CN106040313A - Preparation method of modified biomass carbon catalyst carrier - Google Patents
Preparation method of modified biomass carbon catalyst carrier Download PDFInfo
- Publication number
- CN106040313A CN106040313A CN201610492241.1A CN201610492241A CN106040313A CN 106040313 A CN106040313 A CN 106040313A CN 201610492241 A CN201610492241 A CN 201610492241A CN 106040313 A CN106040313 A CN 106040313A
- Authority
- CN
- China
- Prior art keywords
- limax
- preparation
- deionized water
- carbon catalyst
- biomass carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 51
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000003054 catalyst Substances 0.000 title claims abstract description 46
- 239000002028 Biomass Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000008367 deionised water Substances 0.000 claims abstract description 27
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 27
- 238000005406 washing Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 16
- 210000001835 viscera Anatomy 0.000 claims abstract description 16
- 239000012043 crude product Substances 0.000 claims abstract description 14
- 238000007599 discharging Methods 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 7
- 241001523405 Limax Species 0.000 claims description 38
- 241000255791 Bombyx Species 0.000 claims description 27
- 238000001914 filtration Methods 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 15
- 230000004048 modification Effects 0.000 claims description 14
- 238000012986 modification Methods 0.000 claims description 14
- 230000010355 oscillation Effects 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000012634 fragment Substances 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 230000037396 body weight Effects 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 6
- 230000001186 cumulative effect Effects 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 238000011068 loading method Methods 0.000 claims description 6
- 239000013049 sediment Substances 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 abstract description 11
- 239000011148 porous material Substances 0.000 abstract description 9
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 241000237858 Gastropoda Species 0.000 abstract 3
- 241000255789 Bombyx mori Species 0.000 abstract 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract 1
- 229910017604 nitric acid Inorganic materials 0.000 abstract 1
- 239000000463 material Substances 0.000 description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 7
- 239000012620 biological material Substances 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 4
- 229910001961 silver nitrate Inorganic materials 0.000 description 4
- 102000004190 Enzymes Human genes 0.000 description 3
- 108090000790 Enzymes Proteins 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000003610 charcoal Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 229940088598 enzyme Drugs 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 210000003097 mucus Anatomy 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000004382 Amylase Substances 0.000 description 1
- 102000013142 Amylases Human genes 0.000 description 1
- 108010065511 Amylases Proteins 0.000 description 1
- 108010059892 Cellulase Proteins 0.000 description 1
- 102000005598 Chondroitin Sulfate Proteoglycans Human genes 0.000 description 1
- 108010059480 Chondroitin Sulfate Proteoglycans Proteins 0.000 description 1
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 1
- 108091005804 Peptidases Proteins 0.000 description 1
- 239000004365 Protease Substances 0.000 description 1
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 235000019418 amylase Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 229940106157 cellulase Drugs 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 238000010353 genetic engineering Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- 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
- B01J23/70—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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/617—500-1000 m2/g
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/63—Pore volume
- B01J35/633—Pore volume less than 0.5 ml/g
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of a modified biomass carbon catalyst carrier, and belongs to the technical field of the preparation of catalysts. The preparation method comprises the following steps: by using a snail as a raw material and taking internal organs of the snail after dirt is removed from the internal organs, preparing a modified solution, mixing the modified solution and a silkworm cocoon-based biological carbon carrier crude product, modifying to obtain filter residue, adding a nitric acid solution, shaking, washing by using deionized water, drying, and discharging to obtain the modified biomass carbon catalyst carrier. Examples prove that the method is unique and novel; by using the snail and silkworm cocoon as raw materials, the energy is saved, and the cost is reduced; the preparation method belongs to an environment-friendly process; moreover, the process is simple, and no special instrument is used; and the finally prepared biomass carbon catalyst carrier is high in dispersity, high in absorption capacity, good in pore volume and specific surface area, uniform in pores and wide in application prospect.
Description
Technical field
The invention discloses the preparation method of a kind of modified biomass carbon catalyst support, belong to catalyst preparation technology neck
Territory.
Background technology
The energy is All Around The World development and the most basic driving force of economic growth, is the bases depended on for existence of the mankind.But
The mankind are enjoying while the energy brings economic development, scientific and technological progress interests, also run into a series of unavoidable energy shortage,
The problems such as contention for resource and the excessive environmental pollution using the energy to cause, what this was serious threatens the survival and development of the mankind.
In the face of the serious challenge of energy crisis, countries in the world are all improved traditional energy make great efforts or find alternative traditional energy
New forms of energy meet the demand of life.
Biomass-based material is the functional material that a class has development potentiality, and it can substitute traditional material, and it is right to reduce
The problems such as the dependence of fossil resource and environmental pollution.Meanwhile, biological material is because having high specific surface area and abundant sense
Group, it is possible to chelated metal ions and nanoparticle, can in most organic solvents stable existence.Additionally, biomass also have
There are the advantages such as of a great variety, biodegradable and good biocompatibility, are the ideal carrier preparing catalyst.Therefore, if
Meter and the structure catalyst system tool with biomass as carrier is of great significance.
The specific surface area of material with carbon element and aperture are not only closely related with its preparation method, are also affected by raw material, select
Suitably raw material is extremely important to producing high quality carbon material.Traditional material with carbon element is to be main by coal, oil or its processing product etc.
Raw material is wanted to be prepared by processed.But nowadays the deterioration of the energy in global range, crisis of resource and ecological environment is right
The development further of conventional carbon material proposes challenge.Biological material such as forestry biomass, agricultural wastes, energy-source plant etc.
Belong to Renewable resource, and major part biological material all contains abundant carbon, becomes and prepares the rich of various material with carbon element
Rich raw material.Utilize biological material to prepare various material with carbon element for raw material, material with carbon element production cost can be reduced, it is achieved material with carbon element
Sustainable development.But it is low that biomass carbon material but also exists dispersion, hole heterogeneity and the little defect of pore capacities, limit
Its application in catalyst carrier field.
In the prior art, Snailase extract the Limax mucus that self is secreted under stimulation of main live body Limax and
The internal organs of Limax are raw material, and Limax mucus composition includes protein, Snailase, mucoitin, chondroitin sulfate proteoglycan, hydroxyl
Acetic acid etc.；Containing more than 20 kind of enzyme in the prolixity capsule of Limax and digestive tract, Snailase is multiple mixed enzyme；Wherein there is cellulase, really
Glue enzyme, amylase, protease etc.；It is worth height, is widely used in cytology, genetic engineering field, medically, adding of feedstuff
Adding agent, health product have application.
Summary of the invention
The technical problem that present invention mainly solves: prepare various material with carbon element for currently with biological material, though permissible
Reducing the cost of material with carbon element, but it is low to there is dispersion, hole heterogeneity and the little present situation of boring ratio capacity, it is provided that Yi Zhongli
It is raw material with Limax, by taking internal organs after telling dirty blowdown, makes modification liquid by oneself, and mix with Bombyx bombycis base biological carbon carrier crude product, change
Obtain filtering residue after property, add salpeter solution, utilize deionized water drip washing, dried discharging after oscillation treatment, thus obtain modified raw
The preparation method of material carbon catalyst support.The method uniqueness is novel, is not raw material merely with Limax and Bombyx bombycis, has saved energy
Source, reduces cost, belongs to environmental protection technique, and simple process, it is not necessary to specific apparatus so that the final biomass prepared
Carbon catalyst support dispersion is high, high adsorption capacity, has bigger pore volume and specific surface area, and hole is uniform, has wide
Application prospect.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) Limax selecting more than 30～40 body weight 15g is put in the beaker equipped with 1～2cm deep deionized water of the bottom, then drips
Add 15～20mL Oleum Camelliae, beaker is put in 20～30 DEG C of water-baths, stand and make Limax tell dirty blowdown 3～5 days；
(2) being taken out by the Limax after above-mentioned blowdown, artificial broken shell also takes out the Limax internal organs loading conical flask with agitator, to
Add the deionized water of Limax internal organs cumulative volume 5～8 times 20～25 DEG C in Ping, start agitator with 500～600r/min rotating speeds
Stir process 3～5h；
(3) filter after stirring terminates to separate and remove filtering residue, filtrate is loaded high speed centrifuge, turns with 10000～12000r/min
Speed centrifugal 15～20min, separates and removes lower sediment, obtain supernatant, i.e. make modification liquid by oneself, puts in 4～6 DEG C of ice-water baths and protects
Deposit standby；
(4) weigh 200～300g Bombyx bombycis put into buchner funnel successively by dehydrated alcohol and deionized water filtering and washing 10～
20min, will be cut into the fragment of 1～3cm, then puts in retort by Bombyx bombycis fragment, be passed through argon after the cocoon drying after washing
As protection gas, at 800～900 DEG C, discharging after insulation calcining 2～4h, obtains Bombyx bombycis base biological carbon carrier crude product；
(5) 40～50g Bombyx bombycis base biological carbon carrier crude products obtained above are poured into 300～400mL standby self-control modifications
In the ceramic pot of liquid, put in the calorstat of 30～40 DEG C, filter after dipping modified 10～12h and separate to obtain filtering residue；
(6) filtering residue obtained above is poured into its volume 8～10 times of concentration are in 2mol/L salpeter solution, put into sonic oscillation
Instrument, with 200～300W power ultrasonic oscillation treatment 6～8h under the conditions of 75～85 DEG C, and with deionized water drip washing until drip washing
Liquid is neutrality, puts into discharging after baking oven is dried 8～10h at 105～110 DEG C, obtains modified biomass carbon catalyst support.
The application process of the present invention is: weighs 5～6g silver nitrate, 8～10g nickel nitrate and is placed in 200～300mL deionized waters,
Stirring, the modified biomass carbon catalyst support present invention prepared afterwards is put into wherein, soaks 8～10h, filters
Must precipitate, move in Muffle furnace, at 600～800 DEG C, calcine 3～4h, treat that calcining terminates, i.e. can get nickel-base catalyst, warp
Detection, prepare nickel-base catalyst compared with traditional catalyst, catalysis activity improve 30～32%, catalytic efficiency improve 40～
45%, additionally catalytic life is 1～2 times for the traditional catalyst life-span, has broad application prospects.
The modified biomass carbon catalyst support specific surface area that the present invention prepares is up to 715～735m2g-1, pore size is
28～32nm, mesopore volume is 0.2～0.3mg/L, and intensity is 8.0～9.0N/mm.
The invention has the beneficial effects as follows:
(1) the inventive method uniqueness is novel, utilize Limax and Bombyx bombycis for raw material, it is to avoid the evil of crisis of resource and ecological environment
Change, saved the energy, reduced cost, belonged to environmental protection technique；
(2) present invention process is easy, it is not necessary to specific apparatus, and the final biomass carbon catalyst carrier dispersion prepared is high, absorption
Ability is strong, has preferable pore volume and specific surface area, and hole is uniform；
(3) the biomass carbon catalyst carrier that the present invention prepares has broad application prospects, and can be in large-scale application.
Detailed description of the invention
First the Limax selecting more than 30～40 body weight 15g puts into the bottom beaker equipped with 1～2cm deep deionized water
In, then drip 15～20mL Oleum Camelliae, beaker is put in 20～30 DEG C of water-baths, stand and make Limax tell dirty blowdown 3～5 days；
Then being taken out by the Limax after above-mentioned blowdown, artificial broken shell also takes out the Limax internal organs loading conical flask with agitator, to bottle
The middle deionized water adding Limax internal organs cumulative volume 5～8 times 20～25 DEG C, starts agitator and stirs with 500～600r/min rotating speeds
Mix process 3～5h；Stirring is filtered to separate after terminating and is removed filtering residue, filtrate is loaded high speed centrifuge, with 10000～12000r/
Min rotating speed is centrifuged 15～20min, separates and removes lower sediment, obtains supernatant, i.e. make modification liquid by oneself, put into 4～6 DEG C of frozen water
Bath saves backup；Next weigh 200～300g Bombyx bombycis and put into buchner funnel successively with dehydrated alcohol and deionized water sucking filtration
Washing 10～20min, will be cut into the fragment of 1～3cm, then puts in retort by Bombyx bombycis fragment after the cocoon drying after washing,
Be passed through argon as protection gas, at 800～900 DEG C insulation calcining 2～4h after discharging, obtain Bombyx bombycis base biological carbon carrier crude product；
Then 40～50g Bombyx bombycis base biological carbon carrier crude products obtained above are poured into 300～400mL standby self-control modification liquids
In ceramic pot, put in the calorstat of 30～40 DEG C, filter after dipping modified 10～12h and separate to obtain filtering residue；Finally obtain above-mentioned
To filtering residue pour its volume 8 into～10 times of concentration are in 2mol/L salpeter solution, put into sonic oscillation instrument, 75～85 DEG C of conditions
Under with 200～300W power ultrasonic oscillation treatment 6～8h, and with deionized water drip washing until leacheate is neutrality, put into baking oven
Discharging after being dried 8～10h at 105～110 DEG C, obtains modified biomass carbon catalyst support.
Example 1
First the Limax selecting more than 30 body weight 15g is put in the beaker equipped with the deep deionized water of 1cm of the bottom, then drips 15mL
Oleum Camelliae, puts in 20 DEG C of water-baths by beaker, stands and makes Limax tell dirty blowdown 3 days；Then the Limax after above-mentioned blowdown is taken
Going out, artificial broken shell also takes out the Limax internal organs loading conical flask with agitator, adds Limax internal organs cumulative volume 5 times 20 in bottle
DEG C deionized water, start agitator with 500r/min rotating speed stir process 3h；Stirring is filtered to separate after terminating and is removed filtering residue, will
Filtrate loads high speed centrifuge, is centrifuged 15min with 10000r/min rotating speed, separates and removes lower sediment, obtains supernatant, i.e. certainly
Modification liquid processed, puts in 4 DEG C of ice-water baths and saves backup；Next weigh 200g Bombyx bombycis to put into buchner funnel and use dehydrated alcohol successively
With deionized water filtering and washing 10min, the fragment of 1cm will be cut into after the cocoon drying after washing, then Bombyx bombycis fragment is put into charcoal
Changing in stove, be passed through argon as protection gas, at 800 DEG C, discharging after insulation calcining 2h, obtains Bombyx bombycis base biological carbon carrier crude product；So
After Bombyx bombycis base biological carbon carrier crude product obtained above for 40g is poured in the ceramic pot with 300mL standby self-control modification liquid, put
Enter in the calorstat of 30 DEG C, filter after the modified 10h of dipping and separate to obtain filtering residue；Finally filtering residue obtained above is poured into its volume 8
Times concentration is in 2mol/L salpeter solution, puts into sonic oscillation instrument, with 200W power ultrasonic oscillation treatment 6h under the conditions of 75 DEG C,
And with deionized water drip washing until leacheate is neutrality, put into baking oven at 105 DEG C, be dried discharging after 8h, obtain modified biomass
Carbon catalyst support.
This example operation is easy, and the modified biomass carbon catalyst support specific surface area prepared is up to 715m2g-1, pore size is
28nm, mesopore volume is 0.2mg/L, and intensity is 8.0N/mm；During use, weigh 5g silver nitrate, 8g nickel nitrate is placed in 200mL and goes
In ionized water, stirring, the modified biomass carbon catalyst support present invention prepared afterwards is put into wherein, soaks
8h, filters to obtain precipitation, moves in Muffle furnace, calcines 3h, treats that calcining terminates, i.e. can get nickel-base catalyst, through inspection at 600 DEG C
Surveying, the nickel-base catalyst prepared is compared with traditional catalyst, and catalysis activity improves 30%, and catalytic efficiency improves 40%, additionally urges
The change life-span is 1 times for the traditional catalyst life-span, has broad application prospects.
Example 2
First the Limax selecting more than 40 body weight 15g is put in the beaker equipped with the deep deionized water of 2cm of the bottom, then drips 20mL
Oleum Camelliae, puts in 30 DEG C of water-baths by beaker, stands and makes Limax tell dirty blowdown 5 days；Then the Limax after above-mentioned blowdown is taken
Going out, artificial broken shell also takes out the Limax internal organs loading conical flask with agitator, adds Limax internal organs cumulative volume 8 times 25 in bottle
DEG C deionized water, start agitator with 600r/min rotating speed stir process 5h；Stirring is filtered to separate after terminating and is removed filtering residue, will
Filtrate loads high speed centrifuge, is centrifuged 18min with 12000r/min rotating speed, separates and removes lower sediment, obtains supernatant, i.e. certainly
Modification liquid processed, puts in 5 DEG C of ice-water baths and saves backup；Next weigh 250g Bombyx bombycis to put into buchner funnel and use dehydrated alcohol successively
With deionized water filtering and washing 15min, the fragment of 2cm will be cut into after the cocoon drying after washing, then Bombyx bombycis fragment is put into charcoal
Changing in stove, be passed through argon as protection gas, at 850 DEG C, discharging after insulation calcining 3h, obtains Bombyx bombycis base biological carbon carrier crude product；So
After Bombyx bombycis base biological carbon carrier crude product obtained above for 45g is poured in the ceramic pot with 350mL standby self-control modification liquid, put
Enter in the calorstat of 35 DEG C, filter after the modified 11h of dipping and separate to obtain filtering residue；Finally filtering residue obtained above is poured into its volume 9
Times concentration is in 2mol/L salpeter solution, puts into sonic oscillation instrument, with 250W power ultrasonic oscillation treatment 7h under the conditions of 80 DEG C,
And with deionized water drip washing until leacheate is neutrality, put into baking oven at 108 DEG C, be dried discharging after 9h, obtain modified biomass
Carbon catalyst support.
This example operation is easy, and the modified biomass carbon catalyst support specific surface area prepared is up to 715m2g-1, pore size is
28nm, mesopore volume is 0.2mg/L, and intensity is 8.0N/mm；During use, weigh 5.5g silver nitrate, 9g nickel nitrate is placed in 250mL
In deionized water, stirring, the modified biomass carbon catalyst support present invention prepared afterwards is put into wherein, soaks
9h, filters to obtain precipitation, moves in Muffle furnace, calcines 3.5h, treat that calcining terminates, i.e. can get nickel-base catalyst, warp at 700 DEG C
Detection, prepare nickel-base catalyst compared with traditional catalyst, catalysis activity improve 31%, catalytic efficiency improve 43%, additionally
1.5 times that catalytic life is the traditional catalyst life-span, have broad application prospects.
Example 3
First the Limax selecting more than 40 body weight 15g is put in the beaker equipped with the deep deionized water of 2cm of the bottom, then drips 20mL
Oleum Camelliae, puts in 30 DEG C of water-baths by beaker, stands and makes Limax tell dirty blowdown 5 days；Then the Limax after above-mentioned blowdown is taken
Going out, artificial broken shell also takes out the Limax internal organs loading conical flask with agitator, adds Limax internal organs cumulative volume 8 times 25 in bottle
DEG C deionized water, start agitator with 600r/min rotating speed stir process 5h；Stirring is filtered to separate after terminating and is removed filtering residue, will
Filtrate loads high speed centrifuge, is centrifuged 20min with 12000r/min rotating speed, separates and removes lower sediment, obtains supernatant, i.e. certainly
Modification liquid processed, puts in 6 DEG C of ice-water baths and saves backup；Next weigh 300g Bombyx bombycis to put into buchner funnel and use dehydrated alcohol successively
With deionized water filtering and washing 20min, the fragment of 3cm will be cut into after the cocoon drying after washing, then Bombyx bombycis fragment is put into charcoal
Changing in stove, be passed through argon as protection gas, at 900 DEG C, discharging after insulation calcining 4h, obtains Bombyx bombycis base biological carbon carrier crude product；So
After Bombyx bombycis base biological carbon carrier crude product obtained above for 50g is poured in the ceramic pot with 400mL standby self-control modification liquid, put
Enter in the calorstat of 40 DEG C, filter after the modified 12h of dipping and separate to obtain filtering residue；Finally filtering residue obtained above is poured into its volume 10
Times concentration is in 2mol/L salpeter solution, puts into sonic oscillation instrument, with 300W power ultrasonic oscillation treatment 8h under the conditions of 85 DEG C,
And with deionized water drip washing until leacheate is neutrality, put into baking oven at 110 DEG C, be dried discharging after 10h, obtain modification biological
Matter carbon catalyst support.
This example operation is easy, and the modified biomass carbon catalyst support specific surface area prepared is up to 715m2g-1, pore size is
28nm, mesopore volume is 0.2mg/L, and intensity is 8.0N/mm；During use, weigh 6g silver nitrate, 10g nickel nitrate is placed in 300mL and goes
In ionized water, stirring, the modified biomass carbon catalyst support present invention prepared afterwards is put into wherein, soaks
10h, filters to obtain precipitation, moves in Muffle furnace, calcines 4h, treat that calcining terminates, i.e. can get nickel-base catalyst, warp at 800 DEG C
Detection, prepare nickel-base catalyst compared with traditional catalyst, catalysis activity improve 32%, catalytic efficiency improve 45%, additionally
2 times that catalytic life is the traditional catalyst life-span, have broad application prospects.
Claims (1)
1. the preparation method of a modified biomass carbon catalyst support, it is characterised in that concrete preparation process is:
(1) Limax selecting more than 30～40 body weight 15g is put in the beaker equipped with 1～2cm deep deionized water of the bottom, then drips
Add 15～20mL Oleum Camelliae, beaker is put in 20～30 DEG C of water-baths, stand and make Limax tell dirty blowdown 3～5 days；
(2) being taken out by the Limax after above-mentioned blowdown, artificial broken shell also takes out the Limax internal organs loading conical flask with agitator, to
Add the deionized water of Limax internal organs cumulative volume 5～8 times 20～25 DEG C in Ping, start agitator with 500～600r/min rotating speeds
Stir process 3～5h；
(3) filter after stirring terminates to separate and remove filtering residue, filtrate is loaded high speed centrifuge, turns with 10000～12000r/min
Speed centrifugal 15～20min, separates and removes lower sediment, obtain supernatant, i.e. make modification liquid by oneself, puts in 4～6 DEG C of ice-water baths and protects
Deposit standby；
(4) weigh 200～300g Bombyx bombycis put into buchner funnel successively by dehydrated alcohol and deionized water filtering and washing 10～
20min, will be cut into the fragment of 1～3cm, then puts in retort by Bombyx bombycis fragment, be passed through argon after the cocoon drying after washing
As protection gas, at 800～900 DEG C, discharging after insulation calcining 2～4h, obtains Bombyx bombycis base biological carbon carrier crude product；
(5) 40～50g Bombyx bombycis base biological carbon carrier crude products obtained above are poured into 300～400mL standby self-control modifications
In the ceramic pot of liquid, put in the calorstat of 30～40 DEG C, filter after dipping modified 10～12h and separate to obtain filtering residue；
(6) filtering residue obtained above is poured into its volume 8～10 times of concentration are in 2mol/L salpeter solution, put into sonic oscillation
Instrument, with 200～300W power ultrasonic oscillation treatment 6～8h under the conditions of 75～85 DEG C, and with deionized water drip washing until drip washing
Liquid is neutrality, puts into discharging after baking oven is dried 8～10h at 105～110 DEG C, obtains modified biomass carbon catalyst support.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610492241.1A CN106040313A (en) | 2016-06-29 | 2016-06-29 | Preparation method of modified biomass carbon catalyst carrier |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610492241.1A CN106040313A (en) | 2016-06-29 | 2016-06-29 | Preparation method of modified biomass carbon catalyst carrier |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106040313A true CN106040313A (en) | 2016-10-26 |
Family
ID=57166044
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610492241.1A Pending CN106040313A (en) | 2016-06-29 | 2016-06-29 | Preparation method of modified biomass carbon catalyst carrier |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106040313A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103252214A (en) * | 2013-05-21 | 2013-08-21 | 济南大学 | Active carbon fiber and graded porous Ni-Ni3P/active carbon fiber composite material as well as preparation and application of two |
| CN104560931A (en) * | 2015-02-16 | 2015-04-29 | 曾丽娟 | Extraction method of glusulase |
| CN105502383A (en) * | 2015-11-30 | 2016-04-20 | 北京化工大学 | Silkworm cocoon-based hierarchical porous carbon and preparation method thereof |
-
2016
- 2016-06-29 CN CN201610492241.1A patent/CN106040313A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103252214A (en) * | 2013-05-21 | 2013-08-21 | 济南大学 | Active carbon fiber and graded porous Ni-Ni3P/active carbon fiber composite material as well as preparation and application of two |
| CN104560931A (en) * | 2015-02-16 | 2015-04-29 | 曾丽娟 | Extraction method of glusulase |
| CN105502383A (en) * | 2015-11-30 | 2016-04-20 | 北京化工大学 | Silkworm cocoon-based hierarchical porous carbon and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103771407B (en) | Take biomass power plant ash as the method that super-activated carbon prepared by raw material | |
| CN103406105B (en) | A kind of modified abandoned tealeaf residue adsorbent, preparation method and application | |
| CN103710158B (en) | Method for producing biodiesel by using kitchen wastes | |
| CN107601502A (en) | The preparation and the application in terms of capacitive property of a kind of nitrogen phosphorus doping porous charcoal | |
| CN112010302A (en) | Method for preparing hierarchical porous phosphorus-doped carbon material from biomass | |
| CN107673365A (en) | Produce the ripple cleavage method of modified zeolite | |
| CN104107705A (en) | Solid base catalyst for preparing biodiesel | |
| CN103623618B (en) | A kind of take quartz sand as the preparation method of the Hydrophobic filter material of carrier | |
| Balajii et al. | Ultrasound-assisted biodiesel production from Ceiba pentandra oil using Musa spp Nendran banana peduncle derived heterogeneous catalyst | |
| CN107488519B (en) | Method for preparing biodiesel by catalyzing restaurant waste oil through magnetic carbon loaded acid-base | |
| CN102513081B (en) | Alkaline catalytic membrane and preparation method thereof | |
| CN103301811A (en) | preparation method of biomass charcoal adsorbent and method for treating oily wastewater by biomass charcoal adsorbent | |
| CN106000436A (en) | Preparation method of heterogeneous catalyst with camphor tree ash as carrier and application thereof | |
| CN106040313A (en) | Preparation method of modified biomass carbon catalyst carrier | |
| CN107335418A (en) | Novel hollow TiO2Preparation method of nano cup catalyst and application of nano cup catalyst after metal loading | |
| CN116440866B (en) | Preparation method and application of three-dimensional spongy porous heavy metal ion adsorbent based on activated eggshells | |
| CN102259874A (en) | Method for preparing white carbon black by continuous carbon precipitation | |
| CN106145380A (en) | A kind of biologically active charing stalk/diatomite molecular sieve demanganization filtrate | |
| CN101780415A (en) | Coal cinder supported solid base catalyst and preparation method and use thereof | |
| CN206359492U (en) | Single variety waste lubricant oil regeneration system | |
| CN111250045B (en) | H2SO4Preparation method of modified granular anthracite and H2SO4Modified granular anthracite and application thereof | |
| CN112938968A (en) | Method for producing activated carbon by using furfural residues | |
| CN107099380A (en) | A kind of preparation method of biodiesel | |
| KR102519758B1 (en) | Method for producing biodiesel from biomass | |
| CN109111994B (en) | KOH-K2CO3-Al2O3Method for preparing biodiesel by catalyzing cottonseed oil with solid mixed base |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161026 |