CN107308912B - Novel carbon-based material and preparation method thereof - Google Patents
Novel carbon-based material and preparation method thereof Download PDFInfo
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- CN107308912B CN107308912B CN201610580917.2A CN201610580917A CN107308912B CN 107308912 B CN107308912 B CN 107308912B CN 201610580917 A CN201610580917 A CN 201610580917A CN 107308912 B CN107308912 B CN 107308912B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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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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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28064—Surface area, e.g. B.E.T specific surface area being in the range 500-1000 m2/g
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- 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
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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- 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
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
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Abstract
The present invention relates to a kind of novel carbon-based material and preparation method thereof, mainly solve the problems, such as that existing adsorption recovery material hydrophobicity under high humidity environment is poor, adsorbed target organic molecule capacity is low, vacuum desorption difficulty is high, adsorption desorption rate is slow.The present invention is by using a kind of novel carbon-based material and preparation method thereof, with phenol or melamine, acid for reaction raw materials, aldehydes aqueous solution is reaction dissolvent, the technical solution that hydrophobic type high specific area carbon adsorbing material is made by collosol and gel freeze-drying and carbonization-activation process preferably solves the above problem, can be used in engineering material technology.
Description
Technical field
The present invention relates to a kind of novel carbon-based materials and preparation method thereof.
Background technology
Crude oil is from exploitation, refinery to during finally moving towards consumption market in the form of product oil, needing experience multiple
Storage and transportation cargo handling process inevitably can cause the volatilizing loss of oil product even to leak among this, cause under energy waste, oil quality
Drop, environmental pollution or even security risk.A kind of adsorption separation technology ripe and economical and efficient the most storage and transportation damage as principle
Control means are consumed, the fields such as absorption method petroleum vapor recovery are widely used in.However China comes into effect recently《Petroleum refining industry
Pollutant emission standard》(GB31570-2015) and《Petro chemical industry pollutant emission standard》(GB31571-2015),
In require non-methane total hydrocarbons treatment effeciency >=97%, benzene≤4mg/m is required in organic properties pollutant emission limit3, toluene≤
15mg/m3, dimethylbenzene≤20mg/m3, traditional " absorption+absorption process " device for recovering oil and gas has been extremely difficult to so high want
It asks, therefore the improvement of technique, the promotion of sorbing material is imperative.
The adsorbent industrially applied at present is mainly activated carbon and adsorption silica gel (such as 102989414 B of CN), these materials
It is small in the presence of the specific surface area that can be efficiently used although material has many advantages, such as that cheap, operability is easy, close duct
Caused by desorption difficulty it is big and the defects of hydrophobicity is poor.For this present situation, this patent passes through sol-gal process and titanium dioxide
Carbon high-temp activation combination processing means, be prepared for it is a kind of have high-specific surface area, hydrophobic property, ideal pore diameter range, it can be achieved that
For the carbon-based sorbing material of volatile organic compounds adsorption recovery.The obtained carbon-based sorbing material of the present invention, which has, to be opened
Property grade three-dimensional porous structure, good adsorption performance, it is not easy to moisture absorption, recycle performance it is good, volatile organic compounds inhale
Attached recycling field has shown wide application prospect and commercial value.
Invention content
The first technical problem to be solved by the present invention be existing adsorption recovery material hydrophobicity under high humidity environment it is poor,
The problem that adsorbed target organic molecule capacity is low, vacuum desorption difficulty is high, adsorption desorption rate is slow, provides a kind of new New Type of Carbon
Sill.The material is good with adsorption recovery material hydrophobicity under high humidity environment, adsorbed target organic molecule capacity is high,
The advantage that vacuum desorption difficulty is low, adsorption desorption rate is fast.The second technical problem to be solved by the present invention is to provide a kind of and solution
The certainly preparation method of the corresponding novel carbon-based material of one of technical problem.
One of in order to solve the above problem, the technical solution adopted by the present invention is as follows：A kind of novel carbon-based material, it is described carbon-based
Sorbing material specific surface area is 500~2300m2/ g, mesoporous content is 30~70%, microcosmic to show three-dimensional cross-linked netted grade
Pore structure, mesoporous pore size size are 2~60nm, and most probable pore size is 1.7~3.8nm, the contact angle of carbon-based sorbing material and water
More than 120 °.
In order to solve the above problem two, the technical solution adopted by the present invention is as follows：A kind of preparation side of novel carbon-based material
Method, with phenol or melamine, acid for reaction raw materials, aldehydes aqueous solution is reaction dissolvent, by gelatin wrapping-freeze drying and
Carbonization-activation process is made hydrophobic type high specific area carbon adsorbing material, and the aldehydes is acetaldehyde, benzaldehyde or propionic aldehyde, described
Acid is one kind in formic acid, ethanedioic acid, succinic acid, phosphoric acid, hydrochloric acid, benzoic acid or phenylacetic acid；Specifically preparation process includes：
(1) phenol or melamine and aldehydes aqueous solution are mixed first, acid is then added and is uniformly mixed；
(2) after the mixed solution obtained in step (1) persistently being stirred and is cured, carry out pre-freeze handle to -80 DEG C hereinafter,
It is subsequently placed into vacuum freezing drying oven and water removal is dried；
(3) the gel block that step obtains will be freeze-dried to be positioned in carbonization-activation equipment, empties reactor carbonization
It is filled with inertia protection gas after inner air tube, reaction in-furnace temperature is risen to 600 DEG C or more, the reaction time is more than 3 hours, heats the phase
Between keep inert gas be continually fed into；
(4) after reaction, reaction temperature is increased, inert protective gas atmosphere is during which cut off and is passed through two into reactor
Carbon oxide gas carries out activation 3 hours or more by other gaseous mixtures of key component of carbon dioxide, waits for that product is cooled to room
It is taken out after temperature, finally obtains the carbon-based sorbing material of hydrophobic type.
In above-mentioned technical proposal, it is preferable that other gaseous mixtures are carbon dioxide/vapor, carbon dioxide/hydrogen, dioxy
Change carbon/nitrogen gas.
In above-mentioned technical proposal, it is preferable that the mixed solution stirs hardening time>12 hours；It is persistently stirred in step 2)
The temperature mixed is 70~100 DEG C；Sample sublimation drying>24 hours；Heating rate is in reacting furnace<10 DEG C/min；Inertia
Protection gas is nitrogen, and it is 600~800 DEG C that in-furnace temperature is reacted in nitrogen atmosphere；Reaction time is 3~6 hours；Carbon dioxide gas
Activation temperature is 850~1100 DEG C in atmosphere, and soak time is 3~8 hours.
In above-mentioned technical proposal, it is preferable that reacting furnace is tubular heater, high temperature cabonization bed, Muffle furnace.
In above-mentioned technical proposal, it is preferable that the mass ratio of phenols and aldehydes is 20~30, the mass ratio of acid and aldehydes is 35
~45.
The hydrophobic carbon adsorbing material preparation method that this patent proposes is simple, and product pattern is easy to regulate and control, recycling
Can it is excellent, convenient for recycling Reusability, while can large-scale production, contribute to product from laboratory prepare to commercial Application turn
Change.Novel carbon-based material produced by the invention has good hydrophobic performance (angle of wetting>120 °), microcosmic grade porous structure production
Raw small scale confinement effect makes diffusion path of the volatile organic compounds molecule on binding matrix shorten, and fundamentally changes
Adsorption desorption kinetic property is become, adsorption desorption rate is caused to be accelerated, desorption temperature reduces.Meanwhile the distinctive big ratio of nano material
Surface area and internal abundant cross-linked network and micro channel, can improve the active site and selective activization of adsorbent, promote
Into absorption, separative efficiency and ensure good mechanical stability, achieves preferable technique effect.
Description of the drawings
The carbon-based sorbing material electron scanning micrograph of Fig. 1 hydrophobic types.
The BET analyses of Fig. 2 carbon-based material specific surface areas.
Fig. 3 product pore-size distributions.
Fig. 4 product hydrophobicitys are tested.
The present invention will be further described below by way of examples, but is not limited only to the present embodiment.
Specific implementation mode
【Embodiment 1】
(1) first, 20g phenol is dissolved in the acetaldehyde solution that 40ml mass fractions are 37%, then 0.9g formic acid is added dropwise,
10 minutes are stirred to solution substantially uniformity.
(2) then, above-mentioned mixed solution is at the uniform velocity stirred 72 hours in 80 DEG C of constant temperature water bath environment, it is solidifying obtains Chinese red
Blob of viscose material.
(3) the rapid pre-freeze of liquid nitrogen is used, is put into and is placed in drying 24 hours in -80 DEG C of vacuum freeze driers.Obtain drying
It is put into tubular heater after sample, nitrogen protection gas is filled with after emptying inner air tube, gas velocity 50sccm, in following reaction stove
Temperature rises to 750 DEG C by 5 DEG C/min of heating rates, continues 3 hours, keeps nitrogen to be continually fed into during heating；
(4) 900 DEG C then are warming up to by 5 DEG C/min and are kept for 5 hours, during which use carbon dioxide gas to replace initial
Nitrogen atmosphere, cooled product to room temperature is taken out after the completion of activation, obtains hydrophobic carbon adsorbing material.
Fig. 1 is that the scanning electron microscope (SEM) of carbon-based sorbing material characterizes, and shows that product appearance is carbonarius respectively,
Inside is the three-dimensional grade porous structure of crosslinking net, wherein mesoporous pore size ranging from 20~60nm；
BET in Fig. 2 is analysis shows that sample specific surface area is up to 2334m2/ g, average pore size 3.11nm, most probable pore size
For 2.63nm, Kong Rongwei 1.78cm3/g；
Show that product pore-size distribution is concentrated mainly between 1~5nm in Fig. 3, intermediary hole rate is 69%；
Showing that product is positioned in water body in Fig. 4 can swim on the water surface, have good hydrophobicity, angle of wetting big
In 119 ° ± 1.2 °, illustrate that the present invention relates to carbon-based sorbing materials to have good hydrophobic property.
【Embodiment 2】
(1) first, by 115g melamines and 170g dissolution of benzaldehyde in 300ml deionized waters, after mixing well again
4g ethanedioic acids are added, stirring obtains mixed solution in 15 minutes.
(2) then, above-mentioned mixed solution is at the uniform velocity stirred 24 hours in 80 DEG C of constant temperature water bath environment, it is solidifying obtains Chinese red
Blob of viscose material.
(3) the rapid pre-freeze of liquid nitrogen is used, is put into and is placed in drying 24 hours in -80 DEG C of vacuum freeze driers.Obtain drying
It is put into tubular heater after sample, it, will be warm in tube furnace by 5 DEG C/min under the nitrogen atmosphere protection that gas velocity is 50sccm
Degree rises to 800 DEG C, continues 3 hours, keeps nitrogen to be continually fed into during heating；
(4) cutting off stream of nitrogen gas then uses carbon dioxide to replace, and gas velocity remains unchanged, while being warming up to by 5 DEG C/min
950 DEG C and keep 4 hours, after the completion of activation cooled product to room temperature take out, obtain hydrophobic carbon adsorbing material.
The SEM results of gained sample are similar with Fig. 1 results in embodiment 1, it was demonstrated that reproducibility after embodiment 1 scales up
Well.
Products obtained therefrom specific surface area is reduced to 1835m after the priming reaction time is shortened in the display of BET results2/ g, average pore size
For 2.71nm, most probable pore size 1.72nm, Kong Rongwei 1.19cm3/g；
Hydrophobic test result shows that the water angle of wetting of product is 116 ± 1.6 °, does not substantially change, also with embodiment
1 products obtained therefrom is similar.
Present invention design preparation method gained hydrophobic carbon adsorbing material under the conditions of differential responses under optimum controlling condition
Specific surface area, Kong Rong, Micropore volume parameter are as shown in table 1：
1 preparation temperature of table influences hydrophobic carbon fiber aeroge absorption property
【Embodiment 3】
(1) first, 12g phenol and 18g propionic aldehyde are dissolved in 95ml deionized waters, 0.45g is added after mixing well
Succinic acid, stirring obtain mixed solution in 20 minutes.
(2) then, above-mentioned mixed solution is at the uniform velocity stirred 48 hours in 90 DEG C of constant temperature water bath environment, it is solidifying obtains Chinese red
Blob of viscose material.
(3) the rapid pre-freeze of liquid nitrogen is used, is put into and is placed in drying 36 hours in -85 DEG C of vacuum freeze driers.Obtain drying
It is put into tubular heater after sample, it, will be warm in tube furnace by 7 DEG C/min under the nitrogen atmosphere protection that gas velocity is 50sccm
Degree rises to 600 DEG C, continues 6 hours, keeps nitrogen to be continually fed into during heating；
(4) cutting off stream of nitrogen gas then uses carbon dioxide to replace, and gas velocity remains unchanged, while being warming up to by 7 DEG C/min
850 DEG C and keep 8 hours, after the completion of activation cooled product to room temperature take out, obtain hydrophobic carbon adsorbing material.
The SEM results of gained sample are similar with Fig. 1 results, specific surface area 1534m2/ g, most probable pore size 2.7nm,
Hydrophobic test result shows that the water angle of wetting of product is 118 ± 0.7 °, does not substantially change, and is also produced with 1 gained of embodiment
Category is seemingly.
【Embodiment 4】
(1) first, 9g phenol and 15.7g acetaldehyde are dissolved in 70ml deionized waters, 0.45g is added after mixing well
Phenylacetic acid, stirring obtain mixed solution in 30 minutes.
(2) then, above-mentioned mixed solution is at the uniform velocity stirred 12 hours in 100 DEG C of constant temperature water bath environment, obtains Chinese red
Gel bulk.
(3) the rapid pre-freeze of liquid nitrogen is used, is put into and is placed in drying 48 hours in -80 DEG C of vacuum freeze driers.Obtain drying
It is put into tubular heater after sample, it, will be warm in tube furnace by 9 DEG C/min under the nitrogen atmosphere protection that gas velocity is 50sccm
Degree rises to 780 DEG C, continues 3 hours, keeps nitrogen to be continually fed into during heating；
(4) cutting off stream of nitrogen gas then uses carbon dioxide to replace, and gas velocity remains unchanged, while being warming up to by 9 DEG C/min
1100 DEG C and keep 3 hours, after the completion of activation cooled product to room temperature take out, obtain hydrophobic carbon adsorbing material.
The SEM results of gained sample are similar with Fig. 1 results, specific surface area 1690m2/ g, most probable pore size 2.9nm,
Hydrophobic test result shows that the water angle of wetting of product is 113 ± 1.5 °, does not substantially change, and is also produced with 1 gained of embodiment
Category is seemingly.
【Embodiment 5】
(1) first, 27g melamines and 40.5g propionic aldehyde are dissolved in 200ml deionized waters, are added again after mixing well
Enter 0.9g phosphoric acid, stirring obtains mixed solution in 30 minutes.
(2) then, above-mentioned mixed solution is at the uniform velocity stirred 24 hours in 80 DEG C of constant temperature water bath environment, it is solidifying obtains Chinese red
Blob of viscose material.
(3) the rapid pre-freeze of liquid nitrogen is used, is put into and is placed in drying 72 hours in -80 DEG C of vacuum freeze driers.Obtain drying
It is put into tubular heater after sample, it, will be warm in tube furnace by 3 DEG C/min under the nitrogen atmosphere protection that gas velocity is 50sccm
Degree rises to 700 DEG C, continues 4 hours, keeps nitrogen to be continually fed into during heating；
(4) cutting off stream of nitrogen gas then uses carbon dioxide to replace, and gas velocity remains unchanged, while being warming up to by 3 DEG C/min
950 DEG C and keep 5.5 hours, after the completion of activation cooled product to room temperature take out, obtain hydrophobic carbon adsorbing material.
The SEM results of gained sample are similar with Fig. 1 results, specific surface area 1307m2/ g, most probable pore size 3.5nm,
Hydrophobic test result shows that the water angle of wetting of product is 118 ± 1.1 °, does not substantially change, and is also produced with 1 gained of embodiment
Category is seemingly.
Claims (2)
1. a kind of novel carbon-based material, the carbon-based sorbing material specific surface area is 500~2300m2/ g, mesoporous content be 30~
70%, microcosmic to show three-dimensional cross-linked netted grade pore structure, mesoporous pore size size is 2~60nm, most probable pore size is 1.7~
The contact angle of 3.8nm, carbon-based sorbing material and water is more than 120 °；The preparation method of the novel carbon-based material, with phenol or three
Poly cyanamid, acid are reaction raw materials, and aldehydes aqueous solution is reaction dissolvent, by gelatin wrapping-freeze drying and carbonization-activation process
Hydrophobic type high specific area carbon adsorbing material is made, the aldehydes is acetaldehyde, benzaldehyde or propionic aldehyde, and the acid is formic acid, second
One kind in diacid, succinic acid, phosphoric acid, hydrochloric acid, benzoic acid or phenylacetic acid；Specifically preparation process includes：
(1) phenol or melamine and aldehydes aqueous solution are mixed first, acid is then added and is uniformly mixed；
(2) it after the mixed solution obtained in step (1) persistently being stirred and cured, carries out pre-freeze and handles to -80 DEG C hereinafter, then
It is put into vacuum freezing drying oven and water removal is dried；
(3) the gel block that step obtains will be freeze-dried to be positioned in carbonization-activation equipment, is emptied in reactor carbonized tube
It is filled with inertia protection gas after air, reaction in-furnace temperature is risen to 600 DEG C or more, the reaction time is more than 3 hours, is protected during heating
Inert gas is held to be continually fed into；
(4) after reaction, reaction temperature is increased, inert protective gas atmosphere is during which cut off and is passed through into reactor with dioxy
Change other gaseous mixtures that carbon is key component and carry out activation 3 hours or more, takes out, finally obtain thin after product is cooled to room temperature
The carbon-based sorbing material of water type；
Other gaseous mixtures are carbon dioxide/vapor, carbon dioxide/hydrogen, titanium dioxide carbon/nitrogen gas；The mixed solution stirring
Hardening time>12 hours；The temperature persistently stirred in step 2) is 70~100 DEG C；Sample sublimation drying>24 hours；Instead
The heating rate in stove is answered to be<10 DEG C/min；It is nitrogen that inertia, which protects gas, and it is 600~800 that in-furnace temperature is reacted in nitrogen atmosphere
℃；Reaction time is 3~6 hours；Activation temperature is 850~1100 DEG C in carbon dioxide atmosphere, and soak time is 3~8 hours；
The mass ratio of phenols and aldehydes is 20~30, the mass ratio of acid and aldehydes is 35~45.
2. the preparation method of novel carbon-based material according to claim 1, it is characterised in that reacting furnace is tubular heater, height
Temperature carbonization bed, Muffle furnace.
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