CN109092246A - A kind of preparation method of porous carbon adsorbing material - Google Patents
A kind of preparation method of porous carbon adsorbing material Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
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Abstract
The invention discloses a kind of preparation methods of porous carbon adsorbing material, belong to porous material technical field.After modified gel to be kept the temperature to 1~2h of charing under nitrogen atmosphere, obtain porous carbon adsorbing material blank, porous carbon adsorbing material blank and water 1:10~1:15 in mass ratio are mixed in flask, and with mass fraction be 20~28% sodium hydroxide solution adjust flask in material pH to 9~10, after being standing and soaking 8~12h under room temperature, filtering obtains filter residue, under conditions of being 60~80 DEG C in temperature by filter residue after dry 2~3h, porous carbon adsorbing material is obtained.The porous carbon adsorbing material of technical solution of the present invention preparation has the characteristics that porosity height and excellent compressive property, has broad prospects in the development of porous material technology industry.
Description
Technical field
The invention discloses a kind of preparation methods of porous carbon adsorbing material, belong to porous material technical field.
Background technique
Porous material is a kind of by being mutually communicated or the hole of envelope constitutes the material of network structure.Porous material is in nature
Generally existing such as timber, cork, sponge and coral in boundary, over the past thousands of years, these natural porous materials are sharp extensively by people
With.For opposite continuous media material, porous material generally has many advantages, such as that relative density is low, specific strength is high, specific surface area is high.
Therefore, porous material is widely used in the fields such as ion exchange, absorption and separation, energy storage and conversion.Porous material mesoporous
The size of gap, quantity, distribution are to influence the principal element of porous material performance.
Porous carbon materials due to its high-specific surface area, the characteristics such as flourishing, good, acid and alkali-resistance of chemical stability of pore structure with
And excellent electrical and thermal conductivity and biocompatibility and by extensive research and application.It is usually used in preparing nanoporous carbon at present,
Especially the process with meso-hole structure mainly includes activation method (including physically activated and chemical activation), template (packet
Include hard template and soft template), catalytic activation method, mixed with polymers carbonizatin method and organic gel carbonization method etc..Activation method can obtain
The porous carbon of high specific surface area is obtained, but poor to the regulating power in aperture；Template, which can obtain duct by duplication template, to be had
Sequence, uniform carbon material, but the porous carbon specific surface area obtained is generally relatively low, template is expensive, significantly limits the technique
Large-scale application.Other several methods, which are also difficult to, not only obtains high specific area carbon, but also can carry out to hole and microstructure
It effectively adjusts, therefore is difficult to meet growing application demand.
And traditional porous carbon adsorbing material the problem of there is also porosity is low and compression strength can not further increase, because
This, the shortcomings that water resistance and adhesion strength for how improving conventional porous carbon adsorbing material can not further increase, in the hope of visiting
It is problem to be solved that rope, which develops the porous carbon adsorbing material with good comprehensive performance,.
Summary of the invention
The present invention solves the technical problem of: for conventional porous carbon adsorbing material porosity is low and compression strength without
The shortcomings that method further increases provides a kind of preparation method of porous carbon adsorbing material.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of porous carbon adsorbing material, specific preparation step are as follows:
(1) polyallylamine hydrochlorides are mixed with water 1:100~1:110 in mass ratio, after being stirred, adjusting pH to 9.8~
10.0, polyallylamine hydrochlorides solution is obtained, under intense agitation, by modified glucose mixed liquor and polyallylamine hydrochlorides
Liquor capacity ratio 1:8~1:10 mixing, after being stirred to react, obtains polyallylamine hydrochlorides-modified glucose mixed liquor；
(2) polyallylamine hydrochlorides-modified glucose mixed liquor is mixed with sodium borohydride 200:1~250:1 in mass ratio, is stirred
After mixing reaction, gel mixture is obtained, gel mixture is dialysed, it is dry, obtain gel；
(3) gel is mixed with ethyl acetate 1:10~1:15 in mass ratio, and 0.2~0.4 times of gel quality of positive silicon is added
Acetoacetic ester, the organo-aluminium and 0.08~0.10 times of gel quality of potassium hydroxide that 0.1~0.2 times of gel quality, after being stirred,
Ultrasonic disperse obtains gel dispersion liquid, and gel dispersion liquid is mixed with fatty acid 20:1~20:2 in mass ratio, and gel point is added
The immobilized lipase that 0.01~0.02 times of dispersion liquid quality after being stirred to react, filters, dry, obtains modified gel；
(4) modified gel is carbonized under nitrogen atmosphere, obtains porous carbon adsorbing material blank, by porous carbon adsorbing material blank with
Water 1:10~1:15 in mass ratio mixing, adjusts pH to 9.0~10.5, after being standing and soaking, filters, dry, obtains porous carbon adsorption
Material.
Modified glucose mixed liquor described in step (1) be glucose is mixed with water 1:20~1:25 in mass ratio, and
0.1~0.2 times of glucose quality of Potassiumiodate is added, after being stirred, glucose mixed liquor is obtained, by glucose mixed liquor and chlorine
Change barium solution 1:3~1:5 in mass ratio mixing, filtering obtains filtrate, filtrate and metabisulfite solution 1:3~1:4 in mass ratio are mixed
It closes, filtering obtains modified glucose mixed liquor.
The molecular cut off of bag filter used in step (2) described dialysis is 10000.
Step (3) organo-aluminium is any one in aluminium isopropoxide or aluminium ethylate.
Step (3) fatty acid is lauric acid, any one in myristic acid or palmitinic acid.
Step (4) carbonization temperature is 450~600 DEG C.
The beneficial effects of the present invention are:
The present invention is used when preparing porous carbon adsorbing material to be prepared as raw material using polyallylamine hydrochlorides and modified glucose
Gel, and gel is modified, firstly, there is pH using the gel that polyallylamine hydrochlorides and modified glucose are prepared as raw material
Sensibility, in product preparation process, gel can be expanded, so that the porosity of product is improved in carbonization process, secondly,
After modification, with fatty acid esterification can occur for glucose under the action of immobilized lipase in gel, thus in gel
In uniformly generate moisture, make be added organo-aluminium and ethyl orthosilicate hydrolyze and uniformly filled to expanded gel in the product
Inside, and after modified gel charing, the precipitating of silica and aluminium oxide is formed in the inside of porous carbon adsorbing material blank, is made
The compression strength of product improves, and the glucose after esterification can form richer gas in carbonization process, to make to produce
The porosity of product improves, furthermore, in rear soaking process, aluminium oxide can be partly dissolved, thus in porous carbon adsorbing material blank
The porous silica support construction containing abundant hole is formed, and then further improves the porosity of product, so that producing
The compression strength of product improves.
Specific embodiment
Glucose and water 1:20~1:25 in mass ratio are mixed in beaker, and glucose quality is added into beaker
0.1~0.2 times of Potassiumiodate is 45~65 DEG C in temperature, under conditions of revolving speed is 250~350r/min, it is stirred 100~
After 180min, obtain glucose mixed liquor, by glucose mixed liquor and mass fraction be 15~20% barium chloride solution in mass ratio
1:3~1:5 mixing is 30~45 DEG C in temperature, under conditions of revolving speed is 300~400r/min, is stirred 30~40min
Afterwards, it filters, obtains filtrate, filtrate is mixed with metabisulfite solution 1:3~1:4 in mass ratio that mass fraction is 15~22%, Yu Wen
Degree is 30~45 DEG C, and under conditions of revolving speed is 300~400r/min, after being stirred 30~40min, filtering removes filter cake, obtains
Modified glucose mixed liquor；Polyallylamine hydrochlorides are mixed with water 1:100~1:110 in mass ratio, in temperature be 30~50
DEG C, under conditions of revolving speed is 300~400r/min, after being stirred 30~60min, the hydroxide for being 8~12% with mass fraction
Sodium solution adjusts the pH to 9.8~10.0 of polyallylamine hydrochlorides and aqueous mixtures, polyallylamine hydrochlorides solution is obtained, in revolving speed
Under conditions of 800~1000r/min, by modified glucose mixed liquor and polyallylamine hydrochlorides liquor capacity ratio 1:8~1:
10 mixing are 40~55 DEG C in temperature, under conditions of revolving speed is 300~400r/min, after being stirred to react 1~2h, obtain polyene third
Amine hydrochlorate-modified glucose mixed liquor；In mass ratio by polyallylamine hydrochlorides-modified glucose mixed liquor and sodium borohydride
200:1~250:1 mixing is 30~38 DEG C in temperature, under conditions of revolving speed is 300~320r/min, is stirred to react 2~3h
Afterwards, gel mixture is obtained, gel mixture is dialysed, and under conditions of temperature is 75~85 DEG C, after dry 3~5h, is obtained solidifying
Glue；Gel and ethyl acetate 1:10~1:15 in mass ratio are mixed in three-necked flask, and gel is added into three-necked flask
The ethyl orthosilicate that 0.2~0.4 times of quality, the organo-aluminium that 0.1~0.2 times of gel quality and 0.08~0.10 times of gel quality
Potassium hydroxide, in temperature be 35~50 DEG C, revolving speed be 300~400r/min under conditions of, after being stirred 50~80min, then
Under conditions of frequency is 45~55kHz after 15~30min of ultrasonic disperse, gel dispersion liquid is obtained, by gel dispersion liquid and fat
Acid 20:1~20:2 in mass ratio mixing, and gel dispersion liquid quality is added into the mixture of gel dispersion liquid and fatty acid
0.01~0.02 times of immobilized lipase is 30~38 DEG C in temperature, under conditions of revolving speed is 300~380r/min, stirs
After reacting 1~2h, filtering obtains modified gel blank, by modified gel blank under conditions of temperature is 70 DEG C, vacuum drying 3
After~4h, modified gel is obtained；Modified gel is moved into retort, and nitrogen is passed through with the rate of 30~60mL/min into retort
Gas obtains porous carbon adsorbing material blank, by porous carbon adsorbing material blank and water 1:10 in mass ratio after heat preservation carbonizes 1~2h
~1:15 is mixed in flask, and the sodium hydroxide solution for being 20~28% with mass fraction adjusts the pH to 9.0 of material in flask
~10.5, after being standing and soaking 8~12h under room temperature, filtering obtains filter residue, the condition for being 60~80 DEG C in temperature by filter residue
After 2~3h of lower drying, porous carbon adsorbing material is obtained.The molecular cut off of bag filter used in the dialysis is 10000.It is described organic
Aluminium is any one in aluminium isopropoxide or aluminium ethylate.The fatty acid is lauric acid, any one in myristic acid or palmitinic acid.Institute
Stating carbonization temperature is 450~600 DEG C.
Example 1
Glucose and water 1:25 in mass ratio are mixed in beaker, and 0.2 times of glucose quality of acid iodide is added into beaker
Potassium is 65 DEG C in temperature, under conditions of revolving speed is 350r/min, after being stirred 180min, glucose mixed liquor is obtained, by grape
The barium chloride solution 1:5 in mass ratio that sugared mixed liquor and mass fraction are 20% mix, in temperature be 45 DEG C, revolving speed 400r/
Under conditions of min, after being stirred 40min, filtering obtains filtrate, and the metabisulfite solution that filtrate and mass fraction are 22% is pressed matter
Amount is mixed than 1:4, is 45 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred 40min, is filtered, removal filter
Cake obtains modified glucose mixed liquor；Polyallylamine hydrochlorides are mixed with water 1:110 in mass ratio, in temperature be 50 DEG C, revolving speed
Under conditions of 400r/min, after being stirred 60min, polyallylamine is adjusted with the sodium hydroxide solution that mass fraction is 12%
The pH to 10.0 of hydrochloride and aqueous mixtures, obtains polyallylamine hydrochlorides solution, will under conditions of revolving speed is 1000r/min
Modified glucose mixed liquor is mixed with polyallylamine hydrochlorides liquor capacity ratio 1:10, in temperature be 55 DEG C, revolving speed 400r/
Under conditions of min, after being stirred to react 2h, polyallylamine hydrochlorides-modified glucose mixed liquor is obtained；By polyallylamine hydrochlorides-
Modified glucose mixed liquor is mixed with sodium borohydride 250:1 in mass ratio, is 38 DEG C in temperature, revolving speed is the condition of 320r/min
Under, after being stirred to react 3h, gel mixture is obtained, gel mixture is dialysed, and under conditions of temperature is 85 DEG C, dry 5h
Afterwards, gel is obtained；Gel and ethyl acetate 1:15 in mass ratio are mixed in three-necked flask, and gel is added into three-necked flask
The ethyl orthosilicate that 0.4 times of quality, the organo-aluminium and 0.10 times of gel quality of potassium hydroxide that 0.2 times of gel quality, in temperature
It is 50 DEG C, is ultrasonic disperse under conditions of 55kHz then at frequency after being stirred 80min under conditions of revolving speed is 400r/min
After 30min, gel dispersion liquid is obtained, gel dispersion liquid is mixed with fatty acid 20:2 in mass ratio, and to gel dispersion liquid and rouge
In the mixture of fat acid be added 0.02 times of gel dispersion liquid quality immobilized lipase, in temperature be 38 DEG C, revolving speed 380r/
Under conditions of min, after being stirred to react 2h, filtering obtains modified gel blank, the condition for being 70 DEG C in temperature by modified gel blank
Under, after being dried in vacuo 4h, obtain modified gel；Modified gel is moved into retort, and into retort with the rate of 60mL/min
It is passed through nitrogen, after heat preservation charing 2h, obtains porous carbon adsorbing material blank, by porous carbon adsorbing material blank and water in mass ratio 1:
15 are mixed in flask, and the sodium hydroxide solution for being 28% with mass fraction adjusts the pH to 10.5 of material in flask, in room temperature
Under the conditions of be standing and soaking 12h after, filtering obtains filter residue, under conditions of being 80 DEG C in temperature by filter residue after dry 3h, obtains porous carbon suction
Enclosure material.The molecular cut off of bag filter used in the dialysis is 10000.The organo-aluminium is aluminium isopropoxide.The fatty acid
For lauric acid.The carbonization temperature is 600 DEG C.
Example 2
Glucose and water 1:25 in mass ratio are mixed in beaker, and 0.2 times of glucose quality of acid iodide is added into beaker
Potassium is 65 DEG C in temperature, under conditions of revolving speed is 350r/min, after being stirred 180min, glucose mixed liquor is obtained, by grape
The barium chloride solution 1:5 in mass ratio that sugared mixed liquor and mass fraction are 20% mix, in temperature be 45 DEG C, revolving speed 400r/
Under conditions of min, after being stirred 40min, filtering obtains filtrate, and the metabisulfite solution that filtrate and mass fraction are 22% is pressed matter
Amount is mixed than 1:4, is 45 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred 40min, is filtered, removal filter
Cake obtains modified glucose mixed liquor；Polyallylamine hydrochlorides are mixed with water 1:110 in mass ratio, in temperature be 50 DEG C, revolving speed
Under conditions of 400r/min, after being stirred 60min, polyallylamine is adjusted with the sodium hydroxide solution that mass fraction is 12%
The pH to 10.0 of hydrochloride and aqueous mixtures, obtains polyallylamine hydrochlorides solution, will under conditions of revolving speed is 1000r/min
Modified glucose mixed liquor is mixed with polyallylamine hydrochlorides liquor capacity ratio 1:10, in temperature be 55 DEG C, revolving speed 400r/
Under conditions of min, after being stirred to react 2h, polyallylamine hydrochlorides-modified glucose mixed liquor is obtained；By polyallylamine hydrochlorides-
Modified glucose mixed liquor is mixed with sodium borohydride 250:1 in mass ratio, is 38 DEG C in temperature, revolving speed is the condition of 320r/min
Under, after being stirred to react 3h, gel mixture is obtained, gel mixture is dialysed, and under conditions of temperature is 85 DEG C, dry 5h
Afterwards, gel is obtained；Gel and ethyl acetate 1:15 in mass ratio are mixed in three-necked flask, and gel is added into three-necked flask
The organo-aluminium and 0.10 times of gel quality of potassium hydroxide that 0.2 times of quality are 50 DEG C in temperature, and revolving speed is the condition of 400r/min
Under, after being stirred 80min, then at frequency be 55kHz under conditions of after ultrasonic disperse 30min, gel dispersion liquid is obtained, by gel
Dispersion liquid is mixed with fatty acid 20:2 in mass ratio, and gel dispersion liquid is added into the mixture of gel dispersion liquid and fatty acid
The immobilized lipase that 0.02 times of quality, in temperature be 38 DEG C, revolving speed be 380r/min under conditions of, after being stirred to react 2h, mistake
Filter, obtains modified gel blank, by modified gel blank under conditions of temperature is 70 DEG C, after being dried in vacuo 4h, obtains modified gel；
Modified gel is moved into retort, and the rate into retort with 60mL/min is passed through nitrogen and obtains porous after heat preservation carbonizes 2h
Porous carbon adsorbing material blank and water 1:15 in mass ratio are mixed in flask, and use mass fraction by carbon adsorbing material blank
The pH to 10.5 of material in flask is adjusted for 28% sodium hydroxide solution, after being standing and soaking 12h under room temperature, filtering is obtained
Filter residue obtains porous carbon adsorbing material under conditions of being 80 DEG C in temperature by filter residue after dry 3h.Bag filter used in the dialysis
Molecular cut off is 10000.The organo-aluminium is aluminium isopropoxide.The fatty acid is lauric acid.The carbonization temperature is 600
℃。
Example 3
Glucose and water 1:25 in mass ratio are mixed in beaker, and 0.2 times of glucose quality of acid iodide is added into beaker
Potassium is 65 DEG C in temperature, under conditions of revolving speed is 350r/min, after being stirred 180min, glucose mixed liquor is obtained, by grape
The barium chloride solution 1:5 in mass ratio that sugared mixed liquor and mass fraction are 20% mix, in temperature be 45 DEG C, revolving speed 400r/
Under conditions of min, after being stirred 40min, filtering obtains filtrate, and the metabisulfite solution that filtrate and mass fraction are 22% is pressed matter
Amount is mixed than 1:4, is 45 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred 40min, is filtered, removal filter
Cake obtains modified glucose mixed liquor；Polyallylamine hydrochlorides are mixed with water 1:110 in mass ratio, in temperature be 50 DEG C, revolving speed
Under conditions of 400r/min, after being stirred 60min, polyallylamine is adjusted with the sodium hydroxide solution that mass fraction is 12%
The pH to 10.0 of hydrochloride and aqueous mixtures, obtains polyallylamine hydrochlorides solution, will under conditions of revolving speed is 1000r/min
Modified glucose mixed liquor is mixed with polyallylamine hydrochlorides liquor capacity ratio 1:10, in temperature be 55 DEG C, revolving speed 400r/
Under conditions of min, after being stirred to react 2h, polyallylamine hydrochlorides-modified glucose mixed liquor is obtained；By polyallylamine hydrochlorides-
Modified glucose mixed liquor is mixed with sodium borohydride 250:1 in mass ratio, is 38 DEG C in temperature, revolving speed is the condition of 320r/min
Under, after being stirred to react 3h, gel mixture is obtained, gel mixture is dialysed, and under conditions of temperature is 85 DEG C, dry 5h
Afterwards, gel is obtained；Gel and ethyl acetate 1:15 in mass ratio are mixed in three-necked flask, and gel is added into three-necked flask
The ethyl orthosilicate and 0.10 times of gel quality of potassium hydroxide that 0.4 times of quality are 50 DEG C in temperature, and revolving speed is 400r/min's
Under the conditions of, after being stirred 80min, then at frequency be 55kHz under conditions of after ultrasonic disperse 30min, obtain gel dispersion liquid, will
Gel dispersion liquid is mixed with fatty acid 20:2 in mass ratio, and gel point is added into the mixture of gel dispersion liquid and fatty acid
The immobilized lipase that 0.02 times of dispersion liquid quality is 38 DEG C in temperature, under conditions of revolving speed is 380r/min, is stirred to react 2h
Afterwards, it filters, obtains modified gel blank, by modified gel blank under conditions of temperature is 70 DEG C, after being dried in vacuo 4h, obtain modification
Gel；Modified gel is moved into retort, and the rate into retort with 60mL/min is passed through nitrogen, after heat preservation carbonizes 2h,
Porous carbon adsorbing material blank is obtained, porous carbon adsorbing material blank and water 1:15 in mass ratio are mixed in flask, and use matter
The pH to 10.5 that the sodium hydroxide solution that score is 28% adjusts material in flask is measured, after being standing and soaking 12h under room temperature,
Filtering, obtains filter residue, under conditions of being 80 DEG C in temperature by filter residue after dry 3h, obtains porous carbon adsorbing material.Used in the dialysis
The molecular cut off of bag filter is 10000.The fatty acid is lauric acid.The carbonization temperature is 600 DEG C.
Example 4
Glucose and water 1:25 in mass ratio are mixed in beaker, and 0.2 times of glucose quality of acid iodide is added into beaker
Potassium is 65 DEG C in temperature, under conditions of revolving speed is 350r/min, after being stirred 180min, glucose mixed liquor is obtained, by grape
The barium chloride solution 1:5 in mass ratio that sugared mixed liquor and mass fraction are 20% mix, in temperature be 45 DEG C, revolving speed 400r/
Under conditions of min, after being stirred 40min, filtering obtains filtrate, and the metabisulfite solution that filtrate and mass fraction are 22% is pressed matter
Amount is mixed than 1:4, is 45 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred 40min, is filtered, removal filter
Cake obtains modified glucose mixed liquor；Polyallylamine hydrochlorides are mixed with water 1:110 in mass ratio, in temperature be 50 DEG C, revolving speed
Under conditions of 400r/min, after being stirred 60min, polyallylamine is adjusted with the sodium hydroxide solution that mass fraction is 12%
The pH to 10.0 of hydrochloride and aqueous mixtures, obtains polyallylamine hydrochlorides solution, will under conditions of revolving speed is 1000r/min
Modified glucose mixed liquor is mixed with polyallylamine hydrochlorides liquor capacity ratio 1:10, in temperature be 55 DEG C, revolving speed 400r/
Under conditions of min, after being stirred to react 2h, polyallylamine hydrochlorides-modified glucose mixed liquor is obtained；By polyallylamine hydrochlorides-
Modified glucose mixed liquor is mixed with sodium borohydride 250:1 in mass ratio, is 38 DEG C in temperature, revolving speed is the condition of 320r/min
Under, after being stirred to react 3h, gel mixture is obtained, gel mixture is dialysed, and under conditions of temperature is 85 DEG C, dry 5h
Afterwards, gel is obtained；Gel and ethyl acetate 1:15 in mass ratio are mixed in three-necked flask, and gel is added into three-necked flask
The ethyl orthosilicate that 0.4 times of quality, the organo-aluminium and 0.10 times of gel quality of potassium hydroxide that 0.2 times of gel quality, in temperature
It is 50 DEG C, is ultrasonic disperse under conditions of 55kHz then at frequency after being stirred 80min under conditions of revolving speed is 400r/min
After 30min, gel dispersion liquid is obtained；Gel dispersion liquid is moved into retort, and is passed through into retort with the rate of 60mL/min
Nitrogen obtains porous carbon adsorbing material blank, porous carbon adsorbing material blank and water 1:15 in mass ratio is mixed after heat preservation carbonizes 2h
Together in flask, and the sodium hydroxide solution for being 28% with mass fraction adjusts the pH to 10.5 of material in flask, in room temperature condition
Under be standing and soaking 12h after, filtering obtains filter residue, under conditions of being 80 DEG C in temperature by filter residue after dry 3h, obtains porous carbon adsorption material
Material.The molecular cut off of bag filter used in the dialysis is 10000.The organo-aluminium is aluminium isopropoxide.The carbonization temperature is
600℃。
Comparative example: the porous carbon adsorbing material of Wuxi material production Co., Ltd production.
Example 1 to the resulting porous carbon adsorbing material of example 4 and comparative example product are subjected to performance detection, specific detection side
Method is as follows:
Porosity is measured using mercury injection apparatus (Autopore9500)；And survey its specific surface area.Hole is measured when pressure is 500N
Rate.
Specific testing result is as shown in table 1:
The porous carbon adsorbing material performance test results of table 1
| Detection project | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example |
| Specific surface area/m2g-1 | 1763 | 1752 | 1646 | 1324 | 1112 |
| Porosity/% | 94 | 91 | 86 | 81 | 78 |
| 500N porosity/% | 91 | 87 | 83 | 76 | 70 |
By 1 testing result of table it is found that the porous carbon adsorbing material of technical solution of the present invention preparation has porosity height and excellent
The characteristics of compressive property, has broad prospects in the development of porous material technology industry.
Claims (6)
1. a kind of preparation method of porous carbon adsorbing material, which is characterized in that specific preparation step are as follows:
(1) polyallylamine hydrochlorides are mixed with water 1:100~1:110 in mass ratio, after being stirred, adjusting pH to 9.8~
10.0, polyallylamine hydrochlorides solution is obtained, under intense agitation, by modified glucose mixed liquor and polyallylamine hydrochlorides
Liquor capacity ratio 1:8~1:10 mixing, after being stirred to react, obtains polyallylamine hydrochlorides-modified glucose mixed liquor；
(2) polyallylamine hydrochlorides-modified glucose mixed liquor is mixed with sodium borohydride 200:1~250:1 in mass ratio, is stirred
After mixing reaction, gel mixture is obtained, gel mixture is dialysed, it is dry, obtain gel；
(3) gel is mixed with ethyl acetate 1:10~1:15 in mass ratio, and 0.2~0.4 times of gel quality of positive silicon is added
Acetoacetic ester, the organo-aluminium and 0.08~0.10 times of gel quality of potassium hydroxide that 0.1~0.2 times of gel quality, after being stirred,
Ultrasonic disperse obtains gel dispersion liquid, and gel dispersion liquid is mixed with fatty acid 20:1~20:2 in mass ratio, and gel point is added
The immobilized lipase that 0.01~0.02 times of dispersion liquid quality after being stirred to react, filters, dry, obtains modified gel；
(4) modified gel is carbonized under nitrogen atmosphere, obtains porous carbon adsorbing material blank, by porous carbon adsorbing material blank with
Water 1:10~1:15 in mass ratio mixing, adjusts pH to 9.0~10.5, after being standing and soaking, filters, dry, obtains porous carbon adsorption
Material.
2. a kind of preparation method of porous carbon adsorbing material according to claim 1, it is characterised in that: step (1) is described
Modified glucose mixed liquor be glucose is mixed with water 1:20~1:25 in mass ratio, and be added glucose quality 0.1~
0.2 times of Potassiumiodate after being stirred, obtains glucose mixed liquor, by glucose mixed liquor and barium chloride solution 1:3 in mass ratio
~1:5 mixing, filtering obtain filtrate, filtrate are mixed with metabisulfite solution 1:3~1:4 in mass ratio, filter, obtain modified grape
Sugared mixed liquor.
3. a kind of preparation method of porous carbon adsorbing material according to claim 1, it is characterised in that: step (2) is described
The molecular cut off of bag filter used in dialysing is 10000.
4. a kind of preparation method of porous carbon adsorbing material according to claim 1, it is characterised in that: step (3) is described
Organo-aluminium is any one in aluminium isopropoxide or aluminium ethylate.
5. a kind of preparation method of porous carbon adsorbing material according to claim 1, it is characterised in that: step (3) is described
Fatty acid is lauric acid, any one in myristic acid or palmitinic acid.
6. a kind of preparation method of porous carbon adsorbing material according to claim 1, it is characterised in that: step (4) is described
Carbonization temperature is 450~600 DEG C.
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