CN109759023A - A kind of pumpkin base contains TiO2The preparation method of charcoal-aero gel - Google Patents
A kind of pumpkin base contains TiO2The preparation method of charcoal-aero gel Download PDFInfo
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- CN109759023A CN109759023A CN201910065106.2A CN201910065106A CN109759023A CN 109759023 A CN109759023 A CN 109759023A CN 201910065106 A CN201910065106 A CN 201910065106A CN 109759023 A CN109759023 A CN 109759023A
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- pumpkin
- charcoal
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- aero gel
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Abstract
The present invention provides a kind of pumpkin bases to contain TiO2The preparation method of charcoal-aero gel, Step 1: pumpkin is cleaned and is cut into pumpkin fritter;Step 2: pumpkin fritter is put into reaction kettle, heat up to obtain pumpkin base charcoal wet gel block;Step 3: cleaning solution cleans pumpkin base charcoal wet gel block, it is put into freezing chamber and freezes after cleaning;Step 4: being freeze-dried in freeze drier, pumpkin based charcoal aerogel is obtained;Step 5: pumpkin based charcoal aerogel is put into addition organotitanium precursor body mixed liquor in roller tank;Step 6: sour mixed solution is added into roller tank;Step 7: being centrifugated after cleaning;Step 8: dry pumpkin base containing TiO2Charcoal-aero gel.Present invention load nano-titanium dioxide on the pumpkin based charcoal aerogel being prepared using organotitanium precursor body, preparation method is simple, and load is secured.
Description
Technical field
The invention belongs to charcoal-aero gel preparation fields, and in particular to a kind of pumpkin base contains TiO2The preparation side of charcoal-aero gel
Method.
Background technique
Charcoal-aero gel is a kind of agraphitic carbon cellulosic material of novel light nanoporous, the charcoal-aero gel porosity prepared
Height, and its foam structure can be by process adjustments, and its preparation process is also relatively simple, in terms of have compared with
Big application value.The existing method for preparing cellulose base charcoal-aero gel mostly uses prepare cellulose gas-gel after, directly
The adsorptivity of high temperature pyrolysis under an inert atmosphere, the charcoal-aero gel of this method preparation is stronger, but its intensity is weaker, and after absorption
Absorption weight it is bigger, require the bond strengths of charcoal-aero gel interior molecules higher, and the method system of directly high temperature pyrolysis
Intensity inside standby charcoal-aero gel is insufficient.Pumpkin is cheap, and abundance belongs to renewable raw materials, can be used as charcoal airsetting
The raw material sources of glue have good Development volue.
Nano-titanium dioxide has good dispersibility and a weatherability, and the sterilizing function based on nano-titanium dioxide, anti-
Ultraviolet light function and photo-catalysis function, nano-titanium dioxide are widely used in anti-ultraviolet material, textile industry, photocatalysis catalyst
In equal fields.There is the disadvantages of difficult separation, easy in inactivation in nano-titanium dioxide powder suspension, be not easy to two in application process
The recycling of titanium oxide and sustainable utilization.
Summary of the invention
To solve the above problems, the present invention provides a kind of pumpkin base containing TiO2The preparation method of charcoal-aero gel, in pumpkin base
Load nano-titanium dioxide on charcoal-aero gel, preparation method is simple, and load is secured.
To achieve the goals above, the technical solution adopted by the present invention are as follows:
A kind of pumpkin base contains TiO2The preparation method of charcoal-aero gel, it is characterised in that: specific steps are as follows:
Step 1: pumpkin is cleaned and is cut into pumpkin fritter;
Step 2: the pumpkin fritter after step 1 is cleaned is put into reaction kettle, the south of distillation water immersion is added in reaction kettle
It is sealed after melon fritter, 180 DEG C is warming up in reaction kettle, the reaction time is 10 ~ 14h, takes out after reaction, it is wet to obtain pumpkin base charcoal
Gel mass;
Step 3: the pumpkin base charcoal wet gel block with two gained pumpkin base charcoal wet gel block of cleaning solution cleaning step, after cleaning
Body is also put into freezing chamber and freezes;
Step 4: the pumpkin base charcoal wet gel block after step 3 is freezed is freeze-dried in freeze drier, pumpkin base is obtained
Charcoal-aero gel;
Step 5: pumpkin based charcoal aerogel obtained by step 4 is put into roller tank, under roller tank rotary state, by organic titanium
Presoma mixed liquor is added into roller tank, is totally submerged the pumpkin based charcoal aerogel in roller tank mixed in organotitanium precursor body
It closes in liquid, roller tank continues to rotate 20 ~ 40min after addition;
Step 6: sour mixed solution is added into roller tank, 18 ~ 24 h are kept at 140 ~ 160 DEG C after rotation mixing, are cooled to room
Temperature;
Step 7: respectively being cleaned 2 ~ 4 times with distilled water and dehydrated alcohol, it is centrifugated after cleaning every time;
Step 8: drying in 35 ~ 50 DEG C of baking ovens, pumpkin base is obtained containing TiO2Charcoal-aero gel.
Further, in step 1, the pumpkin after cleaning removes epidermis and capsula interna and is cut into pumpkin fritter, and pumpkin fritter is again
Wash with distilled water.
Further, in step 3, cleaning solution is the mixed liquor of dehydrated alcohol and water, and the volume ratio of dehydrated alcohol and water is
1:1。
Further, the pumpkin base charcoal wet gel block in step 3 pays off that be washed till mixed liquor transparent, and pumpkin base charcoal is wet solidifying
Cooling time of the blob of viscose body in freezing chamber is 10 ~ 14h, and cryogenic temperature is -50 ~ -30 DEG C.
Further, the temperature being freeze-dried in step 4 is -50 DEG C, vacuum degree < 20 Pa.
Further, in step 5, organotitanium precursor body mixed liquor includes organic titanium precursors and dehydrated alcohol, organic titanium
The volume ratio of presoma and dehydrated alcohol is 1:1 ~ 1:2.
Further, the organotitanium precursor body is tetrabutyl titanate ester.
Further, the sour mixed solution includes the acid and dehydrated alcohol mixed in equal volume, the acid be glacial acetic acid or
One of hydrochloric acid.
Further, the volume ratio of the sour mixed solution and organotitanium precursor body mixed liquor is 1 ~ 3.
Further, the roller tank includes cylinder closed at both ends and the rotating circular disk being set on cylinder, cylinder
Central axis is horizontally disposed, and pumpkin based charcoal aerogel is also placed in the inside of the cylinder;One end of the cylinder connects
In the rotating disk of rotating circular disk, the central axes of rotating disk and the central axes of cylinder coincide, and cylinder follows rotating circular disk to do rotation
Movement;The other end of cylinder is reserved for the inlet that organotitanium precursor body mixed liquor and sour mixed solution enter, the inlet
Input duct is also connected by valve;The side wall of cylinder is also reserved for the material hole of pumpkin based charcoal aerogel blowing and discharging, described
To expect to be equipped with bin gate at hole, the side of bin gate is articulated at the material hole, and when bin gate is closed, the bin gate covers the material hole,
The other end of bin gate is also fixed by bolts on the side wall of cylinder, is additionally provided with gasket between the bin gate and material hole, described
Bin gate and the cylinder also constitute closed tubular.
The invention has the benefit that
1, a kind of pumpkin base of the invention contains TiO2The preparation method of charcoal-aero gel prepares pumpkin based charcoal aerogel using pumpkin,
Pumpkin belongs to renewable resource, using pumpkin biomass as raw material, prepares biomass carbon aeroge using low-temperature carbonization method, have at
Originally the advantages such as cheap, environmental-friendly;
2, the present invention loads TiO on pumpkin based charcoal aerogel using organotitanium precursor body2, charcoal-aero gel, which has to adsorb by force, to be made
With the pumpkin base of preparation contains TiO2The Load Balanced of charcoal-aero gel, organotitanium precursor body also in roller tank with pumpkin base charcoal gas
Gel mixes, and can be avoided charcoal-aero gel and is wrapped on conventional blender, and then prevents convention stir device to load effect
Influence and damage to mixing plant.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of roller tank;
Fig. 2 is the structural schematic diagram of cylinder.
Wherein, each label in figure are as follows: 1, cylinder;2, rotating circular disk;3, pumpkin based charcoal aerogel;4, inlet;5, feed liquor
Pipeline;6, expect hole;7, bin gate;8, bolt.
Specific embodiment
Embodiment 1
A kind of pumpkin base contains TiO2The preparation method of charcoal-aero gel prepares pumpkin based charcoal aerogel, pumpkin base by raw material of pumpkin
The preparation of charcoal-aero gel: it will be cut into about 1 cm × 1cm × 1cm fritter after the pumpkin removal epidermis and capsula interna after cleaning, with steaming
Distilled water washs 10min, appropriate pumpkin fritter is put into the stainless steel cauldron that liner is polytetrafluoroethylene (PTFE), with distillation water immersion
It after pumpkin block, is sealed at 180 DEG C and reacts 12h, take out after reaction, obtain pumpkin base charcoal wet gel block;With anhydrous second
Until mixed liquor (volume ratio 1: 1) the cleaning block to mixed liquor clear of alcohol and water.Then block is put into refrigerator
Freeze 12 h;Finally, block is put into drying in freeze drier (temperature is -50 DEG C, vacuum degree < 20 Pa), south can be obtained
Melon based charcoal aerogel 3.
Pumpkin base contains TiO2The preparation of charcoal-aero gel: opening bin gate 7, and pumpkin based charcoal aerogel 3 is led to material path and is packed into rolling
In the cylinder 1 of canister, pumpkin based charcoal aerogel 3 is distributed in 20 mL dehydrated alcohols, is slowly added dropwise and ethyl alcohol equivalent thereto
Tetrabutyl titanate ester, start rotating circular disk 2, rotating circular disk 2 drive cylinder 1 rotate 20min after, by input duct 5 and into
20mL dehydrated alcohol and 20mL glacial acetic acid is added in liquid mouth 4, keeps 18h at 140 DEG C after being transferred to roller tank, is cooled to room temperature, and uses
Distilled water and dehydrated alcohol respectively clean 2 times, and centrifuge separation is dried in 35 DEG C of baking oven, can be prepared by pumpkin base containing TiO2Charcoal
Aeroge.
Embodiment 2
A kind of pumpkin base contains TiO2The preparation method of charcoal-aero gel prepares pumpkin based charcoal aerogel, pumpkin base by raw material of pumpkin
The preparation of charcoal-aero gel: it will be cut into about 2cm × 2cm × 2cm fritter after the pumpkin removal epidermis and capsula interna after cleaning, with distillation
Appropriate pumpkin fritter is put into the stainless steel cauldron that liner is polytetrafluoroethylene (PTFE) by water washing 10min, with distillation water immersion south
It after melon block, is sealed at 180 DEG C and reacts 13h, take out after reaction, obtain pumpkin base charcoal wet gel block;Use dehydrated alcohol
Until cleaning block to mixed liquor clear with the mixed liquor (volume ratio 1: 1) of water.Then block is put into cold in refrigerator
Freeze 12 h;Finally, block is put into drying in freeze drier (temperature is -50 DEG C, vacuum degree < 20 Pa), pumpkin can be obtained
Based charcoal aerogel 3.
Pumpkin base contains TiO2The preparation of charcoal-aero gel: opening bin gate 7, and pumpkin based charcoal aerogel 3 is led to material path and is packed into rolling
In the cylinder 1 of canister, pumpkin based charcoal aerogel 3 is distributed in 20 mL dehydrated alcohols, four fourths of 10mL are slowly added dropwise thereto
Base titanate esters start rotating circular disk 2, after rotating circular disk 2 drives cylinder 1 to rotate 30min, are added by input duct 5 and inlet 4
Enter 10mL dehydrated alcohol and 10mL hydrochloric acid, the mass fraction of hydrochloric acid is 37%, and 20 h are kept at 150 DEG C after being transferred to roller tank, cold
But it to room temperature, is respectively cleaned 3 times with distilled water and dehydrated alcohol, is centrifugated, is dried in 40 DEG C of baking oven, can be prepared by pumpkin
Base contains TiO2Charcoal-aero gel.
Embodiment 3
A kind of pumpkin base contains TiO2The preparation method of charcoal-aero gel prepares pumpkin based charcoal aerogel, pumpkin base by raw material of pumpkin
The preparation of charcoal-aero gel: it will be cut into about 1 cm × 1cm × 1cm fritter after the pumpkin removal epidermis and capsula interna after cleaning, with steaming
Distilled water washs 10min, appropriate pumpkin fritter is put into the stainless steel cauldron that liner is polytetrafluoroethylene (PTFE), with distillation water immersion
It after pumpkin block, is sealed at 180 DEG C and reacts 14h, take out after reaction, obtain pumpkin base charcoal wet gel block;With anhydrous second
Until mixed liquor (volume ratio 1: 1) the cleaning block to mixed liquor clear of alcohol and water.Then block is put into refrigerator
Freeze 12 h;Finally, block is put into drying in freeze drier (temperature is -50 DEG C, vacuum degree < 20 Pa), south can be obtained
Melon based charcoal aerogel 3.
Pumpkin base contains TiO2The preparation of charcoal-aero gel: opening bin gate 7, and pumpkin based charcoal aerogel 3 is led to material path and is packed into rolling
In the cylinder 1 of canister, pumpkin based charcoal aerogel 3 is distributed in 20 mL dehydrated alcohols, is slowly added dropwise and ethyl alcohol equivalent thereto
Tetrabutyl titanate ester, start rotating circular disk 2, after rotating circular disk 2 rotates 40 min, pass through input duct 5 and inlet 4 and be added
20mL dehydrated alcohol and 10mL glacial acetic acid keep 24 h after being transferred to roller tank at 160 DEG C, are cooled to room temperature, with distilled water and
Dehydrated alcohol alternately cleaning 4 times, centrifuge separation are dried in 50 DEG C of baking oven, can be prepared by pumpkin base containing TiO2Charcoal-aero gel.
Roller tank can be avoided pumpkin based charcoal aerogel 3 with blender is twined in organotitanium precursor body blending process
Around avoiding the stacking of pumpkin based charcoal aerogel 3 and the damage to blender, the bin gate 7 on cylinder 1 is also cut with scissors by hinge or shaft
It being connected on the cylindrical wall around material hole 6, gasket is fixed on bin gate 7 or expects around hole 6, when covering bin gate 7, gasket
Also between cylinder 1 and bin gate 7, the liquid leakage in cylinder 1 is prevented.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
The present invention will not be limited to the embodiments shown herein, and is to fit to special with principles disclosed herein and novelty
The consistent widest scope of point.
Claims (10)
1. a kind of pumpkin base contains TiO2The preparation method of charcoal-aero gel, it is characterised in that: specific steps are as follows:
Step 1: pumpkin is cleaned and is cut into pumpkin fritter;
Step 2: the pumpkin fritter after step 1 is cleaned is put into reaction kettle, the south of distillation water immersion is added in reaction kettle
It is sealed after melon fritter, 180 DEG C is warming up in reaction kettle, the reaction time is 10 ~ 14h, takes out after reaction, it is wet to obtain pumpkin base charcoal
Gel mass;
Step 3: the pumpkin base charcoal wet gel block with two gained pumpkin base charcoal wet gel block of cleaning solution cleaning step, after cleaning
Body is also put into freezing chamber and freezes;
Step 4: the pumpkin base charcoal wet gel block after step 3 is freezed is freeze-dried in freeze drier, pumpkin base is obtained
Charcoal-aero gel;
Step 5: pumpkin based charcoal aerogel obtained by step 4 is put into roller tank, under roller tank rotary state, by organic titanium
Presoma mixed liquor is added into roller tank, is totally submerged the pumpkin based charcoal aerogel in roller tank mixed in organotitanium precursor body
It closes in liquid, roller tank continues to rotate 20 ~ 40min after addition;
Step 6: sour mixed solution is added into roller tank, 18 ~ 24 h are kept at 140 ~ 160 DEG C after rotation mixing, are cooled to room
Temperature;
Step 7: respectively being cleaned 2 ~ 4 times with distilled water and dehydrated alcohol, it is centrifugated after cleaning every time;
Step 8: drying in 35 ~ 50 DEG C of baking ovens, pumpkin base is obtained containing TiO2Charcoal-aero gel.
2. a kind of pumpkin base according to claim 1 contains TiO2The preparation method of charcoal-aero gel, it is characterised in that: step 1
In, pumpkin after cleaning removal epidermis and capsula interna are simultaneously cut into pumpkin fritter, and pumpkin fritter is again wash with distilled water.
3. a kind of pumpkin base according to claim 1 contains TiO2The preparation method of charcoal-aero gel, it is characterised in that: step 3
In, cleaning solution is the mixed liquor of dehydrated alcohol and water, and the volume ratio of dehydrated alcohol and water is 1:1.
4. a kind of pumpkin base according to claim 3 contains TiO2The preparation method of charcoal-aero gel, it is characterised in that: step 3
In pumpkin base charcoal wet gel block pay off and be washed till that mixed liquor is transparent, when freezing of the pumpkin base charcoal wet gel block in freezing chamber
Between be 10 ~ 14h, cryogenic temperature be -50 ~ -30 DEG C.
5. a kind of pumpkin base according to claim 1 contains TiO2The preparation method of charcoal-aero gel, it is characterised in that: step 4
The temperature of middle freeze-drying is -50 DEG C, vacuum degree < 20 Pa.
6. a kind of pumpkin base according to claim 1 contains TiO2The preparation method of charcoal-aero gel, it is characterised in that: step 5
In, organotitanium precursor body mixed liquor includes organic titanium precursors and dehydrated alcohol, the volume of organotitanium precursor body and dehydrated alcohol
Than for 1:1 ~ 1:2.
7. a kind of pumpkin base according to claim 1 or 6 contains TiO2The preparation method of charcoal-aero gel, it is characterised in that: described
Organotitanium precursor body is tetrabutyl titanate ester.
8. a kind of pumpkin base according to claim 1 contains TiO2The preparation method of charcoal-aero gel, it is characterised in that: the acid
Mixed solution includes the acid and dehydrated alcohol mixed in equal volume, and the acid is one of glacial acetic acid or hydrochloric acid.
9. a kind of pumpkin base according to claim 8 contains TiO2The preparation method of charcoal-aero gel, it is characterised in that: the acid
The volume ratio of mixed solution and organotitanium precursor body mixed liquor is 1 ~ 3.
10. a kind of pumpkin base according to claim 1 contains TiO2The preparation method of charcoal-aero gel, it is characterised in that: the rolling
Canister includes cylinder and the rotating circular disk being set on cylinder closed at both ends, and the central axis of cylinder is horizontally disposed, south
Melon based charcoal aerogel is also placed in the inside of the cylinder;One end of the cylinder is connected to the rotating disk of rotating circular disk, rotation
The central axes of disk and the central axes of cylinder coincide, and cylinder follows rotating circular disk to do rotation movement;The other end of cylinder is reserved for
The inlet that organotitanium precursor body mixed liquor and sour mixed solution enter, the inlet also pass through valve and connect input duct;
The side wall of cylinder is also reserved for the material hole of pumpkin based charcoal aerogel blowing and discharging, is equipped with bin gate at the material hole, and the one of bin gate
Side is articulated at the material hole, and when bin gate is closed, the bin gate covers the material hole, and the other end of bin gate is also solid by bolt
Due on the side wall of cylinder, gasket is additionally provided between the bin gate and material hole, the bin gate and the cylinder also constitute closing
Tubular.
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CN106390970A (en) * | 2015-07-31 | 2017-02-15 | 镇江华科生态电镀科技发展有限公司(外商独资) | Method for preparing titanium dioxide loaded biomass carbon aerogel material |
CN107684886A (en) * | 2017-09-29 | 2018-02-13 | 华纺股份有限公司 | One kind doping TiO2The compound carbon aerogels of cotton fiber preparation method |
CN108355485A (en) * | 2018-02-10 | 2018-08-03 | 黄旭东 | A kind of preparation method of air purification solid carbon dioxide material |
CN108816259A (en) * | 2018-06-12 | 2018-11-16 | 石狮市川大先进高分子材料研究中心 | A kind of compound carbon aerogels of titanium dioxide load-type and its preparation and application |
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2019
- 2019-01-23 CN CN201910065106.2A patent/CN109759023A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8664143B2 (en) * | 2009-01-27 | 2014-03-04 | Lawrence Livermore National Security, Llc. | High surface area, electrically conductive nanocarbon-supported metal oxide |
CN106390970A (en) * | 2015-07-31 | 2017-02-15 | 镇江华科生态电镀科技发展有限公司(外商独资) | Method for preparing titanium dioxide loaded biomass carbon aerogel material |
CN107684886A (en) * | 2017-09-29 | 2018-02-13 | 华纺股份有限公司 | One kind doping TiO2The compound carbon aerogels of cotton fiber preparation method |
CN108355485A (en) * | 2018-02-10 | 2018-08-03 | 黄旭东 | A kind of preparation method of air purification solid carbon dioxide material |
CN108816259A (en) * | 2018-06-12 | 2018-11-16 | 石狮市川大先进高分子材料研究中心 | A kind of compound carbon aerogels of titanium dioxide load-type and its preparation and application |
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