CN107324332A - New Type of Carbon adsorbing material and preparation method thereof - Google Patents
New Type of Carbon adsorbing material and preparation method thereof Download PDFInfo
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- CN107324332A CN107324332A CN201610586218.9A CN201610586218A CN107324332A CN 107324332 A CN107324332 A CN 107324332A CN 201610586218 A CN201610586218 A CN 201610586218A CN 107324332 A CN107324332 A CN 107324332A
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Abstract
The present invention relates to a kind of New Type of Carbon adsorbing material and preparation method thereof, the problem of existing adsorption recovery material hydrophobicity under high humidity environment is poor, adsorbed target organic molecule capacity is low, vacuum desorption difficulty high, adsorption desorption speed is slow is mainly solved.The present invention is by using a kind of New Type of Carbon adsorbing material and preparation method thereof, using resorcinol or phloroglucin, glacial acetic acid as reaction raw materials, formalin is reaction dissolvent, it is freeze-dried by collosol and gel and the technical scheme of the obtained hydrophobic type high specific area carbon adsorbing material of carbonization-activation process preferably solves above mentioned problem, available in engineering material technology.
Description
Technical field
The present invention relates to a kind of New Type of Carbon adsorbing material and preparation method thereof.
Background technology
Crude oil is from exploitation, refinery to finally during moving towards consumption market in the form of product oil, it is necessary to undergo repeatedly
Accumulating cargo handling process, can cause the volatilizing loss of oil product even to leak unavoidably in the middle of this, cause under energy waste, oil quality
Drop, environmental pollution or even potential safety hazard.Adsorption separation technology is damaged as a kind of principle maturation and the most accumulating of economical and efficient
Control device is consumed, is widely used in the fields such as absorption method petroleum vapor recovery.But China comes into effect recently《Petroleum refining industry
Pollutant emission standard》(GB31570-2015) and《Petro chemical industry pollutant emission standard》(GB31571-2015), its
In require to require benzene≤4mg/m in NMHC treatment effeciency >=97%, organic properties pollutant emission limit3, toluene≤
15mg/m3, dimethylbenzene≤20mg/m3, traditional " absorption+absorption process " device for recovering oil and gas be extremely difficult to it is so high will
Ask, therefore the improvement of technique, the lifting of sorbing material is imperative.
The adsorbent industrially applied at present is mainly activated carbon and adsorption silica gel (such as B of CN 102989414), these materials
It is small in the presence of the specific surface area that can effectively utilize although material has the advantages that cheap, operability is easy, close duct
The desorption difficulty that causes is big and the defect such as hydrophobicity difference.For this present situation, this patent passes through sol-gal process and titanium dioxide
Carbon high-temp activation combination processing means, being prepared for one kind has high-specific surface area, hydrophobic property, preferable pore diameter range, can be achieved
For the carbon-based sorbing material of VOC adsorption recovery.Carbon-based sorbing material obtained by the present invention, which has, to be opened
Property grade three-dimensional porous structure, good adsorption performance, be difficult moisture absorption, recycle performance it is good, VOC inhale
Attached recycling field has shown wide application prospect and commercial value.
The content of the invention
One of technical problems to be solved by the invention be existing adsorption recovery material hydrophobicity under high humidity environment it is poor,
There is provided a kind of new New Type of Carbon for the problem of adsorbed target organic molecule capacity is low, vacuum desorption difficulty high, adsorption desorption speed is slow
Adsorbing material.The material has that adsorption recovery material hydrophobicity under high humidity environment is good, adsorbed target organic molecule holds
Amount is high, the advantage that vacuum desorption difficulty is low, adsorption desorption speed is fast.The two of the technical problems to be solved by the invention are to provide one kind
Preparation method with solving one of technical problem corresponding New Type of Carbon adsorbing material.
One of to solve the above problems, the technical solution adopted by the present invention is as follows：A kind of New Type of Carbon adsorbing material, it is described
Carbon-based sorbing material specific surface area is 500~2300m2/ g, mesoporous content be 30~70%, it is microcosmic show it is three-dimensional cross-linked netted
Grade pore structure, mesoporous pore size size is 2~60nm, and most probable pore size is 1.7~3.8nm, and carbon-based sorbing material and water connect
Feeler is more than 120 °.
For solve the above problems two, the technical solution adopted by the present invention is as follows：A kind of system of New Type of Carbon adsorbing material
Preparation Method, using resorcinol or phloroglucin, glacial acetic acid as reaction raw materials, formalin is reaction dissolvent, solidifying by colloidal sol
Hydrophobic type high specific area carbon adsorbing material is made in glue-freeze-drying and carbonization-activation process；Specific preparation process includes：
(1) resorcinol or phloroglucin and formalin are mixed first, then adds glacial acetic acid stirring mixing equal
It is even；
(2) after the mixed solution obtained in step (1) persistently being stirred and solidified, carry out pre-freeze and handle to less than -80 DEG C,
It is subsequently placed into vacuum freezing drying oven and water removal is dried；
(3) the gel block for obtaining freeze-drying step is positioned in carbonization-activation equipment, the carbonization of emptying reactor
Inertia protection gas is filled with after inner air tube, reaction in-furnace temperature is risen to more than 600 DEG C, the reaction time, more than 3 hours, heats the phase
Between keep inert gas be continually fed into；
(4) after reaction terminates, reaction temperature is raised, inert protective gas atmosphere is during which cut off and is passed through two into reactor
Carbon oxide gas or other gaseous mixtures by key component of carbon dioxide carry out activation more than 3 hours, treat that product is cooled to room
Taken out after temperature, finally give 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；Step 2) in persistently stir
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 reaction in-furnace temperature is 600~800 DEG C 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 resorcinol or phloroglucin and formaldehyde is 20~30, glacial acetic acid
Mass ratio with formaldehyde is 35~45.
The hydrophobic carbon adsorbing material preparation method that this patent is proposed is simple, and product pattern is easy to regulation and control, recycling
Can it is excellent, be easy to reclaim Reusability, while can large-scale production, contribute to product from laboratory prepare to commercial Application turn
Change.New carbon-based material produced by the invention has good hydrophobic performance (angle of wetting>120 °), microcosmic grade loose structure production
Raw small yardstick confinement effect causes diffusion path of the VOC molecule on binding matrix to shorten, and fundamentally changes
Become adsorption desorption kinetic property, cause adsorption desorption speed to be accelerated, desorption temperature reduction.Meanwhile, the distinctive big ratio of nano material
Surface area and internal abundant cross-linked network and micro channel, it is possible to increase the avtive spot and selective activization of adsorbent, promote
Enter absorption, separative efficiency and ensure good mechanical stability, achieve preferable technique effect.
Brief description of the drawings
The carbon-based sorbing material electron scanning micrograph of Fig. 1 hydrophobic types.
Fig. 2 carbon-based material specific surface areas BET is analyzed.
Fig. 3 product pore-size distributions.
Fig. 4 products hydrophobicity is tested.
Below by embodiment, the invention will be further elaborated, but is not limited only to the present embodiment.
Embodiment
【Embodiment 1】
(1) first, 20g resorcinols are dissolved in the formalin that 40ml mass fractions are 37%, then 0.9g is added dropwise
Glacial acetic acid, stirs 10 minutes 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, obtains Chinese red and coagulate
Blob of viscose material.
(3) the rapid pre-freeze of liquid nitrogen is used, is put into be placed in -80 DEG C of vacuum freeze driers and dries 24 hours.Obtain drying
It is put into after sample in tubular heater, nitrogen protection gas is filled with after emptying inner air tube, gas velocity is in 50sccm, 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 replace initial using carbon dioxide
Cooled product to room temperature is taken out after the completion of nitrogen atmosphere, activation, obtains hydrophobic carbon adsorbing material.
Fig. 1 characterizes for the SEM (SEM) of carbon-based sorbing material, and it is carbonarius that product appearance is shown respectively,
Inside is the three-dimensional grade loose structure of crosslinking net, and wherein mesoporous pore size scope is 20~60nm；
BET analyses show that sample specific surface area is up to 2322m in Fig. 22/ g, average pore size is 3.03nm, most probable pore size
For 2.54nm, pore volume is 1.76cm3/g；
Show that product pore-size distribution is concentrated mainly between 1~5nm in Fig. 3, its intermediary hole rate is 70%；
Showing that product is positioned in water body in Fig. 4 can swim on the water surface, and with good hydrophobicity, its angle of wetting is big
In 120 ° ± 1.2 °, illustrate that there is good hydrophobic property the present invention relates to carbon-based sorbing material.
【Embodiment 2】
(1) first, 115g resorcinols and 170g formaldehyde are dissolved in 300ml deionized waters, added again after fully mixing
Enter 4g glacial acetic acid, 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, obtains Chinese red and coagulate
Blob of viscose material.
(3) the rapid pre-freeze of liquid nitrogen is used, is put into be placed in -80 DEG C of vacuum freeze driers and dries 24 hours.Obtain drying
Be put into after sample in tubular heater, in gas velocity under 50sccm nitrogen atmosphere protection, by 5 DEG C/min will in tube furnace it is warm
Degree rises to 800 DEG C, continues 3 hours, keeps nitrogen to be continually fed into during heating；
(4) cut off stream of nitrogen gas then using carbon dioxide to replace, gas velocity keeps constant, 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 reappearance after embodiment 1 is scaled up
Well.
The display of BET results shortens products obtained therefrom specific surface area after the priming reaction time and is reduced to 1836m2/ g, average pore size
For 2.69nm, most probable pore size is 1.69nm, and pore volume is 1.23cm3/g；
Hydrophobic test result shows that the water angle of wetting of product is 114 ± 1.6 °, does not occur 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, pore volume, Micropore volume parameter are as shown in table 1：
The preparation temperature of table 1 influences on hydrophobic carbon fiber aeroge absorption property
【Embodiment 3】
(1) first, 12g resorcinols and 18g formaldehyde are dissolved in 95ml deionized waters, added after fully mixing
0.45g glacial acetic acid, stirring obtains 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, obtains Chinese red and coagulate
Blob of viscose material.
(3) the rapid pre-freeze of liquid nitrogen is used, is put into be placed in -85 DEG C of vacuum freeze driers and dries 36 hours.Obtain drying
Be put into after sample in tubular heater, in gas velocity under 50sccm nitrogen atmosphere protection, by 7 DEG C/min will in tube furnace it is warm
Degree rises to 600 DEG C, continues 6 hours, keeps nitrogen to be continually fed into during heating；
(4) cut off stream of nitrogen gas then using carbon dioxide to replace, gas velocity keeps constant, 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, and specific surface area is 1583m2/ g, most probable pore size is 2.9nm,
Hydrophobic test result shows that the water angle of wetting of product is 122 ± 0.7 °, does not occur substantially change, is also produced with the gained of embodiment 1
Category is seemingly.
【Embodiment 4】
(1) first, 9g resorcinols and 15.7g formaldehyde are dissolved in 70ml deionized waters, added after fully mixing
0.45g glacial acetic acid, stirring obtains 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 be placed in -80 DEG C of vacuum freeze driers and dries 48 hours.Obtain drying
Be put into after sample in tubular heater, in gas velocity under 50sccm nitrogen atmosphere protection, by 9 DEG C/min will in tube furnace it is warm
Degree rises to 780 DEG C, continues 3 hours, keeps nitrogen to be continually fed into during heating；
(4) cut off stream of nitrogen gas then using carbon dioxide to replace, gas velocity keeps constant, 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, and specific surface area is 1720m2/ g, most probable pore size is 3.2nm,
Hydrophobic test result shows that the water angle of wetting of product is 118 ± 1.3 °, does not occur substantially change, is also produced with the gained of embodiment 1
Category is seemingly.
【Embodiment 5】
(1) first, 27g phloroglucins and 40.5g formaldehyde are dissolved in 200ml deionized waters, added again after fully mixing
Enter 0.9g glacial acetic 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, obtains Chinese red and coagulate
Blob of viscose material.
(3) the rapid pre-freeze of liquid nitrogen is used, is put into be placed in -80 DEG C of vacuum freeze driers and dries 72 hours.Obtain drying
Be put into after sample in tubular heater, in gas velocity under 50sccm nitrogen atmosphere protection, by 3 DEG C/min will in tube furnace it is warm
Degree rises to 700 DEG C, continues 4 hours, keeps nitrogen to be continually fed into during heating；
(4) cut off stream of nitrogen gas then using carbon dioxide to replace, gas velocity keeps constant, 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, and specific surface area is 1320m2/ g, most probable pore size is 3.7nm,
Hydrophobic test result shows that the water angle of wetting of product is 120 ± 1.1 °, does not occur substantially change, is also produced with the gained of embodiment 1
Category is seemingly.
Claims (6)
1. a kind of New Type of Carbon adsorbing material, the 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 is 2~60nm, and most probable pore size is
1.7~3.8nm, the contact angle of carbon-based sorbing material and water is more than 120 °.
2. the preparation method of New Type of Carbon adsorbing material described in claim 1, is anti-using resorcinol or phloroglucin, glacial acetic acid
Raw material is answered, formalin is reaction dissolvent, hydrophobic type height, which is made, by gelatin wrapping-freeze drying and carbonization-activation process compares
Area carbon adsorbing material；Specific preparation process includes：
(1) resorcinol or phloroglucin and formalin are mixed first, then adds glacial acetic acid and be uniformly mixed；
(2) after the mixed solution obtained in step (1) persistently being stirred and solidified, carry out pre-freeze and handle to less than -80 DEG C, then
It is put into vacuum freezing drying oven and water removal is dried；
(3) the gel block for obtaining freeze-drying step is positioned in carbonization-activation equipment, in emptying reactor carbonized tube
Inertia protection gas is filled with after air, reaction in-furnace temperature more than 600 DEG C are risen to, the reaction time, more than 3 hours, protects during heating
Inert gas is held to be continually fed into；
(4) after reaction terminates, reaction temperature is raised, inert protective gas atmosphere is during which cut off and titanium dioxide is passed through into reactor
Carbon gas or other gaseous mixtures by key component of carbon dioxide carry out activation more than 3 hours, after product is cooled to room temperature
Take out, finally give the carbon-based sorbing material of hydrophobic type.
3. the preparation method of New Type of Carbon adsorbing material according to claim 2, it is characterised in that other gaseous mixtures are dioxy
Change carbon/vapor, carbon dioxide/hydrogen, titanium dioxide carbon/nitrogen gas.
4. the preparation method of New Type of Carbon adsorbing material according to claim 2, it is characterised in that the mixed solution stirring
Hardening time>12 hours；Step 2) in the temperature that persistently stirs be 70~100 DEG C；Sample sublimation drying>24 hours；Instead
The heating rate in stove is answered to be<10 DEG C/min；Inertia protects gas for nitrogen, and reaction in-furnace temperature is 600~800 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.
5. the preparation method of New Type of Carbon adsorbing material according to claim 2, it is characterised in that reacting furnace is tubular type heating
Stove, high temperature cabonization bed, Muffle furnace.
6. the preparation method of New Type of Carbon adsorbing material according to claim 2, it is characterised in that resorcinol or isophthalic three
The mass ratio of phenol and formaldehyde is that the mass ratio of 20~30, glacial acetic acid and formaldehyde is 35~45.
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