CN115400730A - Corrosive atmosphere absorbing material, preparation method and application thereof - Google Patents
Corrosive atmosphere absorbing material, preparation method and application thereof Download PDFInfo
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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
- B01J20/20—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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
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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
- B01J20/28014—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 form
- B01J20/28023—Fibres or filaments
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2257/00—Components to be removed
- B01D2257/20—Halogens or halogen compounds
- B01D2257/204—Inorganic halogen compounds
- B01D2257/2045—Hydrochloric acid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/30—Sulfur compounds
- B01D2257/302—Sulfur oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
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- B01D2257/304—Hydrogen sulfide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/40—Nitrogen compounds
Abstract
The invention provides a corrosive atmosphere absorbing material with high adsorption capacity to corrosive atmosphere and good safety, and provides a preparation method and application of the material. The corrosive atmosphere absorbing material is prepared by dipping activated carbon fiber in hydrogen peroxide and nitrate solution and then drying and roasting; the preparation method comprises the working procedures of boiling the activated carbon fiber, drying, soaking in hydrogen peroxide, soaking in nitrate solution and roasting, and the prepared corrosive atmosphere absorbing material is applied to a packing box. The corrosive atmosphere absorbing material prepared by the invention has high adsorption capacity, can effectively absorb corrosive atmosphere with the concentration within 10ppm, is particularly suitable for absorbing corrosive atmosphere in a packaging box, and has good safety and good corrosive atmosphere absorbing effect.
Description
Technical Field
The invention relates to a technology for treating corrosive atmosphere in a packing box, in particular to a corrosive atmosphere absorbing material, a preparation method and application thereof.
Background
Metal-containing products such as weaponry, electronic components and the like are generally stored, transported and even used in packaging boxes, and particularly, during the storage process, the products in the packaging boxes are susceptible to irreversible corrosive damage caused by the synergistic effect of water vapor and corrosive atmosphere (SO 2, NOx, HCl, H2S and the like), and although the concentration of the corrosive atmosphere in the packaging boxes is low, the products belong to the key factors of the corrosive damage of the products. At present, in most occasions, a drying agent is placed in a packaging box to prevent products from being corroded and damaged, the corrosion is slowed down by absorbing water vapor in the packaging box, and few materials are used for preventing the products from being corroded and damaged by absorbing corrosive atmosphere.
The prior art related to corrosive atmosphere adsorption mainly relates to the treatment of polluted gas in the field of air treatment/treatment, such as activated carbon fiber adsorption materials, silicate or silicon-based adsorption materials loaded with photocatalyst, diatomite, cementing materials, inorganic fillers, inorganic environment-friendly pigments and inorganic framework materials. However, the existing materials mainly treat high-concentration harmful gas and dust in the area to be treated to reach the standard, such as the conventional activated carbon fiber adsorbing material has low adsorption capacity to corrosive atmosphere (for example, SO) 2 、NO 2 The adsorption capacity of NO usually does not exceed 65 mg/g) and is not suitable for adsorbing corrosive atmospheres in packaging boxes.
Research shows that the adsorption material containing polyvinyl alcohol, soda lime, adhesive, water and other substances can perform a better adsorption effect on typical harmful gases when applied to a closed space, and the average adsorption capacity reaches 97.1%. However, when the material is used in a packaging box for storing weapons and ammunition, there is a problem that the danger coefficient is large and the safety is poor.
Disclosure of Invention
In view of the technical problems mentioned in the background art, the invention aims to provide a corrosive atmosphere absorption material with high adsorption capacity to corrosive atmosphere and good safety, and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows.
The corrosive atmosphere absorbing material is prepared with active carbon fiber and through soaking in hydrogen peroxide solution and nitrate solution, stoving and roasting, and features the active carbon fiber comprising viscose-base active carbon fiber, PAN-base active carbon fiber, phenolic resin-base active carbon fiber and asphalt-base active carbon fiber, hydrogen peroxide solution in 10-35 wt% and nitrate solution in metal ion concentration of 5-25 wt%.
Preferably, the nitrate solution is prepared by mixing 0.5-10 parts of copper nitrate and 0.5-10 parts of ferric nitrate according to the weight part ratio.
More preferably, the activated carbon fiber is composed of 1 part by weight of a viscose-based activated carbon fiber, 1 part by weight of a PAN-based activated carbon fiber, 1 part by weight of a phenol resin-based activated carbon fiber, and 1 part by weight of a pitch-based activated carbon fiber.
More preferably, the concentration of the hydrogen peroxide solution is 30wt%, the concentration of the metal ions in the nitrate solution is 10wt%, and the nitrate solution is formed by mixing 1 part of copper nitrate and 1 part of ferric nitrate according to the weight part ratio.
The preparation method of the corrosive atmosphere absorption material comprises the following steps:
3, placing the activated carbon fiber treated in the step 2 in a nitrate solution for soaking for 24 +/-1 h, carrying out ultrasonic treatment for 30 +/-5 min in the soaking process, filtering after the soaking is finished, and collecting fiber materials;
and 4, drying the obtained fiber material in an atmosphere of 50 +/-5 ℃ for 6 hours, then drying the fiber material in an atmosphere of 100 +/-5 ℃ for 6 hours, and finally roasting the fiber material in a nitrogen atmosphere at the temperature of 250 +/-5 ℃ for 2 +/-0.2 hours to obtain the corrosive atmosphere absorbing material.
Preferably, at least 200mL of the impregnation solution is prepared per 10g of the activated carbon fiber.
Furthermore, when the activated carbon fibers are combined, the surface layer adopts viscose-based activated carbon fibers, the other layers are PAN-based activated carbon fibers, phenolic resin-based activated carbon fibers and asphalt-based activated carbon fibers from top to bottom, and the thickness of each layer of activated carbon fibers in a free state is not more than 15mm.
The application of the corrosive atmosphere absorbing material prepared by the invention is that the corrosive atmosphere absorbing material is placed in a packaging box.
As a preferred application, the specification of the packaging box is that the corrosive atmosphere in the packaging box is not higher than 20ppm.
As a preferred application, the corrosive atmosphere absorbing material is attached to the inner wall of a packaging box for storing flammable and explosive articles.
Has the beneficial effects that: the corrosive atmosphere absorbing material prepared by the invention has higher adsorption capacity to various corrosive atmospheres and SO 2 、NO 2 、NO、HCl、H 2 The adsorption capacity of S can reach 110mg/g, 153mg/g, 128mg/g, 215mg/g and 210mg/g respectively, which is much higher than that of the prior conventional activated carbon fiber adsorption material; the corrosive atmosphere absorbing material prepared by the invention can effectively absorb corrosive atmosphere with the concentration within 10ppm, is particularly suitable for absorbing corrosive atmosphere in a packing box, and has good safety and good corrosive atmosphere absorbing effect.
Drawings
FIG. 1 is a surface topography of an activated carbon fiber in an example, wherein (a) is a topography of a viscose-based activated carbon fiber and (b) is a topography of an aggressive atmosphere absorbent material (viscose-based activated carbon fiber) prepared in example 3;
FIGS. 2 to 4 are graphs showing adsorption curves of the corrosive atmosphere absorbent in examples 1, 2 and 3, respectively;
FIG. 5 shows the change of the concentration of the corrosive atmosphere in the packaging container according to examples 1 to 3.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific embodiments, but the following embodiments are only used for understanding the principle of the present invention and the core idea thereof, and do not limit the scope of the present invention. It should be noted that modifications to the invention as described herein, which do not depart from the principles of the invention, are intended to be within the scope of the claims which follow. In the present invention, viscose-based activated carbon fiber (available from Jiangsu Sutong carbon fiber Co., ltd., SFT-1300), PAN-based activated carbon fiber (available from Nantong Senyou carbon fiber Co., ltd., SY-ACF-1001), phenol resin-based activated carbon fiber (available from Nantong Jin Heng environmental protection technology Co., ltd. (custom made), and total pore volume is 1.25 (ml.g.) -1 ) Total specific surface area 1200m 2 .g -1 Average pore diameter of 15-20 nm), asphalt-based activated carbon fibers (self-made), and the thickness of each activated carbon fiber is 10mm; the preparation process of the asphalt-based activated carbon fiber comprises the following steps: cleaning the asphalt fiber cloth with distilled water, soaking in acetone for 5 hours, and then airing; placing asphalt fibers in an oxygen environment at 200 ℃, heating to 400 ℃, keeping for 4 hours, taking out and cooling, putting the cooled asphalt fiber cloth into phosphate solution for soaking for 7 hours, heating the phosphate solution to 120-125 ℃, keeping for 3 hours, taking out the asphalt fiber cloth, drying, sending the asphalt fiber cloth into carbonization equipment filled with nitrogen, heating to 810 +/-5 ℃, introducing carbon dioxide, stopping introducing the carbon dioxide, introducing water vapor, and heating to 900 +/-5 ℃; stopping heating, naturally cooling, taking out, air-cooling, washing with water to neutrality, oven drying, and cutting into required specification.
Example 1
The corrosive atmosphere absorbing material is prepared by dipping activated carbon fibers in hydrogen peroxide and copper nitrate solution, and then drying and roasting, wherein the activated carbon fibers are viscose-based activated carbon fibers, the concentration of the hydrogen peroxide solution is 10wt%, and the concentration of metal ions in the copper nitrate solution is 5wt%.
The preparation method of the corrosive atmosphere absorbing material in the embodiment comprises the following steps:
3, placing the activated carbon fiber treated in the step 2 in a copper nitrate solution for soaking for 24 hours, carrying out ultrasonic treatment for 30min in the soaking process, filtering after the soaking is finished, and collecting fiber materials;
and 4, drying the obtained fiber material in an atmosphere of 50 ℃ for 6h, then drying the fiber material in an atmosphere of 100 ℃ for 6h, and finally roasting the fiber material in a nitrogen atmosphere at the temperature of 250 ℃ for 2h to obtain the corrosive atmosphere absorbing material.
Example 2
The corrosive atmosphere absorbing material is prepared by impregnating activated carbon fibers with hydrogen peroxide and a copper nitrate solution, drying and roasting, wherein the activated carbon fibers are formed by combining 1 part of viscose-based activated carbon fibers, 1 part of PAN-based activated carbon fibers, 1 part of phenolic resin-based activated carbon fibers and 1 part of asphalt-based activated carbon fibers, the concentration of the hydrogen peroxide solution is 10wt%, and the concentration of metal ions in the copper nitrate solution is 10wt%.
The preparation method of the corrosive atmosphere absorbing material in the embodiment comprises the following steps:
3, placing the activated carbon fiber treated in the step 2 in a copper nitrate solution for soaking for 24 hours, carrying out ultrasonic treatment for 30min in the soaking process, filtering after the soaking is finished, and collecting fiber materials;
and 4, drying the obtained fiber material in an atmosphere of 50 ℃ for 6h, then drying the fiber material in an atmosphere of 100 ℃ for 6h, and finally roasting the fiber material in a nitrogen atmosphere at the temperature of 250 ℃ for 2h to obtain the corrosive atmosphere absorbing material.
Example 3
The corrosive atmosphere absorbing material is prepared by impregnating activated carbon fibers with hydrogen peroxide and a nitrate solution, drying and roasting, wherein the activated carbon fibers are formed by combining 1 part of viscose-based activated carbon fibers, 1 part of PAN-based activated carbon fibers, 1 part of phenolic resin-based activated carbon fibers and 1 part of asphalt-based activated carbon fibers, the concentration of the hydrogen peroxide solution is 30wt%, the concentration of metal ions in the nitrate solution is 10wt%, and the nitrate solution is formed by mixing 1 part of copper nitrate and 1 part of ferric nitrate according to the weight part ratio.
The preparation method of the corrosive atmosphere absorbing material in the embodiment comprises the following steps:
3, placing the activated carbon fiber treated in the step 2 in a nitrate solution for soaking for 24 hours, carrying out ultrasonic treatment for 30min in the soaking process, filtering after the soaking is finished, and collecting fiber materials;
and 4, drying the obtained fiber material in an atmosphere of 50 ℃ for 6h, then drying the fiber material in an atmosphere of 100 ℃ for 6h, and finally roasting the fiber material in a nitrogen atmosphere at the temperature of 250 ℃ for 2h to obtain the corrosive atmosphere absorbing material, wherein the shape of the corrosive atmosphere absorbing material is shown as part (b) in figure 1, and obvious strip-shaped grooves can be seen on each viscose-based active carbon fiber.
Comparative example 1
A corrosive atmosphere absorbing material directly adopts commercially available viscose-based activated carbon fiber.
Comparative example 2
A corrosive atmosphere absorbing material directly adopts commercially available sticky asphalt-based active carbon fiber.
The corrosive atmosphere absorbing materials prepared in the respective examples were sampled and subjected to adsorption capacity test, and the test results are shown in table 1 and fig. 2 to 5. In example 1, comparative example 1 and comparative example 2, the corrosive atmosphere absorbing material samples were all four stacked structures of the same material, namely, four layers of activated carbon fibers were stacked to form the samples, and the corrosive atmosphere absorbing material samples in example 2 and example 3 were all four stacked structures of different materials, wherein the surface layer was made of viscose-based activated carbon fibers, and the remaining layers were made of PAN-based activated carbon fibers, phenol resin-based activated carbon fibers and pitch-based activated carbon fibers in this order from top to bottom, and the specification of each layer of activated carbon fibers was 50mm (length) 50mm (width) 10mm (thickness).
SO 2 、NO X The method for calculating the adsorption performance comprises the following steps:
(1) Preparing a sulfur dioxide/nitrogen dioxide/helium monoxide atmosphere with the concentration of about 1000ppm, testing and recording the initial concentration as C, and closing the gas valve;
(2) Adjusting the pressure, temperature and humidity in the reaction vessel to be respectively standard atmospheric pressure, 25 ℃, 40% RH in real time;
(3) Before the test, the sample of the adsorbent material is weighed and recorded as m (to the nearest 0.001 g), and then placed in an adsorption column (note: the sample is not allowed to contact air for a long time in the operation process);
(4) Open the gas valve, measure the outlet gas concentration, record the atmosphere concentration C once per minute 1 、C 2 ……C n ;
(5) When the concentration of the outlet corrosive atmosphere is the same as that of the inlet corrosive atmosphere, stopping the test and calculating the adsorption capacity according to the following formula;
wherein q is gas adsorption capacity in mg/g; c is the real-time concentration of the adsorbed gas in ppm; q is gas flow rate, unit ml/min, M is relative molecular mass of adsorbed gas, unit g/mol; v is the standard state molar volume, 22.4ml/mol; m ACF The unit is the mass of the activated carbon fiber, and the unit is g; t is the adsorption time, min.
HC1、H 2 The S adsorption performance calculation method comprises the following steps:
(1) The absorbent material sample was weighed before testing and recorded as m 1 (to the nearest 0.001 g) and then placed in an adsorption column (note: the sample is not allowed to contact air for a long time during this operation);
(2) The gas valve was opened and H was introduced at a concentration of about 1000ppm 2 The test was stopped in an S/HC1 atmosphere for 12 hours, and the sample of the adsorbent was weighed and recorded as m 2 And calculating the adsorption capacity according to the following formula;
wherein q is gas adsorption capacity in mg/g; m is a unit of 1 Is the mass of the sample of the dried adsorption material before the test, in g; m is 2 The mass of the sample of the adsorbent after adsorbing the corrosive atmosphere is expressed in g.
TABLE 1 results of measuring adsorption capacity in corrosive atmosphere
It can be seen that the corrosive atmosphere absorbing material prepared in the examples has high adsorption capacity to SO 2 、NO 2 、NO、HCl、H 2 The adsorption capacity of S can reach 110mg/g, 153mg/g, 128mg/g, 215mg/g and 210mg/g respectively, which is much higher than that of the prior conventional activated carbon fiber adsorption material.
The corrosive atmosphere absorbing materials prepared in examples 1 to 3 were sampled and subjected to an adsorption capacity test. In example 1, the corrosive atmosphere absorbing material samples are all four layers of the same material stacking structure with the length of 50mm by width of 10mm, in example 2 and example 3, the corrosive atmosphere absorbing material samples are all four layers of different material stacking structures, the surface layer adopts viscose-based activated carbon fibers, the rest layers are sequentially PAN-based activated carbon fibers, phenolic resin-based activated carbon fibers and asphalt-based activated carbon fibers from top to bottom, and the specification of each layer of activated carbon fibers is 50mm by length of 50mm by width of 10 mm. The corrosive atmosphere absorbing material samples of 100 + -0.3 g were taken and attached to the inner wall of a package box (outer dimension: 2100 mm. Times.900 mm. Times.750 mm) having a detection sensor, and a predetermined amount of test gas was introduced into the package box after the package box was sealed, and the corrosive atmosphere concentration was recorded at regular time, and the results are shown in FIG. 1. The result shows that the prepared corrosive atmosphere absorption material can effectively absorb the corrosive atmosphere with the concentration within 10ppm, is particularly suitable for absorbing the corrosive atmosphere in a packing box, and has good safety and good corrosive atmosphere absorption effect.
Claims (10)
1. A corrosive atmosphere absorbing material characterized by: the activated carbon fiber is prepared by impregnating activated carbon fibers with hydrogen peroxide and nitrate solution and then drying and roasting, wherein the activated carbon fibers are formed by combining one or more of viscose-based activated carbon fibers, PAN-based activated carbon fibers, phenolic resin-based activated carbon fibers and asphalt-based activated carbon fibers, the concentration of the hydrogen peroxide solution is 10-35 wt%, and the concentration of metal ions in the nitrate solution is 5-25 wt%.
2. The corrosive atmosphere absorbing material according to claim 1, wherein: the nitrate solution is prepared by mixing 0.5-10 parts of copper nitrate and 0.5-10 parts of ferric nitrate according to the weight part ratio.
3. The corrosive atmosphere absorbing material according to claim 2, wherein: the activated carbon fiber is formed by combining 1 part of viscose-based activated carbon fiber, 1 part of PAN-based activated carbon fiber, 1 part of phenolic resin-based activated carbon fiber and 1 part of asphalt-based activated carbon fiber according to the weight part ratio.
4. A corrosive atmosphere absorbing material according to any one of claims 1 to 3, wherein: the concentration of the hydrogen peroxide solution is 30wt%, the concentration of metal ions in the nitrate solution is 10wt%, and the nitrate solution is formed by mixing 1 part of copper nitrate and 1 part of ferric nitrate according to the weight part ratio.
5. A method for the preparation of a corrosive atmosphere absorbing material according to any of claims 1 to 4, comprising the steps of:
step 1, respectively placing viscose-based activated carbon fibers, PAN-based activated carbon fibers, phenolic resin-based activated carbon fibers and asphalt-based activated carbon fibers in 100 ℃ boiling water for boiling for 0.45-0.55h, then placing each activated carbon fiber in a 100 ℃ vacuum drying oven for drying for 12 +/-1 h, and then naturally cooling for later use;
step 2, combining the activated carbon fibers treated in the step 1 according to the proportion, placing the combined activated carbon fibers in a hydrogen peroxide solution for soaking for 24 +/-1 h, carrying out ultrasonic treatment for 30 +/-5 min in the soaking process, filtering after the soaking is finished, and washing with distilled water;
3, placing the activated carbon fiber treated in the step 2 in a nitrate solution for soaking for 24 +/-1 h, carrying out ultrasonic treatment for 30 +/-5 min in the soaking process, filtering after the soaking is finished, and collecting fiber materials;
and 4, drying the obtained fiber material in an atmosphere of 50 +/-5 ℃ for 6 hours, then drying the fiber material in an atmosphere of 100 +/-5 ℃ for 6 hours, and finally roasting the fiber material in a nitrogen atmosphere at the temperature of 250 +/-5 ℃ for 2 +/-0.2 hours to obtain the corrosive atmosphere absorbing material.
6. The method of claim 5, wherein: at least 200mL of impregnation solution is prepared per 10g of activated carbon fiber.
7. The method of claim 6, wherein: when the activated carbon fibers are combined, the surface layer adopts viscose-based activated carbon fibers, the inner layer sequentially comprises PAN-based activated carbon fibers, phenolic resin-based activated carbon fibers and pitch-based activated carbon fibers, and the thickness of each layer of activated carbon fibers in a free state is not more than 15mm.
8. Use of a corrosive atmosphere absorbing material prepared by the method according to any one of claims 5 to 7, wherein: placing the corrosive atmosphere absorbing material in a packaging box.
9. The use of claim 8, wherein: the specification of the packaging box is that the corrosive atmosphere in the packaging box is not higher than 20ppm.
10. The use of claim 9, wherein: the corrosive atmosphere absorbing material is attached to the wall of the packing box for storing inflammable and explosive articles.
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