CN111450810B - Method for improving pore structure of material - Google Patents
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- 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
Abstract
The invention discloses a method for improving a pore structure of a material, which relates to the field of adsorption materials and comprises the following steps: taking a proper amount of an adsorption material into a wide-mouth stainless steel container, wherein the adsorption material is an inorganic porous material or an organic porous material; step two: slowly adding liquid nitrogen into the stainless steel container, sealing the stainless steel container with a cover, and reacting for the time after the liquid nitrogen is added until the liquid nitrogen is naturally evaporated; step three: and after the adsorbing material in the second step is naturally heated to the room temperature, repeating the second step for 1-4 times. The invention has the characteristics of low modification cost, simple operation, low equipment requirement and low energy consumption.
Description
Technical Field
The invention relates to the field of adsorption materials, in particular to a method for improving a pore structure of a material.
Background
Adsorbents are solid substances that are effective in adsorbing certain components from a gas or liquid. The adsorbent has the characteristics of large specific surface area, proper pore structure and surface structure, strong adsorption capacity to the adsorbate and no chemical reaction with the adsorbate and a medium.
The adsorption materials which can be used as the adsorbent are divided into inorganic porous materials and organic porous materials. Inorganic porous materials such as natural zeolite, artificial zeolite, coal ash, etc., organic porous materials such as various biochar (biochar of various raw materials), various activated carbons (biochar of various raw materials and shapes: column, granule, powder, etc.).
According to the pore size, the porous materials are divided into three types, namely micropores (<2.0nm), mesopores (2.0-50 nm) and macropores (>50.0 nm). The microporous material is mainly prepared by a solid phase method, a hydrothermal method, a solvothermal method and the like; the mesoporous material is mainly prepared by a template method; macroporous materials are generally prepared by emulsion polymerization, biomatex and gel-crystal templating.
The modification path of the porous material is mainly divided into two paths, and the first path is realized by adjusting process parameters during the early-stage synthesis of the material. For example, activated carbon materials, where the activation step is critical to the adjustment of the pore size distribution, and where the addition of chemical activators is different, the pore structure formed will be different, although up to 1000m can be achieved as well2A specific surface area of about/g, however ZnCl2The activated carbon has rich mesopores, while the activated carbon activated by KOH has more micropores; the method has the defects of high requirements on process equipment, control precision and raw material components and the advantage of fundamentally solving the pore requirements of the target porous material.
The second is to carry out later modification on some commercial or existing porous materials, and the following materials are mainly adopted:
(1) the metal salt soaking method has the advantages that the adsorption acting force of the surface of the porous material to a specific adsorption object can be enhanced or weakened; the disadvantage is that additional metal is introduced, causing secondary pollution.
(2) The ultrasonic assisted impregnation method is developed on the basis of a metal salt impregnation method, and has the advantages of solving the phenomena of agglomeration and uneven distribution of effective components in a common impregnation method, ensuring that the active metal ion components have smaller particle size and higher dispersion degree, and further enhancing or weakening the adsorption acting force of the surface of the porous material on a specific adsorption object; the defects are that ultrasonic equipment is additionally arranged, the construction difficulty is improved, and the cost is increased.
(3) The thermal oxidation method is a simple method for modifying the surface of the porous carbon material. The method has the advantages that when the carbon is contacted with high-temperature air, the surface of the carbon can generate oxidation reaction, the acidic oxygen-containing groups on the surface of the carbon are increased, and the surface active adsorption points are increased; the disadvantages are that the carbon material has serious quality loss, the process energy consumption is increased, and the like.
(4) The low-temperature plasma method is a surface modification technology developed mainly aiming at the quality loss of a carbon material caused by the modification of the activated carbon by a thermal oxidation method, has the advantages of promoting the surface of a solid material to generate the change of physical and chemical properties, can be applied to the research in the fields of adsorbent modification, catalyst preparation, membrane material surface modification and the like, and has wider application range; the disadvantage is that the gas molecules can be ionized into aggregates of electrons, ions, atoms, molecules, radicals and the like by energy supply such as external electric field or radiation.
(5) The solid-solid ion exchange method (molecular monolayer spontaneous dispersion) has the advantages that energy is not needed, metal oxides and salts can be maximally dispersed on the surface of a solid matrix in a monolayer form (close to the dispersion threshold value) by utilizing the thermodynamic spontaneous principle, and the method has important significance for supported catalysts and adsorbents with high dispersed active components. The disadvantage is that the salt to support ratio is such that the amount of salt required to cover the support surface, assuming a strict monolayer, is satisfied, so that the BET surface area of the support must first be determined.
Disclosure of Invention
The invention aims to provide a method for improving a pore structure of a material aiming at the defects in the prior art, and the method has the characteristics of low modification cost, simplicity in operation, low equipment requirement and low energy consumption.
The technical scheme is as follows:
a method of modifying the pore structure of a material comprising the steps of:
the method comprises the following steps: taking a proper amount of an adsorption material into a wide-mouth stainless steel container, wherein the adsorption material is an inorganic porous material or an organic porous material;
step two: slowly adding liquid nitrogen into the stainless steel container, sealing the stainless steel container with a cover, and reacting for the time after the liquid nitrogen is added until the liquid nitrogen is naturally evaporated;
step three: and after the adsorbing material in the second step is naturally heated to the room temperature, repeating the second step for 1-4 times.
Further, the inorganic porous material is one of natural zeolite, artificial zeolite or fly ash; the organic porous material is biochar or activated carbon.
Further, when the adsorbing material is an inorganic porous material, after liquid nitrogen is added in the second step, the stacking volume ratio of the inorganic porous material to the liquid nitrogen is 1: 5-200; when the adsorbing material is an organic porous material, liquid nitrogen is added in the second step, and the stacking volume ratio of the organic porous material to the liquid nitrogen is 1: 1-50.
Further, the inorganic porous material is natural zeolite, and the organic porous material is blue algae biochar.
After the metal salt is added in the method for improving the pore structure of the material, the method for improving the pore structure of the material comprises the following steps:
the method comprises the following steps: taking a proper amount of an adsorption material into a wide-mouth stainless steel container, wherein the adsorption material is an inorganic porous material or an organic porous material;
step two: adding a proper amount of metal salt into a stainless steel container, slowly adding liquid nitrogen, sealing the stainless steel container with a cover, and reacting for the time after the liquid nitrogen is added until the liquid nitrogen is naturally evaporated;
step three: and after the adsorbing material in the second step is naturally heated to the room temperature, repeating the second step for 1-3 times, wherein the amount of the added metal salt is zero or is gradually reduced by half each time the second step is repeated.
Further, the mass ratio of the adsorbing material to the metal salt is 1: 0.1 to 5.
Further, the metal salt is one or more of polyaluminium chloride, potassium hydroxide, zinc chloride, aluminum sulfate and zero-valent iron;
further, the stacking volume ratio of the inorganic porous material to the liquid nitrogen is 1: 5-100, and the stacking volume ratio of the organic porous material to the liquid nitrogen is 1: 1-50.
Has the advantages that: the method for improving the pore structure of the material has the advantages of low cost, simple operation, no need of extra energy consumption and special instruments and equipment, and simple operation.
Drawings
FIG. 1 is the adsorption and desorption isotherm curves of natural zeolite and liquid nitrogen modified natural zeolite.
FIG. 2 is an adsorption and desorption isothermal curve of cyanobacteria biochar and liquid nitrogen modified cyanobacteria biochar.
Detailed Description
The technical solution of the present invention is described in detail below with reference to the accompanying drawings, but the scope of the present invention is not limited to the embodiments.
The invention provides a method for improving a pore structure of a material, and particularly relates to a method for modifying an adsorption material by using low-temperature liquid nitrogen in a low-temperature environment so as to improve the pore structure of the material.
Modified adsorbing material in ultralow-temperature liquid nitrogen low-temperature environment
1. The method comprises the following steps:
the method comprises the following steps: taking a proper amount of adsorbing material to a stainless steel container (the container mouth is wide-mouth type, and cannot be small-mouth type, and the small-mouth type container is easy to cause bumping phenomenon);
the adsorption material is an inorganic porous material and an organic porous material, the inorganic porous material is natural zeolite, artificial zeolite, fly ash and the like, and the organic porous material is various biochar (biochar of various raw materials) and various activated carbon (biochar of various raw materials and shapes: column, particle, powder and the like);
step two: slowly adding liquid nitrogen into a stainless steel container;
when the adsorbing material is an inorganic porous material, the stacking volume ratio of the inorganic porous material to liquid nitrogen is 1: 5-200; when the adsorbing material is an organic porous material, the stacking volume ratio of the organic porous material to liquid nitrogen is 1: 1-50;
sealing a cover of the stainless steel container to reduce the evaporation of liquid nitrogen and improve the utilization rate of the liquid nitrogen, wherein the reaction time is after the liquid nitrogen is added until the liquid nitrogen is naturally evaporated;
and (5) after the adsorbing material in the second step is naturally heated (the temperature of the material is extremely low when the second step is finished) to room temperature, repeating the second step for 1-4 times according to the requirements of the specific surface, the pore volume and the pore diameter of the material.
2. The principle is as follows: the boiling effect of the evaporation of liquid nitrogen (at the temperature of 77K) at normal temperature and normal pressure is utilized to realize the medium mixing between the liquid nitrogen and the material, and the low-temperature liquid nitrogen gasification process can perform pore canal dredging and micropore re-manufacturing on the material to a certain extent. However, as the number of repetitions of the steps increases, the material structure becomes brittle and the strength becomes low. The number of repetitions of step two is controlled appropriately. The method has the advantages of low cost, simple operation, no need of additional energy consumption, no introduction of new substances, colorless modifier, no odor, no corrosivity, incombustibility, no toxicity, no secondary pollution and the like, does not need special instruments and equipment, and is simple to operate.
Secondly, adding metal salt modified adsorption material in the ultra-low temperature liquid nitrogen environment
1. The method comprises the following steps:
the method comprises the following steps: taking a proper amount of adsorbing material to a stainless steel container (the container mouth must be wide-mouthed, and cannot be small-mouthed, otherwise bumping);
the adsorption material is an inorganic porous material and an organic porous material, the inorganic porous material is natural zeolite, artificial zeolite, fly ash and the like, and the organic porous material is various biochar (biochar of various raw materials) and various activated carbon (biochar of various raw materials and shapes: column, particle, powder and the like);
step two: adding a proper amount of metal salt into a stainless steel container, wherein the metal salt is one or more of polyaluminium chloride, potassium hydroxide, zinc chloride, aluminum sulfate and zero-valent iron; the mass ratio of the adsorbing material to the metal salt is 1: 0.1 to 5;
slowly adding liquid nitrogen, wherein the stacking volume ratio of the inorganic porous material to the liquid nitrogen is 1: 5-100, and the stacking volume ratio of the organic porous material to the liquid nitrogen is 1: 1-50; sealing a cover of the stainless steel container to reduce the evaporation of liquid nitrogen and improve the utilization rate of the liquid nitrogen, wherein the reaction time is till the natural evaporation of the liquid nitrogen is finished;
step three: and after the adsorbing material in the second step is naturally heated (the temperature of the material is extremely low when the second step is finished) to room temperature, repeating the second step for 1-3 times according to the requirements of the specific surface, the pore volume and the pore diameter of the material, and when the second step is repeated each time, reducing the amount of the added metal salt to zero or half step by step.
2. The principle is as follows:
in a liquid nitrogen environment at an ultralow temperature, metal has special cold medium physical characteristics, the surface characteristics of the adsorption material can be changed, medium mixing between liquid nitrogen and the adsorption material is realized by utilizing the boiling effect of the liquid nitrogen (at 77K, namely-196 ℃) during evaporation at normal temperature and normal pressure, and the low-temperature liquid nitrogen gasification process can perform pore channel dredging and micropore re-manufacturing on the material to a certain extent. However, the more the number of repetition steps is, the more the material structure becomes brittle and the strength becomes low. The number of repetitions of step two is controlled appropriately. The method is simple to operate, does not need to additionally increase energy consumption, and does not need special instruments and equipment.
Example one: modification of natural zeolite under ultralow temperature liquid nitrogen low temperature environment
The modification steps are as follows:
the method comprises the following steps: taking 50g of natural zeolite, and placing the natural zeolite in a 500ml stainless steel container;
step two: slowly adding 100ml of liquid nitrogen into the stainless steel container, standing at normal temperature and normal pressure without stirring, and sealing the stainless steel container until the liquid nitrogen is evaporated;
step three: and after the natural zeolite is naturally heated to the room temperature, slowly adding 100ml of liquid nitrogen into the stainless steel container again, standing at the normal temperature and the normal pressure without stirring, and sealing the stainless steel container by a cover until the liquid nitrogen is completely evaporated.
In the first embodiment: the natural zeolite has a bulk volume of 50g/(2.3 g/cm)3)＝21.7cm3When the total amount of liquid nitrogen used was 200ml, and the bulk volume ratio of natural zeolite to liquid nitrogen was 1:10, the cost of liquid nitrogen for modifying 1.0kg of natural zeolite was about 4.4 yuan.
The modification results are shown in figure 1 and table 1: fig. 1 is an adsorption-desorption isothermal curve of natural zeolite and modified natural zeolite, and the adsorption and desorption capacities of the modified natural zeolite are obviously increased.
Table 1 shows the specific surface area, pore volume and pore diameter parameters of the natural zeolite and the liquid nitrogen modified natural zeolite, and the BET specific surface area of the natural zeolite is from 24.87cm after the liquid nitrogen modification2The/g is increased to 83.16cm2Per g, the adsorption pore volume is 0.0441cm3The/g is increased to 0.1963cm3The diameter of the pore opening is slightly changed from 7.09413nm to 7.64523 nm.
TABLE 1 Zeolite and liquid nitrogen modified Natural Zeolite specific surface area, pore volume and pore size parameters
Example two: modification of blue algae biochar in ultralow liquid nitrogen low-temperature environment
The modification steps are as follows:
the method comprises the following steps: taking 50g of blue algae biochar, and placing the blue algae biochar in a 500ml stainless steel container;
step two: respectively adding polyaluminium chloride and potassium hydroxide into a stainless steel container according to 15% and 5.0% of the weight of the blue algae biochar;
adding 125ml of liquid nitrogen slowly into the stainless steel container, standing at normal temperature and normal pressure without stirring, and sealing the stainless steel container until the liquid nitrogen is evaporated;
step three: after the blue algae biochar naturally rises to the room temperature, slowly adding 125ml of liquid nitrogen again, standing at the normal temperature and the normal pressure without stirring, and sealing a cover of the stainless steel container until the liquid nitrogen is completely evaporated.
The second example shows that the stacking volume of 5g of cyanobacteria biochar is 50g/(0.4 g/cm)3)＝125cm3When the total usage amount of the liquid nitrogen is 125ml, the stacking volume ratio of the cyanobacteria biochar to the liquid nitrogen is 1:2, the cost of the modified 1.0kg of cyanobacteria biochar liquid nitrogen is about 5.0 yuan.
The modification results are shown in fig. 2 and table 2: FIG. 2 is an adsorption-desorption isothermal curve of cyanobacteria biochar and modified cyanobacteria biochar, and the adsorption and desorption capacity of the modified cyanobacteria biochar is increased.
Table 2 shows the specific surface area, pore volume and pore diameter parameters of the cyanobacteria biochar and the liquid nitrogen modified cyanobacteria biochar, and the BET specific surface area of the cyanobacteria biochar is 1.3076cm after liquid nitrogen modification2The/g is increased to 1.6965cm2Per g, the adsorption pore volume is 0.004301cm3The/g is increased to 0.009013cm3The pore diameter changed a large amount from 7.14528nm to 12.65291 nm.
TABLE 2 specific surface area, pore volume and pore diameter parameters of cyanobacterial biochar and liquid nitrogen modified cyanobacterial biochar
The industrial liquid nitrogen is about 1.0 yuan/L, and the density of the natural zeolite is 2.3g/cm3The equipment is a common stainless steel container, the cost is low, and other special equipment is not needed.
As noted above, while the present invention has been shown and described with reference to certain preferred embodiments, it is not to be construed as limited thereto. Various changes in form and detail may be made therein without departing from the spirit and scope as defined by the appended claims.
Claims (4)
1. A method of modifying the pore structure of a material, comprising the steps of:
the method comprises the following steps: taking a proper amount of an adsorption material into a wide-mouth stainless steel container, wherein the adsorption material is an inorganic porous material or an organic porous material; the inorganic porous material is one of natural zeolite, artificial zeolite or fly ash; the organic porous material is biochar or activated carbon;
step two: slowly adding liquid nitrogen into the stainless steel container, sealing the stainless steel container with a cover, and reacting for the time after the liquid nitrogen is added until the liquid nitrogen is naturally evaporated;
when the adsorbing material is an inorganic porous material, the stacking volume ratio of the inorganic porous material to liquid nitrogen is 1: 5-200; when the adsorbing material is an organic porous material, the stacking volume ratio of the organic porous material to liquid nitrogen is 1: 1-50;
step three: and after the adsorbing material in the second step is naturally heated to the room temperature, repeating the second step for 1-4 times.
2. The method for improving the pore structure of a material according to claim 1,
the method comprises the following steps: taking a proper amount of an adsorption material into a wide-mouth stainless steel container, wherein the adsorption material is an inorganic porous material or an organic porous material;
step two: adding a proper amount of metal salt into a stainless steel container, slowly adding liquid nitrogen, sealing the stainless steel container with a cover, and reacting for the time after the liquid nitrogen is added until the liquid nitrogen is naturally evaporated; the mass ratio of the adsorbing material to the metal salt is 1: 0.1 to 5; the stacking volume ratio of the inorganic porous material to the liquid nitrogen is 1: 5-100, and the stacking volume ratio of the organic porous material to the liquid nitrogen is 1: 1-50;
step three: and after the adsorbing material in the second step is naturally heated to the room temperature, repeating the second step for 1-3 times, wherein the amount of the added metal salt is zero or is gradually reduced by half each time the second step is repeated.
3. The method for improving the pore structure of a material according to claim 2, wherein the metal salt is one or more of polyaluminium chloride, potassium hydroxide, zinc chloride, aluminium sulphate, zero valent iron.
4. The method for improving the pore structure of a material according to claim 1, wherein the inorganic porous material is natural zeolite, and the organic porous material is cyanobacteria biochar.
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| Structural characteristics of a carbon adsorbent and influence of organic solvents on interfacial water;Gun"ko, VM et al.;《Applied Surface Science》;20030405;第214卷(第1-4期);第178-189页 * |
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