hydrogenation catalyst of the present invention can catalyze the conversion of furfural to prepare 1,5-pentanediol with high selectivity.
[0006] To achieve the above-mentioned purpose, the present invention provides the following scheme: One of the technical schemes of the present invention: a hydrogenation catalyst, comprising the following raw materials, in mass percentage: Fe 0-1wt%, Cu 1-10wt%, Co20-40wt% and La 50-80wt%, wherein the content of Fe is not 0.
[0007] Furthermore, the hydrogenation catalyst comprises the following raw materials, in terms of mass percentage: Fe 0-1wt%, Cu 5wt%, Co 30wt% and La 64-65wt%, wherein the content of Fe is not zero.
[0008] Furthermore, the hydrogenation catalyst comprises the following raw materials, in terms of mass percentage: 0.2 wt% Fe, 5 wt% Cu, 30 wt% Co and 64.8 wt% La.
[0009] The second technical solution of the present invention is a method for preparing the above-mentioned hydrogenation catalyst, comprising the following steps:
[0010] Iron salt, copper salt, cobalt salt and lanthanum salt are added into water and dissolved, and then the pH is adjusted to alkaline, stirred evenly and subjected to aging reaction, and then filtered, washed, dried, ground, roasted and reduced to obtain the hydrogenation catalyst.
[0011] Furthermore, the pH is 10±0.1; the reagent used to adjust the pH is a mixed solution of sodium hydroxide and sodium carbonate, and the concentration of sodium hydroxide in the mixed solution is 0.5 mol / L and the concentration of sodium carbonate is 1 mol / L.
[0012] Furthermore, the calcination temperature is 400-500° C., and the time is 3-5 hours; the reduction is hydrogen reduction, and the temperature is 400-500° C., and the time is 3-5 hours.
[0013] Furthermore, the heating rate of the calcination is 5°C / min, the temperature is 450°C, and the time is 4h; the heating rate of the reduction is 10°C / min; the reduction is hydrogen reduction, the temperature is 450°C, and the time is 4h.
[0014] Furthermore, the iron salt is Fe(NO3)3, the copper salt is Cu(NO3)2, the cobalt salt is Co(NO3)2, and the lanthanum salt is La(NO3)3.
[0015] Furthermore, the washing is washing with water for multiple times until the pH is 7±0.1.
[0016] Furthermore, the stirring speed is 600r / min, and the time is 30min; the temperature of the aging reaction is 80°C, and the time is 24h; the temperature of the drying is 80°C, and the time is 24h; and the grinding is grinding to a particle size of 80-100 mesh.
[0017] The third technical solution of the present invention: an application of the above hydrogenation catalyst in catalyzing the conversion of furfural into 1,5-pentanediol.
[0018] The fourth technical solution of the present invention is a method for preparing 1,5-pentanediol by catalytic conversion of furfural, comprising the following steps: using furfural as a raw material and ethanol as a solvent, carrying out a hydrogenation ring-opening reaction under the action of the above-mentioned hydrogenation catalyst to obtain the 1,5-pentanediol.
[0019] Furthermore, the temperature of the hydrogenation ring-opening reaction is 140-170° C., and the time is 8-14 hours; and the hydrogen pressure in the reaction system during the hydrogenation ring-opening reaction is 1-5 MPa.
[0020] Furthermore, the temperature of the hydrogenation ring-opening reaction is 140-160° C., and the time is 10-14 hours; and the hydrogen pressure in the reaction system during the hydrogenation ring-opening reaction is 2-4 MPa.
[0021] The present invention discloses the following technical effects:
[0022] (1) The metals in the hydrogenation catalyst of the present invention have a synergistic effect, and can achieve efficient and highly selective conversion of furfural into 1,5-pentanediol.
[0023] (2) The present invention solves the problem of furfural generating byproducts such as tetrahydrofurfuryl alcohol by adding a trace amount of Fe to the hydrogenation catalyst, thereby greatly improving the selectivity and yield of 1,5-pentanediol.
[0024] (3) The hydrogenation catalyst of the present invention uses non-precious metal raw materials, the raw materials are easy and cheap to obtain, the process is simple, and it has good application prospects.
[0025] (4) The present invention can not only realize the high-value utilization of biomass resources, but also alleviate the increasingly scarce energy situation, while also reducing carbon emissions, which is in line with the current concept of sustainable development. DETAILED DESCRIPTION
[0026] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as limiting the present invention, but should be understood as a more detailed description of certain aspects, features, and embodiments of the present invention.
[0027] It should be understood that the terms described in the present invention are only for describing special embodiments and are not intended to limit the present invention. In addition, for the numerical range in the present invention, it should be understood that each intermediate value between the upper and lower limits of the scope is also specifically disclosed. Each smaller range between the intermediate value in any stated value or stated range and any other stated value or intermediate value in the described range is also included in the present invention. The upper and lower limits of these smaller ranges can be independently included or excluded in the scope.
[0028] Unless otherwise indicated, all technical and scientific terms used herein have the same meanings as those generally understood by those skilled in the art. Although the present invention describes only preferred methods and materials, any methods and materials similar or equivalent to those described herein may also be used in the implementation or testing of the present invention. All documents mentioned in this specification are incorporated by reference to disclose and describe the methods and / or materials associated with the documents. In the event of a conflict with any incorporated document, the content of this specification shall prevail.
[0029] It will be apparent to those skilled in the art that various modifications and variations may be made to the specific embodiments of the present invention description without departing from the scope or spirit of the present invention. Other embodiments derived from the present invention description will be apparent to those skilled in the art. The present application description and examples are exemplary only.
[0030] The words “include,” “including,” “have,” “contain,” etc. used in this document are open-ended terms, meaning including but not limited to.
[0031] The “parts” described in the following examples are all “parts by mass”.
[0032] All raw materials used in the examples of the present invention are commercially available.
[0033] Example 1
[0034] A method for preparing a hydrogenation catalyst:
[0035] (1) Copper nitrate, cobalt nitrate and lanthanum nitrate were weighed in a ratio of 5:30:65 among copper, cobalt and lanthanum, added into a beaker containing 75 mL of water, and stirred at 600 r / min for 30 min to obtain a mixed solution.
[0036] (2) A mixed solution containing 0.5 mol / L NaOH and 1 mol / L Na2CO3 was added dropwise into the beaker until the pH reached 10±0.1, and stirring was continued for 30 min (stirring speed was 600 r / min) to obtain a suspension.
[0037] (3) The suspension was aged at 80° C. for 24 h, then filtered, washed with ultrapure water for multiple times until the pH value was 7±0.1, and dried in a drying oven at 80° C. for 24 h to obtain a dried precipitate solid.
[0038] (4) The dried precipitate solid was ground in a mortar and sieved (100 mesh), and then calcined in a muffle furnace (heating rate of 5°C / min, temperature of 450°C, time of 4 h). After calcination, it was placed in a H2 tubular furnace and reduced in a hydrogen atmosphere (heating rate of 10°C / min, temperature of 450°C, time of 4 h) to obtain a hydrogenation catalyst, which was recorded as 5Cu-30Co-La catalyst.
[0039] Reaction evaluation: The 5Cu-30Co-La catalyst prepared in this example was added to a high-pressure reactor, and furfural and ethanol were added, mixed evenly, and the reactor was sealed; wherein, the amount of furfural added was 1 mmol, the amount of ethanol was 10 mL, and the amount of catalyst was 50 mg; then the air in the autoclave was replaced with hydrogen 5 times, and then 3 MPa of hydrogen was filled, and the temperature was increased to 150°C at a heating rate of 5°C / min, and the reaction was carried out for 12 hours. After the reaction was completed, it was cooled to room temperature, and the liquid and gas components were analyzed by gas chromatography and GC-MS, and it was found that the conversion rate of furfural was 100%, and the yield of 1,5-pentanediol was 76.6%. The reaction evaluation conditions and results are shown in Table 1.
[0040] Example 2
[0041] A method for preparing a hydrogenation catalyst:
[0042] (1) Iron nitrate, copper nitrate, cobalt nitrate and lanthanum nitrate were weighed in a ratio of 0.1:5:30:64.9 among iron, copper, cobalt and lanthanum, added into a beaker containing 75 mL of water, and stirred at 600 r / min for 30 min to obtain a mixed solution.
[0043] (2) A mixed solution containing 0.5 mol / L NaOH and 1 mol / L Na2CO3 was added dropwise into the beaker until the pH reached 10±0.1, and stirring was continued for 30 min (stirring speed was 600 r / min) to obtain a suspension.
[0044] (3) The suspension was aged at 80° C. for 24 h, then filtered, washed with ultrapure water for multiple times until the pH value was 7±0.1, and dried in a drying oven at 80° C. for 24 h to obtain a dried precipitate solid.
[0045] (4) The dried precipitate solid was ground in a mortar and sieved (100 mesh), and then calcined in a muffle furnace (heating rate of 5°C / min, temperature of 450°C, time of 4 h). After calcination, it was placed in a H2 tubular furnace and reduced in a hydrogen atmosphere (heating rate of 10°C / min, temperature of 450°C, time of 4 h) to obtain a hydrogenation catalyst, which was recorded as 0.1Fe-5Cu-30Co-La catalyst.
[0046] Reaction evaluation: The operating procedure of the reaction evaluation is consistent with that of Example 1. The reaction conditions and results are shown in Table 1.
[0047] Example 3
[0048] The same as Example 2, except that step (1) is specifically as follows: iron nitrate, copper nitrate, cobalt nitrate and lanthanum nitrate are weighed according to a mass ratio of iron, copper, cobalt and lanthanum of 0.2:5:30:64.8, added to a beaker containing 75 mL of water, and stirred at 600 r / min for 30 min to obtain a mixed solution; the prepared hydrogenation catalyst is recorded as 0.2Fe-5Cu-30Co-La catalyst.
[0049] Reaction evaluation: The operating procedure of the reaction evaluation is consistent with that of Example 1. The reaction conditions and results are shown in Table 1.
[0050] Example 4
[0051] The same as Example 2, except that step (1) is specifically as follows: iron nitrate, copper nitrate, cobalt nitrate and lanthanum nitrate are weighed according to the mass ratio of iron, copper, cobalt and lanthanum of 0.3:5:30:64.7, added to a beaker containing 75 mL of water, and stirred at 600 r / min for 30 min to obtain a mixed solution; the prepared hydrogenation catalyst is recorded as 0.3Fe-5Cu-30Co-La catalyst.
[0052] Reaction evaluation: The operating procedure of the reaction evaluation is consistent with that of Example 1. The reaction conditions and results are shown in Table 1.
[0053] Example 5
[0054] The same as Example 2, except that step (1) is specifically as follows: iron nitrate, copper nitrate, cobalt nitrate and lanthanum nitrate are weighed according to a mass ratio of iron, copper, cobalt and lanthanum of 0.5:3:30:64.5, added to a beaker containing 75 mL of water, and stirred at 600 r / min for 30 min to obtain a mixed solution; the prepared hydrogenation catalyst is recorded as 0.5Fe-5Cu-30Co-La catalyst.
[0055] Reaction evaluation: The operating procedure of the reaction evaluation is consistent with that of Example 1. The reaction conditions and results are shown in Table 1.
[0056] Example 6
[0057] The same as Example 2, except that step (1) is specifically as follows: iron nitrate, copper nitrate, cobalt nitrate and lanthanum nitrate are weighed in a ratio of 0.7:5:30:64.3 of the mass ratio of iron, copper, cobalt and lanthanum, added to a beaker containing 75 mL of water, and stirred at 600 r / min for 30 min to obtain a mixed solution; the prepared hydrogenation catalyst is recorded as 0.7Fe-5Cu-30Co-La catalyst.
[0058] Reaction evaluation: The operating procedure of the reaction evaluation is consistent with that of Example 1. The reaction conditions and results are shown in Table 1.
[0059] Example 7
[0060] The same as Example 2, except that step (1) is specifically as follows: iron nitrate, copper nitrate, cobalt nitrate and lanthanum nitrate are weighed in a ratio of 1:5:30:64 of the mass ratio of iron, copper, cobalt and lanthanum, added to a beaker containing 75 mL of water, and stirred at 600 r / min for 30 min to obtain a mixed solution; the prepared hydrogenation catalyst is recorded as 1Fe-5Cu-30Co-La catalyst.
[0061] Reaction evaluation: The operating procedure of the reaction evaluation is consistent with that of Example 1. The reaction conditions and results are shown in Table 1.
[0062] Example 8
[0063] The same as Example 3, except that step (1) is specifically as follows: the iron nitrate of the raw material is replaced with zinc sulfate, zinc sulfate, copper nitrate, cobalt nitrate and lanthanum nitrate are weighed in a ratio of 0.2:5:30:64.8 of zinc, copper, cobalt and lanthanum, and added to a beaker containing 75 mL of water, and stirred at 600 r / min for 30 min to obtain a mixed solution; the prepared hydrogenation catalyst is recorded as 0.2Zn-5Cu-30Co-La catalyst.
[0064] Reaction evaluation: The operating procedure of the reaction evaluation is consistent with that of Example 1. The reaction conditions and results are shown in Table 1.
[0065] Example 9
[0066] The same as Example 3, except that step (1) is specifically as follows: the copper nitrate of the raw material is replaced with tin sulfate, and iron nitrate, tin sulfate, cobalt nitrate and lanthanum nitrate are weighed in a ratio of 0.2:5:30:64.8 of the mass ratio of iron, tin, cobalt and lanthanum, and added to a beaker containing 75 mL of water, and stirred at 600 r / min for 30 min to obtain a mixed solution; the prepared hydrogenation catalyst is recorded as 0.2Fe-5Sn-30Co-La catalyst.
[0067] Reaction evaluation: The operating procedure of the reaction evaluation is consistent with that of Example 1. The reaction conditions and results are shown in Table 1.
[0068] Example 10
[0069] The same as Example 3, except that step (1) is specifically as follows: the copper nitrate of the raw material is replaced with nickel nitrate, and iron nitrate, nickel nitrate, cobalt nitrate and lanthanum nitrate are weighed in a ratio of 0.2:5:30:64.8 of the mass ratio of iron, nickel, cobalt and lanthanum, and added to a beaker containing 75 mL of water, and stirred at 600 r / min for 30 min to obtain a mixed solution; the prepared hydrogenation catalyst is recorded as 0.2Fe-5Ni-30Co-La catalyst.
[0070] Reaction evaluation: The operating procedure of the reaction evaluation is consistent with that of Example 1. The reaction conditions and results are shown in Table 1.
[0071] Embodiment 11
[0072] A method for preparing 1,5-pentanediol by catalytic conversion of furfural:
[0073] The 0.2Fe-5Cu-30Co-La catalyst prepared in Example 3 was added to a high-pressure reactor, and furfural and ethanol were added, mixed evenly, and the reactor was sealed; wherein the amount of furfural added was 1mmol, the amount of ethanol was 10mL, and the mass of the catalyst was 50mg; then the air in the autoclave was replaced with hydrogen 5 times, and then 1MPa of hydrogen was filled, and the temperature was increased to 150°C at a heating rate of 5°C / min, and the reaction was carried out for 12h. After the reaction was completed, it was cooled to room temperature, and the liquid and gas components were analyzed by gas chromatography and GC-MS, and it was found that the conversion rate of furfural was 100%, and the yield of 1,5-pentanediol was 70.3%. The reaction evaluation conditions and results are shown in Table 1.
[0074] Example 12
[0075] A method for preparing 1,5-pentanediol by catalytic conversion of furfural:
[0076] The 0.2Fe-5Cu-30Co-La catalyst prepared in Example 3 was added to a high-pressure reactor, and furfural and ethanol were added, mixed evenly, and the reactor was sealed; wherein the amount of furfural added was 1mmol, the amount of ethanol was 10mL, and the amount of catalyst was 50mg; then the air in the autoclave was replaced with hydrogen 5 times, and then 2MPa of hydrogen was filled, and the temperature was increased to 150°C at a heating rate of 5°C / min, and the reaction was carried out for 12h. After the reaction was completed, it was cooled to room temperature, and the liquid and gas components were analyzed by gas chromatography and GC-MS, and it was found that the conversion rate of furfural was 100%, and the yield of 1,5-pentanediol was 77.9%. The reaction evaluation conditions and results are shown in Table 1.
[0077] Embodiment 13
[0078] A method for preparing 1,5-pentanediol by catalytic conversion of furfural:
[0079] The 0.2Fe-5Cu-30Co-La catalyst prepared in Example 3 was added to a high-pressure reactor, and furfural and ethanol were added, mixed evenly, and the reactor was sealed; wherein, the amount of furfural added was 1mmol, the amount of ethanol was 10mL, and the amount of catalyst was 50mg; then the air in the autoclave was replaced with hydrogen 5 times, and then 4MPa of hydrogen was filled, and the temperature was increased to 150°C at a heating rate of 5°C / min, and the reaction was carried out for 12h. After the reaction was completed, it was cooled to room temperature, and the liquid and gas components were analyzed by gas chromatography and GC-MS, and it was found that the conversion rate of furfural was 100%, and the yield of 1,5-pentanediol was 91.1%. The reaction evaluation conditions and results are shown in Table 1.
[0080] Embodiment 14
[0081] A method for preparing 1,5-pentanediol by catalytic conversion of furfural:
[0082] The 0.2Fe-5Cu-30Co-La catalyst prepared in Example 3 was added to a high-pressure reactor, and furfural and ethanol were added, mixed evenly, and the reactor was sealed; wherein, the amount of furfural added was 1mmol, the amount of ethanol was 10mL, and the amount of catalyst was 50mg; then the air in the autoclave was replaced with hydrogen 5 times, and then 5MPa of hydrogen was filled, and the temperature was increased to 150°C at a heating rate of 5°C / min, and the reaction was carried out for 12h. After the reaction was completed, it was cooled to room temperature, and the liquid and gas components were analyzed by gas chromatography and GC-MS, and it was found that the conversion rate of furfural was 100%, and the yield of 1,5-pentanediol was 82.7%. The reaction evaluation conditions and results are shown in Table 1.
[0083] Embodiment 15
[0084] A method for preparing 1,5-pentanediol by catalytic conversion of furfural:
[0085] The 0.2Fe-5Cu-30Co-La catalyst prepared in Example 3 was added to a high-pressure reactor, and furfural and ethanol were added, mixed evenly, and the reactor was sealed; wherein, the amount of furfural added was 1mmol, the amount of ethanol was 10mL, and the amount of catalyst was 50mg; then the air in the autoclave was replaced with hydrogen 5 times, and then 3MPa of hydrogen was filled, and the temperature was increased to 140°C at a heating rate of 5°C / min, and the reaction was carried out for 12h. After the reaction was completed, it was cooled to room temperature, and the liquid and gas components were analyzed by gas chromatography and GC-MS, and it was found that the conversion rate of furfural was 100%, and the yield of 1,5-pentanediol was 85.4%. The reaction evaluation conditions and results are shown in Table 1.
[0086] Example 16
[0087] A method for preparing 1,5-pentanediol by catalytic conversion of furfural:
[0088] The 0.2Fe-5Cu-30Co-La catalyst prepared in Example 3 was added to a high-pressure reactor, and furfural and ethanol were added, mixed evenly, and the reactor was sealed; wherein, the amount of furfural added was 1mmol, the amount of ethanol was 10mL, and the amount of catalyst was 50mg; then the air in the autoclave was replaced with hydrogen 5 times, and then 3MPa of hydrogen was filled, and the temperature was increased to 160°C at a heating rate of 5°C / min, and the reaction was carried out for 12h. After the reaction was completed, it was cooled to room temperature, and the liquid and gas components were analyzed by gas chromatography and GC-MS, and it was found that the conversion rate of furfural was 100%, and the yield of 1,5-pentanediol was 91.1%. The reaction evaluation conditions and results are shown in Table 1.
[0089] Embodiment 17
[0090] A method for preparing 1,5-pentanediol by catalytic conversion of furfural:
[0091] The 0.2Fe-5Cu-30Co-La catalyst prepared in Example 3 was added to a high-pressure reactor, and furfural and ethanol were added, mixed evenly, and the reactor was sealed; wherein, the amount of furfural added was 1mmol, the amount of ethanol was 10mL, and the amount of catalyst was 50mg; then the air in the autoclave was replaced with hydrogen 5 times, and then 3MPa of hydrogen was filled, and the temperature was increased to 170°C at a heating rate of 5°C / min, and the reaction was carried out for 12h. After the reaction was completed, it was cooled to room temperature, and the liquid and gas components were analyzed by gas chromatography and GC-MS, and it was found that the conversion rate of furfural was 100%, and the yield of 1,5-pentanediol was 86.4%. The reaction evaluation conditions and results are shown in Table 1.
[0092] Embodiment 18
[0093] A method for preparing 1,5-pentanediol by catalytic conversion of furfural:
[0094] The 0.2Fe-5Cu-30Co-La catalyst prepared in Example 3 was added to a high-pressure reactor, and furfural and ethanol were added, mixed evenly, and the reactor was sealed; wherein, the amount of furfural added was 1mmol, the amount of ethanol was 10mL, and the amount of catalyst was 50mg; then the air in the autoclave was replaced with hydrogen 5 times, and then 3MPa of hydrogen was filled, and the temperature was increased to 150°C at a heating rate of 5°C / min, and the reaction was performed for 8h. After the reaction was completed, it was cooled to room temperature, and the liquid and gas components were analyzed by gas chromatography and GC-MS, and it was found that the conversion rate of furfural was 100%, and the yield of 1,5-pentanediol was 84.7%. The reaction evaluation conditions and results are shown in Table 1.
[0095] Embodiment 19
[0096] A method for preparing 1,5-pentanediol by catalytic conversion of furfural:
[0097] The 0.2Fe-5Cu-30Co-La catalyst prepared in Example 3 was added to a high-pressure reactor, and furfural and ethanol were added, mixed evenly, and the reactor was sealed; wherein, the amount of furfural added was 1mmol, the amount of ethanol was 10mL, and the amount of catalyst was 50mg; then the air in the autoclave was replaced with hydrogen 5 times, and then 3MPa of hydrogen was filled, and the temperature was increased to 150°C at a heating rate of 5°C / min, and the reaction was carried out for 10h. After the reaction was completed, it was cooled to room temperature, and the liquid and gas components were analyzed by gas chromatography and GC-MS, and it was found that the conversion rate of furfural was 100%, and the yield of 1,5-pentanediol was 92.5%. The reaction evaluation conditions and results are shown in Table 1.
[0098] Embodiment 20
[0099] A method for preparing 1,5-pentanediol by catalytic conversion of furfural:
[0100] The 0.2Fe-5Cu-30Co-La catalyst prepared in Example 3 was added to a high-pressure reactor, and furfural and ethanol were added, mixed evenly, and the reactor was sealed; wherein the amount of furfural added was 1mmol, the amount of ethanol was 10mL, and the amount of catalyst was 50mg; then the air in the autoclave was replaced with hydrogen 5 times, and then 3MPa of hydrogen was filled, and the temperature was increased to 150°C at a heating rate of 5°C / min, and the reaction was carried out for 14h. After the reaction was completed, it was cooled to room temperature, and the liquid and gas components were analyzed by gas chromatography and GC-MS, and it was found that the conversion rate of furfural was 100%, and the yield of 1,5-pentanediol was 94.2%. The reaction evaluation conditions and results are shown in Table 1.
[0101] Table 1 Reaction evaluation conditions and results
[0102]
[0103] The embodiments described above are only descriptions of the preferred modes of the present invention, and are not intended to limit the scope of the present invention. Without departing from the design spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by ordinary technicians in this field should all fall within the protection scope determined by the claims of the present invention.
Claims
1. A hydrogenation catalyst, characterized in that The raw materials include, by mass percentage, Fe 0-1wt%, Cu 1-10wt%, Co 20-40wt% and La 50-80wt%, wherein the content of Fe is not zero.
2. The hydrogenation catalyst according to claim 1, characterized in that The raw materials include, by mass percentage, 0-1 wt% Fe, 5 wt% Cu, 30 wt% Co and 64-65 wt% La, wherein the content of Fe is not zero.
3. A method for preparing the hydrogenation catalyst according to any one of claims 1 to 2, characterized in that: The following steps are involved: Iron salt, copper salt, cobalt salt and lanthanum salt are added into water and dissolved, and then the pH is adjusted to alkaline and an aging reaction is carried out, followed by drying, roasting and reduction to obtain the hydrogenation catalyst.
4. The preparation method according to claim 3, characterized in that: The pH is 10±0.1; the reagent used to adjust the pH is a mixed solution of sodium hydroxide and sodium carbonate, and the concentration of sodium hydroxide in the mixed solution is 0.5 mol / L and the concentration of sodium carbonate is 1 mol / L.
5. The preparation method according to claim 3, characterized in that: The calcination temperature is 400-500° C., and the time is 3-5 hours; the reduction is hydrogen reduction, and the temperature is 400-500° C., and the time is 3-5 hours.
6. Use of the hydrogenation catalyst according to any one of claims 1 to 2 in catalyzing the conversion of furfural into 1,5-pentanediol.
7. A method for preparing 1,5-pentanediol by catalytic conversion of furfural, characterized in that: The following steps are involved: Furfural is used as a raw material and ethanol is used as a solvent, and a hydrogenation ring-opening reaction is carried out under the action of the hydrogenation catalyst described in any one of claims 1 to 2 to obtain the 1,5-pentanediol.
8. The method according to claim 7, characterized in that The temperature of the hydrogenation ring-opening reaction is 140-170° C., and the time is 8-14 hours; the hydrogen pressure in the reaction system during the hydrogenation ring-opening reaction is 1-5 MPa.
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