CN107324332B - 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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Abstract
The present invention relates to a kind of New Type of Carbon adsorbing 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 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, 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 New Type of Carbon adsorbing 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
Adsorbing material.With adsorption recovery material hydrophobicity under high humidity environment, good, adsorbed target organic molecule holds the material
The advantage that amount is high, vacuum desorption difficulty is low, adsorption desorption rate is fast.The second technical problem to be solved by the present invention is to provide one kind
With the preparation method for solving the corresponding New Type of Carbon adsorbing 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 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 are 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 °.
In order to solve the above problem 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；Specifically preparation process includes：
(1) resorcinol or phloroglucin and formalin are mixed first, glacial acetic acid is then added and is stirred
It is even；
(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 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 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 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, 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 2322m2/ g, average pore size 3.03nm, most probable pore size
For 2.54nm, Kong Rongwei 1.76cm3/g；
Show that product pore-size distribution is concentrated mainly between 1~5nm in Fig. 3, intermediary hole rate is 70%；
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 120 ° ± 1.2 °, illustrate that the present invention relates to carbon-based sorbing materials to have good hydrophobic property.
【Embodiment 2】
(1) first, 115g resorcinols and 170g formaldehyde are dissolved in 300ml deionized waters, are added again after mixing well
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, 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 1836m after the priming reaction time is shortened in the display of BET results2/ g, average pore size
For 2.69nm, most probable pore size 1.69nm, Kong Rongwei 1.23cm3/g；
Hydrophobic test result shows that the water angle of wetting of product is 114 ± 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 resorcinols and 18g formaldehyde are dissolved in 95ml deionized waters, are added after mixing well
0.45g glacial acetic 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 1583m2/ g, most probable pore size 2.9nm,
Hydrophobic test result shows that the water angle of wetting of product is 122 ± 0.7 °, does not substantially change, and is also produced with 1 gained of embodiment
Category is seemingly.
【Embodiment 4】
(1) first, 9g resorcinols and 15.7g formaldehyde are dissolved in 70ml deionized waters, are added after mixing well
0.45g glacial acetic 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 1720m2/ g, most probable pore size 3.2nm,
Hydrophobic test result shows that the water angle of wetting of product is 118 ± 1.3 °, does not substantially change, and is also produced with 1 gained of embodiment
Category is seemingly.
【Embodiment 5】
(1) first, 27g phloroglucins and 40.5g formaldehyde are dissolved in 200ml deionized waters, are added again after mixing well
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, 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 1320m2/ g, most probable pore size 3.7nm,
Hydrophobic test result shows that the water angle of wetting of product is 120 ± 1.1 °, does not substantially change, and is also produced with 1 gained of embodiment
Category is seemingly.
Claims (2)
1. a kind of New Type of Carbon adsorbing material, the carbon-based sorbing material specific surface area is 500~2300m2/ g, mesoporous content are
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
The contact angle of 1.7~3.8nm, carbon-based sorbing material and water is more than 120 °；The preparation method of the New Type of Carbon adsorbing material, with
Phloroglucin, glacial acetic acid are reaction raw materials, and formalin is reaction dissolvent, are lived by gelatin wrapping-freeze drying and carbonization
Hydrophobic type high specific area carbon adsorbing material is made in change process；Specifically preparation process includes：
(1) phloroglucin and formalin are mixed first, glacial acetic 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 phloroglucin and formaldehyde is 20~30, the mass ratio of glacial acetic acid and formaldehyde is 35~45.
2. the preparation method of New Type of Carbon adsorbing material according to claim 1, it is characterised in that reacting furnace heats for tubular type
Stove, high temperature cabonization bed, Muffle furnace.
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| CN107308912B (en) * | 2016-07-22 | 2018-08-17 | 中国石油化工股份有限公司 | Novel carbon-based material and preparation method thereof |
| CN116741976A (en) * | 2023-08-16 | 2023-09-12 | 中石油深圳新能源研究院有限公司 | Iron single-atom doped positive electrode material and preparation method and application thereof |
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