A catalyst, its preparation and use

Abstract

The application provides a catalyst and a preparation method and application thereof, the catalyst comprises a mordenite molecular sieve and an active metal loaded in the mordenite molecular sieve, and the active metal is selected from copper and vanadium; wherein, the catalyst comprises, in terms of mass percentage, 5-15% of copper, 1-5% of vanadium, and the balance of the mordenite molecular sieve. The application limits the composition of the catalyst, that is, the catalyst contains 5-15% of copper in terms of mass percentage, 1-5% of vanadium in terms of mass percentage, and the balance of the mordenite (MOR) molecular sieve, the catalyst can convert furfural into 1,5-pentanediol in one step, no solvent is needed in the reaction process, the use and recovery cost of the solvent are saved, less waste is produced, the advantages of environmental protection and low cost are achieved, and the selectivity of the prepared 1,5-pentanediol is relatively high.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of chemical synthesis, and particularly relates to a catalyst, a preparation method and application thereof. BACKGROUND

[0002] 1,5-pentanediol is an important chemical intermediate, which is widely used in the manufacture of polyurethane, polyester, plasticizer, inkjet ink, ink, paint or perfume products. It can also be used as a cutting oil, special detergent, solvent for latex paint, solvent or wetting agent for ink.

[0003] In the prior art, 1,5-pentanediol is prepared by catalytic hydrogenation of tetrahydrofurfural or oxidation of cyclopentadiene in a solvent environment, and then catalytic hydrogenation is performed. This method requires the use of a large amount of organic solvent, generates more waste, has a high cost and low reaction selectivity. Therefore, it is an urgent problem to be solved to develop a preparation method of 1,5-pentanediol without using a solvent, generating less waste, having a low cost and high reaction selectivity. SUMMARY

[0004] The main purpose of the present application is to provide a catalyst, a preparation method and application thereof, which can solve the problems of using a large amount of organic solvent in the preparation process of 1,5-pentanediol, generating more waste, having a high cost and low reaction selectivity.

[0005] The present application provides a catalyst, which comprises mordenite molecular sieve and active metal loaded in the mordenite molecular sieve, and the active metal is selected from copper and vanadium.

[0006] The catalyst comprises copper 5-15%, vanadium 1-5% and the balance of mordenite molecular sieve in terms of mass percentage.

[0007] The specific surface area of the catalyst is 200-400 m 2 / g, and the total pore volume is 0.1-0.2 mL / g.

[0008] The silicon-aluminum ratio of the mordenite molecular sieve in the catalyst is 30:1.

[0009] The catalyst is prepared by a method comprising the following process:

[0010] The mordenite molecular sieve is subjected to equal-volume impregnation treatment by using an aqueous solution comprising a copper source and a vanadium source, and the impregnation system is subjected to post-treatment including filtration, washing and calcination to obtain the catalyst.

[0011] The application further provides a preparation method of the catalyst, comprising the following steps: performing equal-volume impregnation treatment on the mordenite molecular sieve by using an aqueous solution comprising a copper source and a vanadium source, and performing post-treatment, including filtration, washing and calcination, on the impregnation system to obtain the catalyst.

[0012] The preparation method of the catalyst as described above, wherein the equal-volume impregnation treatment is performed under ultrasonic waves.

[0013] The preparation method of the catalyst as described above, wherein the calcination temperature is 500-600 DEG C, and the calcination time is 4-6 h.

[0014] The application further provides a preparation method of 1,5-pentanediol, which is obtained by using the above-mentioned catalyst to catalyze furfural.

[0015] The preparation method of 1,5-pentanediol as described above, comprising the following steps:

[0016] 1) performing activation treatment on the catalyst by using hydrogen to obtain an activated catalyst;

[0017] 2) passing hydrogen and furfural into a reactor in which the activated catalyst is fixed to perform gas-solid contact reaction under the conditions that the temperature is 160-200 DEG C and the pressure is 2-3 MPa, so as to obtain the 1,5-pentanediol.

[0018] The preparation method of 1,5-pentanediol as described above, wherein the reaction space velocity of the gas-solid contact reaction is 10-25 h-1. -1 .

[0019] The application provides a catalyst, and defines the composition of the catalyst, i.e. the catalyst comprises copper with a mass percentage of 5%-15%, vanadium with a mass percentage of 1%-5%, and the balance is mordenite (MOR) molecular sieve. The catalyst can convert furfural into 1,5-pentanediol in one step, and no solvent is needed in the reaction process, thereby saving the use and recovery cost of the solvent, producing less waste, and having the advantages of environmental protection and low cost, and the prepared 1,5-pentanediol has high selectivity. DETAILED DESCRIPTION

[0020] To make the objectives, technical solutions and advantages of the present application clearer, the following will combine the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are some embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all the other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the present application.

[0021] The present application provides a kind of catalyst, including mordenite (MOR) molecular sieve and active metal loaded in mordenite (MOR) molecular sieve, active metal is selected from copper and vanadium;

[0022] Wherein, the catalyst includes copper 5%-15%, vanadium 1%-5% by mass percentage, and the balance is mordenite (MOR) molecular sieve.

[0023] Molecular sieve is a kind of crystal material with regular microporous structure (pore size less than 2 nanometers), and there are adjustable acid and redox active sites in the channel, which makes molecular sieve a widely used catalytic material in modern industrial catalysis. Compared with other supported metal catalysts, molecular sieve supported metal catalyst has smaller metal size and ultra-high thermal stability, and also shows excellent catalytic performance in catalytic reaction, and has been widely used in many important industrial catalytic processes in recent years.

[0024] It can be understood that mordenite (MOR) is one of molecular sieves, which has excellent heat resistance, acid resistance and water vapor resistance, and can be used as a catalyst for some chemical reactions. Due to the existence of certain acid centers on the outer surface of the molecular sieve, the target product diffusing out of the molecular sieve channel may undergo isomerization reaction on the outer surface of the molecular sieve, reducing the selectivity of the target product. To solve this problem, the present application provides a kind of catalyst, including mordenite (MOR) molecular sieve and active metal loaded in mordenite (MOR) molecular sieve, active metal is selected from copper and vanadium.

[0025] In one embodiment, the catalyst includes copper 5%-15%, vanadium 1%-5% by mass percentage, and the balance is mordenite molecular sieve. The catalyst prepared by the method has double active centers, copper as the active center of hydrogenation reaction, catalyzing selective hydrogenation of furfural, vanadium as the active center of catalytic carbon-oxygen bond cleavage, realizing synergistic catalysis of selective hydrogenation and bond cleavage ring-opening reaction, and catalyzing furfural to prepare 1,5-pentanediol in one step. Therefore, when the mass percentage of copper in the catalyst is 5%-15%, the mass percentage of vanadium is 1%-5%, and the balance is mordenite molecular sieve, the reaction process of catalyzing furfural to convert into 1,5-pentanediol does not need to use organic solvent, and the selectivity of 1,5-pentanediol is improved. When the mass percentage of copper in the catalyst is not within 5%-15%, and / or the mass percentage of vanadium is not within 1%-5%, the catalyst cannot play such a role, and thus cannot catalyze furfural to convert into 1,5-pentanediol or the selectivity of furfural to convert into 1,5-pentanediol is low.

[0026] The catalyst in the embodiment contains 5-15% of copper by mass, 1-5% of vanadium by mass, and the balance of mordenite (MOR) molecular sieve, can catalyze the selective hydrogenation and ring-opening reaction of the carbon-oxygen bond of furfural to generate 1,5-pentanediol, so that the reaction process does not need to use a solvent, saves the use and recovery cost of the solvent, produces less waste, has the advantages of environmental protection and low cost, and the selectivity of the prepared 1,5-pentanediol is high.

[0027] In some embodiments of the present application, the specific surface area of the catalyst is 200-400 m 2 / g, and the total pore volume is 0.1-0.2 mL / g.

[0028] It can be understood that the specific surface area of the catalyst refers to the surface area per unit weight of the catalyst, and the total pore volume of the catalyst refers to the total volume of all micropores per unit weight of the catalyst. In the embodiment, the specific surface area of the catalyst is controlled to be 200-400 m 2 / g, and the total pore volume is 0.1-0.2 mL / g.

[0029] If the specific surface area of the catalyst is too small, the contact area between the reactant furfural and the catalyst is too small, the catalyst activity is low, and the catalytic reaction activity is low. If the specific surface area of the catalyst is too large, the contact area between the catalyst and the reactant furfural is large, and the catalyst activity is high, but if the specific surface area of the catalyst is too large, the micropores in the catalyst are too small, which hinders the diffusion of the reactant furfural and affects the catalytic reaction. If the total pore volume of the catalyst is too small, the reactant furfural may not be able to fully diffuse and adsorb to the surface of the catalyst, resulting in incomplete reaction of furfural or decreased selectivity of 1,5-pentanediol. If the total pore volume of the catalyst is too large, although the reactant furfural can fully diffuse and adsorb to the surface of the catalyst, the mechanical strength and thermal stability of the catalyst will decrease, affecting the service life of the catalyst. Therefore, in the embodiment, the specific surface area of the catalyst is controlled to be 200-400 m 2 / g, and the total pore volume is 0.1-0.2 mL / g, which is within a suitable range.

[0030] In the embodiment, the specific surface area of the catalyst is controlled to be 200-400 m 2 / g, and the total pore volume is 0.1-0.2 mL / g, which is within a suitable range, so that the catalyst has high reaction activity, and the conversion rate and selectivity of furfural to 1,5-pentanediol are improved.

[0031] In some embodiments of the present application, the silicon-aluminum ratio of the mordenite (MOR) molecular sieve is 30:1.

[0032] It can be understood that the molecular sieve is a crystalline silicate or aluminosilicate formed by connecting silicon-oxygen tetrahedrons or aluminum-oxygen tetrahedrons through oxygen bridges. The molecular sieve is a silico-aluminic compound with a cubic lattice. The molecular sieve has a uniform microporous structure, the pore diameter of which is uniform, the pores can adsorb molecules smaller than the pore diameter into the pore cavity, and has a preferential adsorption capacity for polar molecules and unsaturated molecules, so that molecules with different polarities, different saturation degrees, different molecular sizes and different boiling points can be separated, that is, the molecular sieve has the function of "sifting" molecules, so it is called molecular sieve. The molecular sieve has the advantages of strong adsorption capacity and strong thermal stability, which are not possessed by other adsorbents, so that the molecular sieve has been widely used.

[0033] In an embodiment, the molar ratio of silicon to aluminum of the mordenite (MOR) molecular sieve is 30:1, and the mass percentage of copper is 5%-15% and the mass percentage of vanadium is 1%-5%, which are used as active metals, and the mordenite (MOR) molecular sieve is used as a catalyst for the conversion of furfural to 1,5-pentanediol. The catalytic activity of the catalyst can be improved, and the selectivity of 1,5-pentanediol can be improved. This is because when the molar ratio of silicon to aluminum of the mordenite (MOR) molecular sieve is 30:1, there is sufficient silicon to form the framework structure of the zeolite, which ensures the structural stability of the zeolite and prolongs the service life of the catalyst. In addition, the appropriate molar ratio of silicon to aluminum makes the acidity of the molecular sieve appropriate. The appropriate mass percentage of copper and vanadium can improve the catalytic performance of the mordenite (MOR) molecular sieve catalyst for the conversion of furfural to 1,5-pentanediol.

[0034] In the embodiment, the molar ratio of silicon to aluminum of the mordenite (MOR) molecular sieve is 30:1, which can make the molecular sieve have a certain acidity. The active metals copper and vanadium are used, and the mass percentage of copper is 5%-15% and the mass percentage of vanadium is 1%-5%. When the mordenite (MOR) molecular sieve is used as a catalyst for the conversion of furfural to 1,5-pentanediol, the catalytic performance of the catalyst can be improved, and the conversion of furfural to 1,5-pentanediol can be promoted.

[0035] In some embodiments of the present application, the catalyst is prepared by a method comprising the following steps:

[0036] The mordenite (MOR) molecular sieve is subjected to equal-volume impregnation treatment using an aqueous solution containing a copper source and a vanadium source. The impregnation system is subjected to post-treatment including filtration, washing and calcination to obtain the catalyst.

[0037] Alternatively, the copper source can be a copper salt, preferably copper nitrate. The vanadium source can be a vanadium salt, preferably vanadyl sulfate.

[0038] It can be understood that the impregnation method is a conventional method for producing catalysts, which puts a carrier with a porous structure into a solution containing active components, under the action of capillary force, the solution containing active components is absorbed into the micropores of the carrier from the surface, the active components diffuse to the inner wall of the micropores, and then are adsorbed by the active sites on the surface of the carrier to load the active components onto the catalyst carrier. At present, the most commonly used impregnation methods for catalyst production mainly include various methods such as excess impregnation method, equal volume impregnation method, multiple impregnation method, etc. In the present embodiment, the equal volume impregnation method is adopted. The equal volume impregnation is that the volume of the carrier molecular sieve and the volume of the solution containing active components, i.e. the impregnation solution, are consistent, the impregnation solution can completely enter the pores of the carrier molecular sieve, and the loading amount of the active components, i.e. the loading amount of the active metal copper, can be conveniently controlled to be 5%-15% by mass percentage, and the loading amount of the metal vanadium can be conveniently controlled to be 1%-5% by mass percentage. The carrier is treated by the impregnation method, which has high efficiency and relatively low cost.

[0039] In one embodiment, a water solution containing a copper source and a vanadium source is used for equal volume impregnation treatment of a mordenite (MOR) molecular sieve, to obtain an impregnation system, and the impregnation system is subjected to post-treatment including filtration, washing and calcination, to obtain a mordenite (MOR) molecular sieve catalyst loaded with 5%-15% by mass percentage of copper and 1%-5% by mass percentage of vanadium. The water solution containing the copper source and the vanadium source can be obtained by dissolving the copper source copper nitrate and the vanadium source vanadyl sulfate in water. Then, an equal volume of the mordenite (MOR) molecular sieve is added to the above water solution for impregnation treatment, so that copper ions and vanadium ions are adsorbed onto the mordenite (MOR) molecular sieve, to obtain the impregnation system, and then the impregnation system is subjected to post-treatment, to obtain the mordenite (MOR) molecular sieve catalyst loaded with the active metal copper and vanadium. The post-treatment includes filtration, washing and calcination. The purpose of filtration is to remove the excess water solution containing copper nitrate and vanadyl sulfate. The purpose of washing is to remove the copper nitrate and vanadyl sulfate which are not adsorbed into the pores of the mordenite (MOR) molecular sieve, and the nitrate and sulfate radicals. Optionally, a solvent is used for washing, for example, water can be used for washing. The calcination treatment can be performed in a muffle furnace, to remove the volatile components in the mordenite (MOR) molecular sieve carrier, to form a stable structure, so that the molecular sieve carrier obtains a certain crystal form, grain size and pore structure, i.e. specific surface area, to obtain the mordenite (MOR) molecular sieve catalyst loaded with the active metal copper and vanadium, wherein the mass percentage of copper is 5%-15%, and the mass percentage of vanadium is 1%-5%.

[0040] Optionally, after the washing treatment, a drying treatment is performed first, for example, drying treatment is performed in an oven at 100-120°C, and then the calcination treatment is performed.

[0041] The preparation method of the catalyst in the embodiment directly performs impregnation treatment on the mordenite (MOR) molecular sieve, omits the synthesis step of the molecular sieve, is simple and easy to implement, and is convenient for industrial scale production.

[0042] The application further provides a preparation method of a catalyst, comprising the following steps: performing isometric volume impregnation treatment on a mordenite (MOR) molecular sieve by using an aqueous solution containing a copper source and a vanadium source, and performing post-treatment, including filtration, washing and calcination, on the impregnation system to obtain the catalyst.

[0043] In one embodiment, the preparation method of the catalyst is as follows: dissolving a copper source, such as copper nitrate, and a vanadium source, such as vanadyl sulfate, in water to prepare an aqueous solution containing copper nitrate and vanadyl sulfate, then adding an isometric volume of mordenite (MOR) molecular sieve into the aqueous solution to perform impregnation treatment, so that copper ions and vanadium ions are adsorbed onto the mordenite (MOR) molecular sieve to obtain an impregnation system, and then performing post-treatment, i.e., filtration, washing and calcination, on the impregnation system to obtain a mordenite (MOR) molecular sieve catalyst loaded with active metals copper and vanadium, wherein the loading amount of the metal copper is 5%-15% by mass percentage, and the loading amount of the metal vanadium is 1%-5% by mass percentage.

[0044] Optionally, the drying treatment can be performed before the calcination treatment after the washing treatment.

[0045] The preparation method of the catalyst in the embodiment directly performs impregnation treatment on the mordenite (MOR) molecular sieve, omits the synthesis step of the molecular sieve, is simple and easy to implement, and is convenient for industrial scale production.

[0046] In some embodiments of the application, the isometric volume impregnation treatment is performed under ultrasonic waves.

[0047] Optionally, the isometric volume impregnation treatment can be performed under ultrasonic waves, so that the active components, i.e., the metals copper and vanadium, are uniformly dispersed and loaded onto the carrier mordenite (MOR) molecular sieve, and at the same time, the capillary resistance is overcome to enter the micropores of the mordenite (MOR) molecular sieve carrier.

[0048] The isometric volume impregnation treatment performed under ultrasonic waves in the embodiment can make the active metals copper and vanadium fully contact with the mordenite (MOR) molecular sieve, and the contact is relatively uniform, and this method is simple to operate and can improve the efficiency of the impregnation treatment.

[0049] In some embodiments of the application, the calcination temperature is 500-600 ℃, and the calcination time is 4-6 h.

[0050] In one embodiment, the impregnation system is subjected to the calcination treatment after the washing treatment, the calcination temperature is 500-600 ℃, and the calcination time is 4-6 h.

[0051] Optionally, the product after washing is subjected to a calcination treatment for removing the volatile components in the mordenite (MOR) molecular sieve carrier to form a stable structure. The calcination treatment can be performed in a muffle furnace, and the temperature of the muffle furnace can be set to 500-600 DEG C, preferably, the temperature of the muffle furnace can be set to 530 DEG C. If the temperature of the muffle furnace is too low, the calcination treatment is not complete, i.e., the volatile components are not completely volatilized, and the time for use is relatively long; if the temperature of the muffle furnace is too high, some substances can be decomposed, which affects the structure of the catalyst obtained by the calcination treatment.

[0052] Optionally, the time for the calcination treatment of the product after washing in the muffle furnace is 4-6 h, preferably, the calcination treatment time is 5 h. If the calcination time is too short, the volatile components are not completely volatilized; if the calcination time is too long, time is wasted, and the efficiency is relatively low.

[0053] In the embodiment, the calcination temperature is controlled to be 500-600 DEG C, and the calcination time is controlled to be 4-6 h, so that the efficiency of volatilization of the volatile components is relatively high, the volatilization of the volatile components is more complete, and time is not wasted, and the efficiency is not low.

[0054] The application further provides a preparation method of 1,5-pentanediol, which is obtained by using the above catalyst to catalyze furfural.

[0055] In one embodiment, the mordenite (MOR) molecular sieve loaded with active copper and vanadium obtained by the above preparation method is used as a catalyst to catalyze furfural to obtain 1,5-pentanediol, and the loading amount of the copper is 5%-15% by mass percentage, and the loading amount of the vanadium is 1%-5% by mass percentage, so that the preparation method of 1,5-pentanediol is simple and easy to implement.

[0056] In some embodiments of the application, the preparation method of 1,5-pentanediol comprises the following steps:

[0057] 1) activating the catalyst by using hydrogen to obtain an activated catalyst;

[0058] 2) passing hydrogen and furfural into a reactor in which the activated catalyst is fixed to perform a gas-solid contact reaction at a temperature of 160-200 DEG C and a pressure of 2-3 MPa, so as to obtain 1,5-pentanediol.

[0059] In one embodiment, the copper and vanadium loaded mordenite (MOR) molecular sieve is first activated by hydrogen to obtain an activated catalyst; then the activated catalyst is fixed in a reactor, hydrogen and furfural are introduced into the reactor with the activated catalyst fixed therein to perform a gas-solid contact reaction under the conditions of a temperature of 160-200°C and a pressure of 2-3 MPa, and furfural is converted into 1,5-pentanediol under the catalysis of the catalyst.

[0060] It can be understood that the catalyst needs to be activated after being prepared, so that the inactive catalyst is converted into an activated catalyst. The purpose of activation is to form active sites required for catalytic reaction on the catalyst, especially on the surface of the catalyst. In this embodiment, the catalyst is activated by hydrogen to obtain an activated catalyst.

[0061] Furfural is in a liquid state before being introduced into the reactor for reaction. The liquid furfural is first gasified into a gaseous state in a gasification chamber, and then introduced into the reactor with hydrogen for a gas-solid contact reaction to obtain 1,5-pentanediol. When the temperature of the reactor is controlled to be 160-200°C and the pressure is controlled to be 2-3 MPa, the furfural and hydrogen in the reactor can be kept in a gaseous state. Alternatively, an inert gas, for example, nitrogen, is introduced into the reactor before the hydrogen and furfural gas are introduced into the reactor with the activated catalyst fixed therein for a gas-solid contact reaction, so as to replace the oxygen and carbon dioxide and other gases in the reactor, so that there is no other gas in the reactor that affects the subsequent gas-solid contact reaction.

[0062] In this embodiment, the mordenite (MOR) molecular sieve loaded with active metals copper and vanadium is used as a catalyst to catalyze the one-step conversion of furfural into 1,5-pentanediol. In this reaction process, no solvent is used, the use and recovery costs of the solvent are saved, the generation of three wastes is less, and the process has the advantages of environmental protection and low cost. In addition, the selectivity of the obtained 1,5-pentanediol is high, the raw material furfural is continuously pumped by a metering pump, and hydrogen is continuously introduced into the system, so that a continuous reaction is realized, and the process has a good application prospect.

[0063] In some embodiments of the present application, the reaction space velocity of the gas-solid contact reaction is 10-25h -1 .

[0064] It can be understood that the space velocity refers to the volume of gas passing through 1 m 3 of catalyst per unit time. In the gas-solid contact reaction, the reciprocal of the reaction space velocity is the residence time of the gas in the catalyst layer. In this embodiment, the reaction space velocity of the gas-solid contact reaction is controlled to be 10-25h -1 , which is within a suitable range.

[0065] A higher space velocity results in a shorter contact time between furfural gas and hydrogen and the mordenite molecular sieve catalyst, which affects the selectivity of furfural to 1,5-pentanediol. Conversely, a lower space velocity results in a longer contact time between furfural gas and hydrogen and the mordenite molecular sieve catalyst, which is more conducive to the conversion of furfural to 1,5-pentanediol. However, if the space velocity is too low, the contact time between furfural gas and hydrogen and the mordenite molecular sieve catalyst may be too long, which may lead to a decrease in the reaction depth and consequently a decrease in the selectivity of the final 1,5-pentanediol.

[0066] In this embodiment, the reaction space velocity of the gas-solid contact reaction is controlled to be 10-25 h. -1 Within a suitable range, the selectivity for converting furfural to 1,5-pentanediol can be improved.

[0067] The technical solution of the present invention will be further described below with reference to specific embodiments.

[0068] Example 1

[0069] The preparation method of 1,5-pentanediol in this embodiment includes the following steps:

[0070] 1) Dissolve 22.16g Cu(NO3)2·3H2O and 4.66g VOSO4 in 100g of water and stir until completely dissolved;

[0071] 2) Add 58.3g of mordenite (silicon-to-aluminum ratio of 30) to the above solution and ultrasonically impregnate for 1 hour;

[0072] 3) Filter, wash, dry at 120℃, and calcine at 600℃ for 5h to obtain a mordenite catalyst with Cu10%V2.5% / MOR supported on active components Cu and V (the metal content in the catalyst is calculated based on the amount of raw materials added).

[0073] 4) The above Cu 10% V 2.5% / MOR catalyst, sieved through a 20-mesh sieve, has a surface area of ​​200 m². 2 / g, with a total pore volume of 0.1mL / g, is used in the catalytic reaction of furfural to prepare 1,5-pentanediol. 1g of sieved Cu10%V2.5% / MOR catalyst is packed into a fixed-bed reactor, and hydrogen is introduced to activate the catalyst to obtain the activated catalyst.

[0074] 5) Then, nitrogen gas is introduced into the fixed-bed reactor to fully displace the gas in the fixed-bed reactor. The temperature of the fixed-bed reactor is adjusted to 200℃ and the pressure to 3MPa. Then, furfural is added using a metering pump at a flow rate of 0.1mL / min, and hydrogen gas is introduced at a flow rate of 10mL / min. The reaction space velocity is controlled at 15h. -1The conversion rate of furfural is 72.4%, and the selectivity of 1,5-pentanediol is 89.7%, as shown in Table 1.

[0075] Example 2-26

[0076] Example 2-26 has the same preparation method of 1,5-pentanediol as Example 1, except that the parameters are different, and the specific parameters are shown in Table 1.

[0077] Comparative Example 1-6

[0078] Comparative Example 1-6 has the same preparation method of 1,5-pentanediol as Example 1, except that the loading amount of metal is different, and the specific parameters are shown in Table 1.

[0079] Table 1

[0080]

[0081]

[0082] As can be seen from Table 1, compared with the comparative examples, the catalyst provided by the present application can catalyze furfural to prepare 1,5-pentanediol, and no solvent is needed in the reaction process, which saves the use and recovery cost of the solvent, produces less waste, has the advantages of environmental protection and low cost, and the selectivity of the prepared 1,5-pentanediol is high, realizes continuous reaction, and has good application prospect.

[0083] As can be seen from the comparison of Example 1-2 and Comparative Example 1-6, the copper-vanadium modified mordenite molecular sieve catalyst provided by the present application can catalyze furfural to convert into 1,5-pentanediol, and the selectivity of the prepared 1,5-pentanediol is high.

[0084] Finally, it should be noted that: the above examples are only used to illustrate the technical solutions of the present application, and not to limit them; although the present application has been described in detail with reference to the foregoing examples, those skilled in the art should understand that: it can still modify the technical solutions recorded in the foregoing examples, or make equivalent replacement for part or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A method for preparing 1,5-pentanediol, characterized in that, Furfural is obtained by catalysis using a catalyst; the catalyst comprises a mordenite molecular sieve and an active metal supported on the mordenite molecular sieve, wherein the active metal is copper and vanadium; wherein the catalyst comprises, by mass percentage: 5%-15% copper, 1%-5% vanadium, and the balance being mordenite molecular sieve. The preparation method includes the following steps: 1) The catalyst is activated using hydrogen gas to obtain an activated catalyst; 2) At a temperature of 160-200℃ and a pressure of 2-3MPa, hydrogen and furfural are introduced into a reactor with the activated catalyst fixed to carry out a gas-solid contact reaction to obtain the 1,5-pentanediol. The catalyst has a specific surface area of ​​200-400 m². 2 / g, with a total pore volume of 0.1-0.2 mL / g.

2. The method for preparing 1,5-pentanediol according to claim 1, characterized in that, The reaction space velocity of the gas-solid contact reaction is 10-25 h⁻¹. -1 .

3. The method for preparing 1,5-pentanediol according to claim 1, characterized in that, The silica-alumina ratio of the silica-alumina ratio of the silica-alumina molecular sieve is 30:

1.

4. The method for preparing 1,5-pentanediol according to claim 1, characterized in that, The catalyst is prepared by a method comprising the following process: The mordenite molecular sieve was impregnated with an aqueous solution containing copper and vanadium sources in equal volumes. The impregnation system was then subjected to post-treatment including filtration, washing, and calcination to obtain the catalyst.

5. The method for preparing 1,5-pentanediol according to claim 4, characterized in that, The equal-volume impregnation process is performed under ultrasonic waves.

6. The method for preparing 1,5-pentanediol according to claim 4, characterized in that, The roasting temperature is 500-600℃, and the roasting time is 4-6h.

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