CN107096528A - A kind of bagasse carbonization load biomass-based catalyst of ruthenium and preparation method and application - Google Patents
A kind of bagasse carbonization load biomass-based catalyst of ruthenium and preparation method and application Download PDFInfo
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- CN107096528A CN107096528A CN201710202565.1A CN201710202565A CN107096528A CN 107096528 A CN107096528 A CN 107096528A CN 201710202565 A CN201710202565 A CN 201710202565A CN 107096528 A CN107096528 A CN 107096528A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/46—Ruthenium, rhodium, osmium or iridium
- B01J23/462—Ruthenium
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/132—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group
- C07C29/136—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH
- C07C29/14—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH of a —CHO group
- C07C29/141—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH of a —CHO group with hydrogen or hydrogen-containing gases
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Abstract
The invention discloses a kind of bagasse carbonization load biomass-based catalyst of ruthenium and preparation method and application.The present invention is used using bagasse as raw material, and carbonization infusion process prepares carbon-based ruthenium catalyst.The load agent bagasse of the bagasse carbonization load biomass-based catalyst of ruthenium of the present invention comes from factory waste.Bagasse is reused as waste agronomic crop, not only energy-conserving and environment-protective but also abundance;As solid catalyst, it can be separated with reaction system, while catalytic activity is high, can repeatedly used, with wide application prospect using suction filtration.
Description
Technical field
The present invention relates to the catalyst technical field that sorbierite is prepared for being catalyzed glucose, and in particular to a kind of bagasse carbon
Change load biomass-based catalyst of ruthenium and preparation method and application.
Background technology
With the continuous exhaustion of petrochemical material, the utilization to renewable resource biomass gradually causes the very big pass of people
Note and research.Biomass energy has the advantages that aboundresources, renewable, low stain because of it so that it is in human lives and society
Value in meeting activity is improved constantly, very big with that using a kind of trend has been formed, can create to biological Quality Research
Ground is worth and facility.China is large agricultural country, and the husk of substantial amounts of agricultural crop straw and agricultural and sideline crop product is produced every year, its
In, have the advantages that to economize on resources to the recycling of waste material bagasse, environmental protection.
Glucose is a kind of most wide and mostly important monose of distributed in nature, can be prepared by biomass resource.Portugal
Grape sugar can prepare a series of chemicals and fuel by physics, chemistry or bioanalysis, be widely used in mankind's daily life.
Wherein, sorbierite is as one of Important Platform compound prepared by glucose, with very big practicality and researching value, in food
The industries such as product, daily use chemicals, medicine play the role of extremely wide, can be used as sweetener, NMF, preservative etc..At present, exist
In industrial production, sorbierite is mainly catalyzed glucose hydrogenation reaction by metallic catalyst and is made.Early stage is studied main using gold
Belong to nickel as active metal, but poor catalyst stability prepared by this metal, easily it is lost in during the course of the reaction.For this skill
Art is not enough, how to obtain catalytic performance height and the good catalyst of stability causes very big concern.It is porous easily attached using activated carbon
The advantage, using bagasse as raw material, carbon-based ruthenium catalyst is prepared using carbonization-infusion process, each side optimizes the property of catalyst
Can, obtain the new catalyst that catalytic performance is good, can repeatedly use.Improvement and optimization to catalyst, so as to obtain
Obtain high transformation efficiency so that glucose prepares sorbierite with bigger application value and meaning.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of bagasse carbonization load biomass-based catalysis of ruthenium
Agent, the catalyst has the ability of well loaded ruthenium, and catalytic performance is good, reusable.
The present invention also aims to provide a kind of preparation method of bagasse carbonization load biomass-based catalyst of ruthenium,
The preparation method is using bagasse as raw material, and carbonization-infusion process prepares carbon-based ruthenium catalyst (Ru/CSB), recycles bagasse and prepares carbon
Change the load biomass-based catalyst of ruthenium.
The present invention also aims to provide a kind of described bagasse carbonization load biomass-based catalyst of ruthenium in catalysis Portugal
Grape sugar prepares the application in sorbierite.
The object of the invention is achieved through the following technical solutions.
A kind of preparation method of the bagasse carbonization load biomass-based catalyst of ruthenium, comprises the following steps:
(1) the size-reduced machine of raw material bagasse is crushed, and be dried in vacuo;
(2) bagasse after crushing is stripped dewaxing, and be dried in vacuo;
(3) bagasse after dewaxing is subjected to high temperature cabonization;
(4) RuCl is taken3·xH2O and the bagasse after carbonization add ultra-pure water, are uniformly mixed in boiling flask;Drop
Plus NaBH4The aqueous solution, is again stirring for being reacted;After reaction terminates, mixture is filtered, washed repeatedly with deionized water, is removed
Chlorion, vacuum drying obtains the bagasse carbonization load biomass-based catalyst of ruthenium.
Further, in step (1), the crushing is to be crushed to bagasse size for 150~180um.
Further, in step (1), the vacuum drying is 10~15h of vacuum drying at 50~80 DEG C.
Further, in step (2), the extracting is in Soxhlet extractor, to utilize toluene-ethano mixed solvent system
It is stripped.
Further, in step (2), in the toluene-ethano mixed solvent system, the volume ratio of toluene and ethanol is
2:1。
Further, in step (2), the temperature of the extracting is 120~150 DEG C, and the time of extracting is 5~8h.
Further, in step (2), the vacuum drying is 12~16h of vacuum drying at 50~80 DEG C.
Further, in step (3), the high temperature cabonization is carried out in tube furnace, under nitrogen atmosphere, the flow velocity of nitrogen
For 70mL/min, the temperature of carbonization is 300~500 DEG C, and preferably 450 DEG C, the time of carbonization is 1.5h, cold after carbonization terminates
But to room temperature;Bagasse after carbonization is the incomplete carbonized product of bagasse (the Carbonized sugarcane of black powder
bagasse,CSB)。
Further, in step (4), the RuCl3·xH2The mass ratio of O and the bagasse after carbonization is 1:5~1:10.
Further, in step (4), the solid-liquid ratio of bagasse and ultra-pure water after the carbonization is 1:50:~1:100g/
mL。
Further, in step (4), the time being uniformly mixed is 2~3h.
Further, in step (4), the NaBH4The aqueous solution is now with the current solution, and concentration is 1wt%.
Further, in step (4), bagasse and NaBH after the carbonization4The solid-liquid ratio of the aqueous solution is 1:100~1:
150g/mL。
Further, in step (4), the time of the reaction is 4~5h.
Further, the number of times that in step (4), the deionized water filters repeatedly, wash is 3~5 times.
Further, in step (4), chlorion go division result by using 0.1mol/L silver nitrate solution detection wash
Liquid is washed to obtain.
Further, in step (4), the vacuum drying is 12~16h of vacuum drying at 50~80 DEG C.
A kind of bagasse carbonization load biomass-based catalyst of ruthenium made from the preparation method as described in any of the above-described.
A kind of application of the described bagasse carbonization load biomass-based catalyst of ruthenium in catalysis glucose prepares sorbierite,
It is as follows including step:
Glucose and the bagasse carbonization load biomass-based catalyst of ruthenium are added in stainless steel cauldron, under hydrogen atmosphere
Heating is reacted, and obtains sorbierite.
Further, the consumption of the bagasse carbonization load biomass-based catalyst of ruthenium for reaction system 0.5wt%~
2.0wt%, preferably 1wt%.
Further, the pressure of the hydrogen is 1~5MPa, preferably 3MPa.
Further, the temperature of the reaction is 80 DEG C~160 DEG C, preferably 120 DEG C.
Further, the time of the reaction is 0.5~3h, preferably 2h.
Compared with prior art, the invention has the advantages that and beneficial effect:
(1) load agent of the bagasse of the invention carbonization load biomass-based catalyst of ruthenium using bagasse as active metal ruthenium,
The loss of ruthenium in the reaction is not only reduced, and has effectively reused agricultural wastes bagasse, energy-conserving and environment-protective;
(2) catalytic performance of the bagasse of the invention carbonization load biomass-based catalyst of ruthenium is good, by suction filtration by bagasse
The carbonization load biomass-based catalyst of ruthenium is separated with reaction system, can be used repeatedly, stability is good;
(3) preparation method of the present invention is simple and easy to apply, Bagasse Material abundance and cheap, with significant Technological Economy effect
Really, it is with a wide range of applications.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Each initiation material is commercially available or prepared according to art methods in preparation method of the present invention.
Embodiment 1
A kind of preparation of the bagasse carbonization load biomass-based catalyst of ruthenium, step is as follows:
1st, bagasse is pre-processed:
Bagasse is crushed after drying through pulverizer, takes 150~180um parts, 60 DEG C of dry 12h in vacuum drying chamber;It is dry
Bagasse powder after dry uses toluene-ethano (2 in 500ml Soxhlet extractors:1, v/v) 6h is extracted at 140 DEG C, dewaxed
Bagasse 60 DEG C of dry 16h in vacuum drying chamber are standby.
2nd, bagasse is carbonized:
The 3g bagasses for learning from else's experience pretreated are placed in tube furnace, are first passed through air-tightness and emptying that nitrogen examines whole pipeline
Air in pipeline;Then whole pipeline is sealed, boiler tube is purified using nitrogen, and control the flow velocity of nitrogen for 70mL/min,
Heating rate is 5 DEG C/min, is heated to 450 DEG C from room temperature and keeps 1.5h at this temperature;After carbonization terminates, room is cooled to
Temperature, obtains the incomplete carbonized product of bagasse of black powder.
3rd, the preparation of the bagasse carbonization load biomass-based catalyst of ruthenium (Ru/CSB catalyst)
The main preparation process of 5wt%Ru/CSB catalyst is as follows:0.8g CSB and 0.1089g are accurately weighed respectively
RuCl3·xH2O adds 60ml ultra-pure water in 250ml boiling flasks;After quick stirring 2h, 1wt% is slowly added dropwise
NaBH4Aqueous solution 100mL, is again stirring for 4h;
Wherein, 1wt%NaBH4The aqueous solution is now with the current:Take 1g NaBH4Powder is placed in 100ml beakers, is added 30ml and is gone
Ionized water dissolves, and transfers in 100ml volumetric flasks, constant volume;
Obtained mixture is filtered, washed 3 times repeatedly with deionized water, to remove chlorion, and using 0.1mol/L's
Silver nitrate solution is detected;Obtained mixture dries 16h in vacuum constant temperature drying box at 50 DEG C, obtain the 5wt%
Ru/CSB catalyst.
Embodiment 2
The preparation of the bagasse carbonization load biomass-based catalyst of ruthenium under different carburizing temperatures:
Change carburizing temperature when bagasse is carbonized, other conditions are same as Example 1, wherein carburizing temperature is respectively 300
℃、350℃、400℃、450℃、500℃。
Embodiment 3
The bagasse carbonization load biomass-based catalyst glucose of ruthenium under the different carburizing temperatures prepared using embodiment 2
Prepare sorbierite:
It will be made under 25ml 10wt% glucose, the different carburizing temperatures of 1wt% (relative to reaction system content) embodiment 2
Standby Ru/CSB catalyst is added in stainless steel cauldron, after hydrogen cleaning reactor, and Hydrogen Vapor Pressure in reactor is adjusted
It is heated to 3Mpa, then by reactor after 120 DEG C, opens stirring, rotating speed is 600rpm, is reacted for 2 hours.
After reaction terminates, reaction solution is through high performance liquid chromatography detection, inversion rate of glucose and gained sorbierite yield such as table 1
It is shown.
The catalytic effect of Ru/CSB catalyst under the different carburizing temperatures of table 1
As shown in Table 1, carburizing temperature is significantly affected to inversion rate of glucose and sorbierite yield.With carburizing temperature
Rise, inversion rate of glucose and sorbierite yield are all improved;When carburizing temperature reaches 450 DEG C, inversion rate of glucose and
Sorbierite yield all reaches maximum, respectively 99.41% and 98.13%.When continuing to improve carbonization temperature, glucose conversion
Rate and sorbierite yield are all declined slightly.Therefore, optimal carburizing temperature is 450 DEG C.
Embodiment 4
Different Ru/CSB catalyst amounts prepare the influence of sorbierite catalytic activity to catalysis glucose:
25ml 10wt% glucose (is contained with 0.5wt%, 1wt%, 1.5wt%, 2wt% relative to reaction system respectively
Amount) embodiment 1 prepare Ru/CSB catalyst be added in stainless steel cauldron, after hydrogen cleaning reactor, by reactor
Interior Hydrogen Vapor Pressure is adjusted to 3Mpa, then reactor is heated to after 120 DEG C, opens stirring, rotating speed is 600rpm, is reacted for 2 hours.
After reaction terminates, reaction solution is through high performance liquid chromatography detection, inversion rate of glucose and gained sorbierite yield such as table 2
It is shown.
The catalytic effect of Ru/CSB catalyst under the different catalysts consumption of table 2
As shown in Table 2, with the increase of catalyst amount, inversion rate of glucose and sorbierite yield are significantly improved;When urging
When agent consumption is 1wt%, inversion rate of glucose and sorbierite yield respectively reach 99.41% and 98.13%.When catalyst is used
When amount continues to increase, inversion rate of glucose and sorbierite yield are only heightened by a small margin, or even decline slightly, reactive group occur
Originally balance is reached.Therefore, optimum catalyst consumption is 1wt%.
Embodiment 5
Ru/CSB catalyst prepares the influence of sorbierite catalytic activity to catalysis glucose under different hydrogen pressure:
Ru/CSB catalysis prepared by 25ml 10wt% glucose and 1wt% (relative to reaction system content) embodiment 1
Agent is added in stainless steel cauldron, after hydrogen cleaning reactor, by Hydrogen Vapor Pressure in reactor be adjusted to respectively 1MPa,
2MPa, 3MPa, 4MPa, 5MPa, then reactor is heated to after 120 DEG C, stirring is opened, rotating speed is 600rpm, reacts small for 2
When.
After reaction terminates, reaction solution is through high performance liquid chromatography detection, inversion rate of glucose and gained sorbierite yield such as table 3
It is shown.
The catalytic effect of Ru/CSB catalyst under the different hydrogen pressure of table 3
As shown in Table 3, with the increase of Hydrogen Vapor Pressure, inversion rate of glucose and sorbierite yield are greatly enhanced;Work as hydrogen
When atmospheric pressure is 3MPa, inversion rate of glucose and sorbierite yield respectively reach 99.41% and 98.13%, and glucose is substantially complete
Full conversion, reaction basically reaches balance.Therefore, optimal Hydrogen Vapor Pressure is 3MPa.
Embodiment 6
Ru/CSB catalyst prepares the influence of sorbierite catalytic activity to catalysis glucose at a temperature of differential responses:
Ru/CSB catalysis prepared by 25ml 10wt% glucose and 1wt% (relative to reaction system content) embodiment 1
Agent is added in stainless steel cauldron, after hydrogen cleaning reactor, and Hydrogen Vapor Pressure in reactor is adjusted into 3MPa, then will reaction
Kettle is separately heated to after 80 DEG C, 100 DEG C, 120 DEG C, 140 DEG C, 160 DEG C, opens stirring, rotating speed is 600rpm, is reacted for 2 hours.
After reaction terminates, reaction solution is through high performance liquid chromatography detection, inversion rate of glucose and gained sorbierite yield such as table 4
It is shown.
The catalytic effect of Ru/CSB catalyst at a temperature of the differential responses of table 4
As shown in Table 4, with the rise of temperature, inversion rate of glucose and sorbierite yield are significantly improved;Work as reaction temperature
When reaching 120 DEG C, inversion rate of glucose and sorbierite yield respectively reach 99.41% and 98.13%, and now glucose is substantially complete
Full conversion, the yield and selectivity of sorbierite is also higher.But when temperature continues to raise, the yield and selectivity of sorbierite are on the contrary
Reduction, illustrates that temperature is too high and is unfavorable for generating sorbierite.Therefore, optimal reaction temperature is 120 DEG C.
Embodiment 7
Ru/CSB catalyst prepares the influence of sorbierite catalytic activity to catalysis glucose under the differential responses time:
Ru/CSB catalysis prepared by 25ml 10wt% glucose and 1wt% (relative to reaction system content) embodiment 1
Agent is added in stainless steel cauldron, after hydrogen cleaning reactor, and Hydrogen Vapor Pressure in reactor is adjusted into 3MPa, then will reaction
Kettle is heated to after 120 DEG C, opens stirring, and rotating speed is 600rpm, and the reaction time is respectively 0.5,1,1.5,2,2.5,3 hours.
After reaction terminates, reaction solution is through high performance liquid chromatography detection, inversion rate of glucose and gained sorbierite yield such as table 5
It is shown.
The catalytic effect of Ru/CSB catalyst under the differential responses time of table 5
As shown in Table 5, inversion rate of glucose and sorbierite yield have very big relation with the reaction time.With the reaction time
Increase, inversion rate of glucose and sorbierite yield are quickly improved;When being 2h between when reacted, inversion rate of glucose and sorbierite
Yield respectively reaches 99.41% and 98.13%, and glucose is converted substantially, and reaction reaches in a basic balance.The continuation in reaction time increases
Plus influence to reaction and little, therefore, optimum reacting time is 2 hours.
Embodiment 8
The recovered frequency of catalyst prepares the influence of sorbierite catalytic activity to catalysis glucose:
Catalyst in above-described embodiment is reclaimed, selection carburizing temperature carries out repeating real for 450 DEG C of catalyst
Test.
Be carbonized Ru/CSB at 450 DEG C that 25ml 10wt% glucose and 1wt% (relative to reaction system content) are reclaimed
Catalyst is added in stainless steel cauldron, after hydrogen cleaning reactor, and Hydrogen Vapor Pressure in reactor is adjusted into 3MPa, then will
Reactor is separately heated to after 120 DEG C, opens stirring, rotating speed is 600rpm, is reacted for 2 hours, repeats experiment 5 times.
After reaction terminates, reaction solution is through high performance liquid chromatography detection, inversion rate of glucose and gained sorbierite yield such as table 6
It is shown.
The catalytic effect for the Ru/CSB catalyst that table 6 is reclaimed
As shown in Table 6, the bagasse carbonization load biomass-based catalyst of ruthenium of recovery can be used repeatedly, and stably
Property keep good, reuse efficiency high.
Claims (10)
1. a kind of preparation method of the bagasse carbonization load biomass-based catalyst of ruthenium, it is characterised in that comprise the following steps:
(1)The size-reduced machine of raw material bagasse is crushed, and is dried in vacuo;
(2)Bagasse after crushing is stripped dewaxing, and is dried in vacuo;
(3)Bagasse after dewaxing is subjected to high temperature cabonization;
(4)Take RuCl3•xH2O and the bagasse after carbonization add ultra-pure water, are uniformly mixed in boiling flask;It is added dropwise
NaBH4The aqueous solution, is again stirring for being reacted;After reaction terminates, mixture is filtered, washed repeatedly with deionized water, except dechlorination
Ion, vacuum drying obtains the bagasse carbonization load biomass-based catalyst of ruthenium.
2. a kind of preparation method of bagasse carbonization load biomass-based catalyst of ruthenium according to claim 1, its feature exists
In step(1)In, the crushing is to be crushed to bagasse size for 150~180 um;The vacuum drying is at 50 ~ 80 DEG C
It is dried in vacuo 10 ~ 15h.
3. a kind of preparation method of bagasse carbonization load biomass-based catalyst of ruthenium according to claim 1, its feature exists
In step(2)In, the extracting is in Soxhlet extractor, to be stripped using toluene-ethano mixed solvent system;It is described
In toluene-ethano mixed solvent system, the volume ratio of toluene and ethanol is 2:1;The temperature of the extracting is 120 ~ 150 DEG C, is taken out
The time carried is 5 ~ 8h;The vacuum drying is 12 ~ 16h of vacuum drying at 50 ~ 80 DEG C.
4. a kind of preparation method of bagasse carbonization load biomass-based catalyst of ruthenium according to claim 1, its feature exists
In step(3)In, the high temperature cabonization is carried out in tube furnace, under nitrogen atmosphere, and the flow velocity of nitrogen is 70 mL/min, carbon
The temperature of change is 300~500 DEG C, and the time of carbonization is 1.5 h, after carbonization terminates, is cooled to room temperature.
5. a kind of preparation method of bagasse carbonization load biomass-based catalyst of ruthenium according to claim 1, its feature exists
In step(4)In, the RuCl3•xH2The mass ratio of O and the bagasse after carbonization is 1:5~1:10;Bagasse after the carbonization with
The solid-liquid ratio of ultra-pure water is 1:50~1:100g/mL;The time being uniformly mixed is 2 ~ 3h.
6. a kind of preparation method of bagasse carbonization load biomass-based catalyst of ruthenium according to claim 1, its feature exists
In step(4)In, the NaBH4The aqueous solution is now with the current solution, and concentration is 1wt%;Bagasse and NaBH after the carbonization4
The solid-liquid ratio of the aqueous solution is 1:100~1:150g/mL;The time of the reaction is 4 ~ 5h.
7. a kind of preparation method of bagasse carbonization load biomass-based catalyst of ruthenium according to claim 1, its feature exists
In step(4)In, the deionized water filters repeatedly, the number of times that washs is 3 ~ 5 times;Chlorion go division result by using
0.1 mol/L silver nitrate solution detection cleaning solution is obtained;The vacuum drying is 12 ~ 16h of vacuum drying at 50 ~ 80 DEG C.
8. a kind of bagasse carbonization load biomass-based catalyst of ruthenium as made from any one of claim 1 ~ 7 preparation method.
9. a kind of bagasse carbonization load biomass-based catalyst of ruthenium described in claim 8 is in catalysis glucose prepares sorbierite
Application, it is characterised in that it is as follows including step:
Glucose and the bagasse carbonization load biomass-based catalyst of ruthenium are added in stainless steel cauldron, heated under hydrogen atmosphere
Reacted, obtain sorbierite.
10. application according to claim 9, it is characterised in that the bagasse carbonization load biomass-based catalyst of ruthenium
Consumption is 0.5wt%~2.0wt% of reaction system;The pressure of the hydrogen is 1~5MPa;The temperature of the reaction be 80 DEG C~
160 DEG C, the time of reaction is 0.5~3h.
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CN112844476A (en) * | 2021-01-18 | 2021-05-28 | 武汉科技大学 | Biomass-based carbon material loaded nano nickel catalyst and preparation method and application thereof |
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CN112919922A (en) * | 2021-04-13 | 2021-06-08 | 西北工业大学 | Chemical vapor infiltration method for preparing pyrolytic carbon with external biomass catalyst |
CN113101925A (en) * | 2021-04-16 | 2021-07-13 | 河北工业大学 | Preparation method and application of lignin-based adsorption-catalysis material |
CN113120989A (en) * | 2021-05-25 | 2021-07-16 | 中国电建集团江西省电力建设有限公司 | Method for treating antibiotic-polluted water body by using functional green carbon material |
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