CN116237058A - Catalyst applicable to preparation of ethanol from lignocellulose, preparation and catalysis method - Google Patents

Catalyst applicable to preparation of ethanol from lignocellulose, preparation and catalysis method Download PDF

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CN116237058A
CN116237058A CN202211556297.0A CN202211556297A CN116237058A CN 116237058 A CN116237058 A CN 116237058A CN 202211556297 A CN202211556297 A CN 202211556297A CN 116237058 A CN116237058 A CN 116237058A
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catalyst
ethanol
lignocellulose
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马隆龙
王海永
张兴华
张琦
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Southeast University
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    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
    • B01J23/892—Nickel and noble metals
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    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
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    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/082—Decomposition and pyrolysis
    • B01J37/084—Decomposition of carbon-containing compounds into carbon
    • C—CHEMISTRY; METALLURGY
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    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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Abstract

The invention discloses a catalyst, a preparation method and a catalysis method for preparing ethanol by lignocellulose. Compared with the existing bimetallic catalyst, the two metal salts are added simultaneously in the precursor preparation process and are roasted at high temperature. In the preparation process of the catalyst, ni particles can be used as a hard template at a lower roasting temperature, and most of Ni particles can be removed by acid washing after roasting, so that graphene shells are left; introducing noble metal particles by an immersion method; noble metal particles serving as reaction centers exist in a nano-reactor formed by carbon shells, so that aggregation and agglomeration of the metal particles are avoided. The biomass raw materials used are wide in source, and can be used only by simple crushing, so that the industrialized preparation of the ethanol by a biomass catalytic method is possible. Compared with the existing catalyst, the Ni content in the catalyst is up to 70%, and the Ni content in the catalyst is only 5%.

Description

Catalyst applicable to preparation of ethanol from lignocellulose, preparation and catalysis method
Technical Field
The invention belongs to the field of ethanol preparation by biomass, and particularly relates to a catalyst, a preparation method and a catalysis method for preparing ethanol by lignocellulose.
Background
Biomass is the only renewable organic carbon resource on earth. Biomass production is about 2000 billions of tons per year worldwide. The China is used as an agricultural large country to have rich biomass resources, and the potential of the biomass resources can reach 10 hundred million tons of standard coal. The total amount of biomass resources that may be utilized as a source of energy per year is about 4.6 hundred million tons of standard coal, mainly agricultural and forestry waste (lignocellulose), and about 60% has not been utilized effectively except for 40% as feed, fertilizer and industrial raw materials. Among the three main constituent units of lignocellulose biomass (cellulose, hemicellulose and lignin), the largest content of cellulose is 30-50% of the weight of lignocellulose, and is the biomass resource with the most abundant reserves in the world, and the high-value conversion of the biomass resource is the key of biomass utilization.
Ethanol is an important popular chemical product and is widely applied in the fields of biofuel, chemical industry, biological medicine, organic synthesis and the like. In the field of biological fuel, ethanol is a high-quality fuel additive, contains oxygen atoms, can promote the combustion of hydrocarbon gasoline, reduces the emission of tail gas harmful substances, and is friendly to the environment; on the other hand, ethanol has higher octane number, has excellent explosion-proof and shock-proof performances, and can be mixed with gasoline to replace tetraethyl lead with higher toxicity and controversial methyl tertiary butyl ether [4]. The method is forced to popularize and use E10 gasoline (10% ethanol is doped in the existing gasoline) in China, and the future consumption of the ethanol is expected to be greatly increased. Therefore, the development of ethanol fuels has become a national strategy, and the green, directional production of ethanol has also become an international research front and hotspot.
One of the source routes of ethanol is to use fossil resources as raw materials (coal, petroleum and natural gas), and the ethanol is obtained by the following conversion routes: ethylene hydration, synthesis gas Fischer-Tropsch direct synthesis and dimethyl ether carbonylation-hydrogenation processes, but these routes have the problems of non-renewable raw materials, low single-pass reaction yield (unreacted raw materials need to be forced to circulate to improve the utilization rate of reactants), long reaction routes, low efficiency and the like. Ethanol can also be prepared by biochemical way by taking lignocellulose biomass as a raw material.
Conventionally, ethanol is prepared from biomass by converting a cellulose component to glucose by enzyme/acidolysis, and fermenting the glucose to obtain ethanol (a two-step method), or fermenting the glucose to obtain ethanol by saccharification in the same reactor (a one-step method). The advantage of biochemical path reaction is that the reaction condition is mild (less than or equal to 50 ℃ C.) and the selectivity of ethanol is high, however, the conversion path of the method has the problems of long production period, high enzyme price, easy poisoning and inactivation and the like whether the method is a two-step method or a one-step method.
The existing chemical preparation method, such as patent CN110092708B, develops a method for preparing ethanol by catalyzing lignocellulose with a graphene-like shell-layer-coated Ni-based catalyst under the synergistic effect of phosphoric acid, and liquid acid phosphoric acid is used as an auxiliary agent. However, the use of liquid acids presents a number of problems such as the materials of the reactor, recovery of the liquid acids, disposal, and environmental pollution. Secondly, in the preparation of the existing catalyst, the metal usage amount is high, the Ni content in the Ni@C catalyst is up to 70%, and the reaction efficiency is low; secondly, in the prior art, noble metal catalysts are used, the noble metal loading is generally about 5% higher, and the stability of the catalyst is poor.
Disclosure of Invention
The invention aims to solve the problems and provide a catalyst, a preparation method and a catalytic method which are suitable for preparing ethanol from lignocellulose, and have the advantages of low reaction efficiency, low metal load and stable catalytic efficiency of the catalyst.
The technical scheme of the invention is as follows: the invention discloses a preparation method of a catalyst suitable for preparing ethanol from lignocellulose, which comprises the following steps:
s1, selecting nickel nitrate, organic matters and deionized water, and stirring for 12 hours at 60-110 ℃ at a stirring speed of 600rpm; heating to 120-160 ℃, and keeping for 12 hours to obtain a powder sample at 400 ℃; roasting the powder sample for 3 hours under the protection of N2 atmosphere to obtain black powder;
s2, rapidly transferring the black powder into a 1M sulfuric acid solution, refluxing for 6 hours, washing with deionized water to be neutral, and freeze-drying to obtain a Ni-based catalyst;
s3, adding Co, pt, pd, ru metal salt and a certain proportion of organic matters into the Ni-based catalyst obtained by freeze drying according to a certain proportion, adding a certain amount of water, stirring and drying, and treating the obtained solid in a mixed gas of 10% H2/N2 at 500-700 ℃ for 1-4 hours to obtain a target catalyst Co-Ni@C, x 1 Pt-Ni@C，x 2 Pd-Ni@C，x 3 Ru-Ni@C。
The invention also discloses a catalyst suitable for preparing ethanol from lignocellulose, wherein the catalyst is a nano metal reactor catalyst and comprises Co-Ni@C, x 1 Pt-Ni@C，x 2 Pd-Ni@C，x 3 Ru-Ni@C；
The shell of the catalyst is a graphene-like shell, the interior of the catalyst is hollow, the graphene-like shell contains Pt, pd and Ru metal nano particles, and the graphene-like shell is internally wrapped with magnetic Ni.
Further, the x is 1 、x 2 、x 3 Is of metal content, x is 1 0.05, x 2 0.10, X 3 0.25.
Further, the catalyst suitable for preparing ethanol from lignocellulose is prepared by the catalyst preparation method suitable for preparing ethanol from lignocellulose.
The invention also discloses a catalyst catalysis method suitable for preparing ethanol by lignocellulose, biomass, cellulose and derivatives C5 and C6 sugar thereof are taken as raw materials, reactants are subjected to selective hydrodeoxygenation reaction under the use of acid and nano metal reactor catalysts to obtain ethanol, the reaction temperature is 180-260 ℃, the reaction time is 0.1-6h, and the hydrogen pressure in a reaction system is 1-5.0MPa;
the acid is phosphoric acid, sulfuric acid, hydrochloric acid and MCM-41, H beta, HY and USY molecular sieves;
the nano metal reactor catalyst is the catalyst suitable for preparing ethanol from lignocellulose.
Further, the acid includes any one of phosphoric acid, sulfuric acid, and hydrochloric acid.
Further, the biomass raw material comprises one of eucalyptus powder, pine powder, birch powder, corn straw, wheat straw, rice straw, sorghum stalk, green bristlegrass, cellulose, glucose, fructose and xylose.
The beneficial effects of the present disclosure are:
1. compared with the existing bimetallic catalyst, the two metal salts are added simultaneously in the precursor preparation process and are roasted at high temperature. In the preparation process of the catalyst, ni particles can be used as a hard template at a lower roasting temperature, and most of Ni particles can be removed by acid washing after roasting, so that graphene shells are left; introducing noble metal particles by an immersion method; noble metal particles serving as reaction centers exist in a nano-reactor formed by carbon shells, so that aggregation and agglomeration of the metal particles are avoided. The biomass raw materials used are wide in source, and can be used only by simple crushing, so that the industrialized preparation of the ethanol by a biomass catalytic method is possible.
2. Compared with the existing catalyst, the Ni content in the catalyst is up to 70%, and the Ni content in the catalyst is only 5%; compared with the existing noble metal catalyst, ni particles partially wrapped by carbon can be used as a magnetic center, and after reaction, solid-liquid separation can be realized by using magnet adsorption. Because the Ni particles are wrapped by carbon, the Ni particles serving as the magnetic center can be stored for a long time, and the Ni particles do not need further reduction before use, have no environmental pollution and are simple and convenient to prepare.
Drawings
FIG. 1 is a TEM image of a 0.1Pt-Ni@C catalyst of example 1 of the invention;
FIG. 2 is a NH view of different molecular sieves in examples 18-17 of the present invention 3 -TPD map.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1: preparation of 0.1Pt-Ni@C catalyst
10mL of deionized water, 0.03mol of metal salt and 0.03mol of organic matter were added to the beaker, stirred at 600rpm for 12 hours at 90℃and heated to 100-140℃until the sample was completely dried. The green powder obtained was taken up in N 2 In the atmosphere, the temperature was raised to 400℃and maintained for 3 hours. The resulting black powder was transferred to a 1M sulfuric acid solution and refluxed for 6 hours. The solid remaining after reflux was filtered, washed and freeze-dried. Subsequently, a certain amount of Ni-based catalyst precursor, organic matter, a certain proportion of metal salt and 5 ml of water were weighed and stirred at 100 degrees until dry. Will give a solid with 10% H at 600 degrees 2 /N 2 And (3) treating the mixture in the gas mixture for 3 hours to finally obtain the catalyst. As can be seen from the TEM image shown in fig. 1, the present method prepares a nano-reactor catalyst having a Ni particle core.
Example 2:
0.15g of 0.05Pt-Ni@C catalyst, 0.4g of cellulose and 40.0ml of 0.05M aqueous phosphoric acid were added to a 100ml autoclave, the autoclave was sealed and purged with H 2 Replacing the gas in the kettle for 6 times and filling H 2 Pressurizing to 3MPa. The stirring paddle (800 rpm) was turned on and the reaction vessel was warmed to 180℃at a heating rate of 5℃per minute, starting the time-lapse reaction. With this catalyst, the reaction time was 1h at a reaction temperature of 180 ℃, and the ethanol product yield was 95.1%.
Examples 3 to 17: reference example 2 differs in that the reaction temperature, pressure and time are different, see in particular table 1. From this table we found that the reaction conditions including temperature, pressure and reaction time all had a significant effect on the reaction, and that under optimal reaction conditions 180oc,3mpa hydrogen initial pressure, ethanol yields up to 95.1% were achieved for 1 hour.
Table 1:
Figure BDA0003982895320000041
examples 18 to 27:
to verify the effect of different acids on the reaction results, it can be seen from Table 2 that the structure and type of the acids are different and the effect on the yield of ethanol is different. Phosphoric acid works best when liquid acid is used, and HY works best when molecular sieves are used.
Reference is made to example 2 and figure 2, except that the molecular sieves used are different and the reaction results are shown in table 2.
Figure BDA0003982895320000051
Examples 28 to 37:
reference example 2 differs in that the metal catalyst used is different, see in particular table 3.
TABLE 3 Table 3
Figure BDA0003982895320000052
As can be seen from the examples in table 3: the effect of the bimetallic catalyst consisting of noble metal and Ni is good because different hydrogenation metals have different influences on the reaction result; when the loading is different, the catalytic effect is different, and when the noble metal loading is too high, excessive hydrogenation exists, and the product can be biased to generate more meteorological products such as methane and the like.
Examples 38 to 49:
reference example 2 differs in that the raw materials used are different, see in particular table 4.
TABLE 4 Table 4
Examples Catalyst Ethanol yield (%)
38 Eucalyptus wood powder 37.2
39 Pine wood powder 36.1
40 Birch wood powder 35.2
41 Corn stalk 31.4
42 Sorghum stalk 30.7
43 Radix Euphorbiae Fischerianae 28.9
44 Wheat straw 31.7
45 Rice pole 29.6
46 Cellulose 95.1
47 Glucose 94.3
48 Fructose 67.7
49 Xylose 75.8
The results of the examples in Table 4 show that: the catalyst and the catalytic system have the same catalytic effect on real biomass.
In the table, the yield of ethanol is the mass ratio of the obtained ethanol to the added raw material.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (7)

1. A preparation method of a catalyst suitable for preparing ethanol from lignocellulose is characterized by comprising the following steps of: comprises the following steps of
S1, selecting nickel nitrate, organic matters and deionized water, and stirring for 12 hours at 60-110 ℃ at a stirring speed of 600rpm; heating to 120-160 ℃, and keeping for 12 hours to obtain a powder sample at 400 ℃; roasting the powder sample for 3 hours under the protection of N2 atmosphere to obtain black powder;
s2, rapidly transferring the black powder into a 1M sulfuric acid solution, refluxing for 6 hours, washing with deionized water to be neutral, and freeze-drying to obtain a Ni-based catalyst;
s3, adding Co, pt, pd, ru metal salt and a certain proportion of organic matters into the Ni-based catalyst obtained by freeze drying according to a certain proportion, adding a certain amount of water, stirring and drying, and treating the obtained solid in a mixed gas of 10% H2/N2 at 500-700 ℃ for 1-4 hours to obtain a target catalyst Co-Ni@C, x 1 Pt-Ni@C，x 2 Pd-Ni@C，x 3 Ru-Ni@C。
2. A catalyst suitable for use in the production of ethanol from lignocellulose, characterized in that: the catalyst is a nano metal reactor catalyst and comprises Co-Ni@C, x 1 Pt-Ni@C，x 2 Pd-Ni@C，x 3 Ru-Ni@C；
The shell of the catalyst is a graphene-like shell, the interior of the catalyst is hollow, the graphene-like shell contains Pt, pd and Ru metal nano particles, and the graphene-like shell is internally wrapped with magnetic Ni.
3. The catalyst for the production of ethanol from lignocellulose according to claim 2, characterized in that: the x is 1 、x 2 、x 3 Is of metal content, x is 1 0.05, x 2 0.10, X 3 0.25.
4. A catalyst suitable for the production of ethanol from lignocellulose according to claim 2 or 3, characterized in that: prepared by the process of claim 1.
5. A catalytic method of a catalyst suitable for preparing ethanol from lignocellulose, which is characterized by comprising the following steps: taking biomass, cellulose and derivatives C5 and C6 sugar thereof as raw materials, and carrying out selective hydrodeoxygenation reaction on reactants under the use of acid and a nano metal reactor catalyst to obtain ethanol, wherein the reaction temperature is 180-260 ℃, the reaction time is 0.1-6h, and the hydrogen pressure in a reaction system is 1-5.0MPa;
the acid is phosphoric acid, sulfuric acid, hydrochloric acid and MCM-41, H beta, HY and USY molecular sieves;
the nano metal reactor catalyst is the catalyst of any one of claims 2-4.
6. The catalytic process for preparing ethanol from lignocellulose according to claim 5, wherein: the acid includes any one of phosphoric acid, sulfuric acid and hydrochloric acid.
7. The catalytic process for preparing ethanol from lignocellulose according to claim 5, wherein: the biomass raw materials comprise eucalyptus powder, pine powder, birch powder, corn straw, wheat straw, rice straw, sorghum stalk, green bristlegrass, cellulose, glucose, fructose and xylose.
CN202211556297.0A 2022-12-06 2022-12-06 Catalyst applicable to preparation of ethanol from lignocellulose, preparation and catalysis method Pending CN116237058A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102671672A (en) * 2011-03-15 2012-09-19 中国科学院大连化学物理研究所 Preparation method and application of carbon-supported nickel-based catalyst
CN109382104A (en) * 2018-10-16 2019-02-26 中国科学技术大学 The method and catalyst of ethyl alcohol are prepared by one step of lignocellulose-like biomass
CN110092708A (en) * 2019-05-17 2019-08-06 中国科学院广州能源研究所 A kind of method that lignocellulosic catalytic hydrogenation prepares ethyl alcohol
CN114057554A (en) * 2020-08-06 2022-02-18 中国科学院广州能源研究所 Method for preparing 2, 5-hexanedione by catalytic hydrogenation of lignocellulose

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102671672A (en) * 2011-03-15 2012-09-19 中国科学院大连化学物理研究所 Preparation method and application of carbon-supported nickel-based catalyst
CN109382104A (en) * 2018-10-16 2019-02-26 中国科学技术大学 The method and catalyst of ethyl alcohol are prepared by one step of lignocellulose-like biomass
CN110092708A (en) * 2019-05-17 2019-08-06 中国科学院广州能源研究所 A kind of method that lignocellulosic catalytic hydrogenation prepares ethyl alcohol
CN114057554A (en) * 2020-08-06 2022-02-18 中国科学院广州能源研究所 Method for preparing 2, 5-hexanedione by catalytic hydrogenation of lignocellulose

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