CN111729651A - Preparation method of formaldehyde adsorbent based on vermiculite - Google Patents
Preparation method of formaldehyde adsorbent based on vermiculite Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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Abstract
The invention discloses a preparation method of a vermiculite-based formaldehyde adsorbent, which comprises the following steps: (1) dissolving chitosan in water, and adding hydrochloric acid to obtain an acidified chitosan solution; (2) mixing vermiculite powder and an acidified chitosan solution, stirring and irradiating low-temperature plasma to obtain carbon chain loaded vermiculite flake slurry, drying, grinding and sieving to obtain carbon chain loaded vermiculite flake powder; (3) and (3) irradiating the carbon chain loaded vermiculite flake powder by low-temperature plasma to obtain the vermiculite-based formaldehyde adsorbent. The vermiculite-based formaldehyde adsorbent prepared by the invention can realize 98% of formaldehyde removal rate; the preparation process involves few chemical reagents; the adsorbent has low cost, simple preparation process and no secondary pollution, solves the problems of secondary pollution and advanced treatment in the traditional modification method, and is suitable for industrial production; the carbon chain amination is realized by ammonia gas, and the use of an amino-containing chemical reagent is avoided.
Description
Technical Field
The invention relates to a preparation method of a formaldehyde adsorbent, in particular to a preparation method of a vermiculite-based formaldehyde adsorbent.
Background
Some building materials in home decoration release formaldehyde which is used as a primary toxic substance, and has toxic and harmful effects on the respiratory system, the immune system, the central nervous system, the cardiovascular system and the reproductive system of a human body, so that the health of the human body is seriously harmed.
Currently, the formaldehyde pollution is mainly treated by applying biocatalysis, photocatalysis and plasma technologies. The methods have advantages and disadvantages, and the biological catalysis method has the problems of small aldehyde absorption amount of vegetation, large seasonal influence and low aldehyde removal efficiency. The photocatalysis utilizes electron hole pairs generated on the surface of a semiconductor to treat formaldehyde, has high formaldehyde removal efficiency, but limits the large-scale popularization and application of the photocatalysis technology due to the problem that the preparation cost of an ultraviolet irradiation device and the preparation cost of the current catalytic material is relatively high. Plasma technology is suitable for removing high concentrations of formaldehyde in industrial environments, but its electromagnetic radiation problems limit its application in domestic locations.
In recent years, physical chemical adsorption is widely used for treating pollutants due to the characteristics of simple operation, strong technical compatibility, wide application range and the like, and the physical chemical adsorption adsorbs the pollutants on adsorbates through hydrogen bonds, van der waals forces, chemical bonds and other mechanisms. The development of materials with high formaldehyde adsorption performance by using conventional mineral raw materials has become a current heat generation point. Vermiculite is an easily available and inexpensive layered clay, a silicate, and has a shape similar to mica. The vermiculite has good stability and a layered structure, and is an ideal adsorbent carrier material. The application of vermiculite to prepare the adsorbing material relates to the stripping and surface modification processes. A large amount of acid reagents and layer-inserting reagents are needed in the process of peeling the vermiculite, secondary pollution is easily caused in the process of cleaning the acid reagents and the layer-inserting reagents, and chemical reagents which are washed down need to be deeply treated. Meanwhile, the acid reagent and the intercalation reagent which are remained on the vermiculite pieces are easy to generate negative effects on the surface modification of the vermiculite. In addition, the surface modification process of the vermiculite sheet also needs to be soaked with specific chemical reagents, and also needs to be subjected to later separation, cleaning and advanced treatment processes.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems, the invention provides a preparation method of a formaldehyde adsorbent based on vermiculite, which is simple, does not need to use a large amount of acid reagents and layer-inserting reagents, does not cause secondary pollution, uses few types of reagents and has low preparation cost.
The technical scheme is as follows: the preparation method of the formaldehyde adsorbent based on vermiculite comprises the following steps:
(1) dissolving chitosan in water, and adding hydrochloric acid to obtain an acidified chitosan solution;
(2) mixing vermiculite powder and an acidified chitosan solution, stirring and irradiating low-temperature plasma to obtain carbon chain loaded vermiculite flake slurry, drying, grinding and sieving to obtain carbon chain loaded vermiculite flake powder;
(3) and (3) irradiating the carbon chain loaded vermiculite flake powder by low-temperature plasma to obtain the vermiculite-based formaldehyde adsorbent.
Wherein, in the step (1), the solid-to-liquid ratio of the chitosan to the water is 2-8: 100, and the concentration of the hydrochloric acid is 1-3 mol/L.
The solid-liquid ratio of the vermiculite powder to the acidified chitosan solution in the step (2) is 3-9.5: 1, and is further preferably 3-9: 1, wherein the vermiculite powder is obtained by grinding vermiculite and sieving the vermiculite with a 200-400-mesh sieve; the stirring speed is 120-360 rpm; the low-temperature plasma irradiation time is 1-2 h, the action voltage is 3-30 kV, and the action atmosphere is oxygen; the drying temperature of the carbon chain loaded vermiculite slice slurry is 50-150 ℃, and the slurry is sieved by a 200-400 mesh sieve after being ground.
The irradiation time of the low-temperature plasma in the step (3) is 1-2 h, the acting voltage is 3-30 kV, the acting atmosphere is a mixed gas of ammonia gas and argon gas, and the volume ratio of the ammonia gas to the argon gas is 4.5-15.5: 100, and is further preferably 5-15: 100.
The high-voltage electrode releases high-energy electron beams and a large amount of heat in the low-temperature plasma irradiation process, and the high-energy electron beams can enable water molecules to be dissociated and ionized to generate hydrogen radicals, hydroxyl radicals and hydrated electrons; so that oxygen is dissociated to generate oxygen free radicals; so that ammonia gas is dissociated to generate hydrogen free radical, amine free radical and nitrogen free radical. The hydroxyl radical and the oxygen radical can accelerate the dissolution of vermiculite interlamination ions through oxidation, expand vermiculite interlamination distance and promote chitosan molecule intercalation, thereby realizing vermiculite stripping. Meanwhile, hydroxyl radicals and oxygen radicals can break partial chitosan molecule carbon chains to generate carbon chain molecules, and the carbon chain molecules are loaded on the surface of the vermiculite stripping sheet in a plasma grafting mode. Under the acid catalysis environment, hydroxyl radicals and hydrated electrons can induce the vermiculite loaded with the carbon chain to be peeled and gelatinized, so that the stability of the loaded carbon chain is enhanced. The amine free radical and the nitrogen free radical can further react with the vermiculite stripping surface loaded carbon chain molecules to generate organic amine, thereby realizing carbon chain amination. Chitosan molecular chains loaded on vermiculite have two active groups of rich amino and hydroxyl, and can interact with aldehyde groups of formaldehyde to effectively adsorb indoor free formaldehyde.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: (1) the vermiculite-based formaldehyde adsorbent prepared by the invention can realize 98% of formaldehyde removal rate; (2) the vermiculite is modified by low-temperature plasma irradiation, the types of chemical reagents involved in the preparation process are few, only two types of chitosan and hydrochloric acid are used, and the chitosan plays two roles of strengthening vermiculite stripping and surface modification at the same time; (3) the adsorbent is low in cost, simple in preparation process, green and environment-friendly, has no secondary pollution, solves the problems of secondary pollution and advanced treatment in the traditional modification method, and is suitable for industrial production; (4) the invention utilizes ammonia gas to realize carbon chain amination, thereby avoiding the use of an amino-containing chemical reagent.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The invention is further described below with reference to the figures and examples.
Example 1
Influence of solid-liquid ratio of chitosan to water on formaldehyde removal performance of prepared vermiculite-based formaldehyde adsorbent
Preparing a vermiculite-based formaldehyde adsorbent: dissolving chitosan into water according to a solid-to-liquid ratio of the chitosan to the water of 1:100, 1.5:100, 1.8:100, 2:100, 5:100, 8:100, 8.5:100, 9:100 and 10:100(mg: mL) to obtain a chitosan solution, and then dripping hydrochloric acid into the chitosan solution to obtain an acidified chitosan solution, wherein the concentration of the hydrochloric acid in the solution is 1 mol/L; grinding vermiculite, sieving with a 200-mesh sieve to obtain vermiculite powder, mixing the vermiculite powder and an acidified chitosan solution according to the solid-to-liquid ratio of 3:1(mg: mL) of the vermiculite powder to the acidified chitosan solution, continuously stirring at 120rpm, simultaneously irradiating the mixed slurry with low-temperature plasma for 1 hour to obtain carbon chain loaded vermiculite flake slurry, wherein the action voltage of the low-temperature plasma is 3kV, the action atmosphere is oxygen, drying the carbon chain loaded vermiculite flake slurry at 50 ℃, grinding, and sieving with a 200-mesh sieve to obtain carbon chain loaded vermiculite flake powder; and (3) irradiating the carbon chain loaded vermiculite flake powder for 1 hour by using low-temperature plasma to obtain the vermiculite-based formaldehyde adsorbent, wherein the action voltage of the low-temperature plasma is 3kV, the action atmosphere is mixed gas of ammonia gas and argon gas, and the volume ratio of the ammonia gas to the argon gas is 5: 100.
Formaldehyde adsorption test: 5g of vermiculite-based formaldehyde adsorbent is placed in an experimental box, 30mL of formaldehyde gas is injected into the box, the formaldehyde injection port is immediately sealed by an adhesive tape after the formaldehyde gas is injected, and an air sampler on the experimental box is opened after 60 min. Wherein the experimental box is a glass square sealed container with a volume of 0.216m3The center of the upper end face of the experiment box is reserved with a formaldehyde injection hole, and the gas sampler is arranged at the left position of the upper end face of the experiment box.
Determination of formaldehyde mass in the experimental box: adding 5mL of distilled water into an absorption tube of an air sampler, sampling at a flow rate of 0.5L/min for 15min, measuring the concentration (mu g/mL) of formaldehyde in the sampled aqueous solution, detecting the concentration of the formaldehyde in the aqueous solution according to acetylacetone spectrophotometry for measuring water quality formaldehyde (HJ 601-2011), and calculating the mass (mu g) of the formaldehyde in the experimental box according to a formula (1), wherein m is the mass (mu g) of the formaldehyde in the experimental box, and c is the concentration (mu g/mL) of the formaldehyde in the sampled aqueous solution.
Calculation of formaldehyde removal rate: the formaldehyde removal rate in the experimental box was calculated according to formula (2), where q％M is the formaldehyde removal rate in the experimental box0The mass m of formaldehyde in the experimental box before the adsorption testtThe mass of formaldehyde in the experimental box after the adsorption test. The test results are shown in Table 1.
TABLE 1 influence of Chitosan and Water-solid-liquid ratio on Formaldehyde removal Performance of prepared vermiculite-based Formaldehyde adsorbent
As can be seen from table 1, when the ratio of chitosan to water-solid-liquid is less than 2:100(mg: mL) (as in table 1, the ratio of chitosan to water-solid-liquid is 1.8:100, 1.5:100, 1:100 and lower ratios not listed in table 1), the amount of chitosan is less, so that the vermiculite flaking effect is deteriorated, the carbon chain molecules generated on the surface of vermiculite are reduced, and the formaldehyde removal rate is significantly reduced as the ratio of chitosan to water-solid-liquid is reduced. When the ratio of chitosan to water-solid-liquid is 2-8: 100(mg: mL) (as shown in Table 1, the ratio of chitosan to water-solid-liquid is 2:100, 5:100 and 8:100), the hydroxyl radicals and the oxygen radicals can accelerate the dissolution of vermiculite interlayer ions through oxidation, expand vermiculite interlayer spacing and promote the intercalation of chitosan molecules, so that vermiculite stripping is realized, meanwhile, the hydroxyl radicals and the oxygen radicals can break partial carbon chains of chitosan molecules to generate carbon chain molecules, and the carbon chain molecules are loaded on the surface of the vermiculite stripping in a plasma grafting manner. Finally, the formaldehyde removal rate of the prepared vermiculite-based formaldehyde adsorbent is more than 91%. When the ratio of chitosan to water-solid-liquid is greater than 8:100(mg: mL) (as in table 1, the ratio of chitosan to water-solid-liquid is 8.5:100, 9:100, 10:100 and higher ratios not listed in table 1), the amount of chitosan is excessive, the carbon chain molecules loaded on the surface of vermiculite are excessive, the carbon chain amination effect is poor, and the formaldehyde removal rate is significantly reduced as the ratio of chitosan to water-solid-liquid is further increased. In general, the benefit and the cost are combined, and when the ratio of chitosan to water-solid-liquid is equal to 2-8: 100(mg: mL), the formaldehyde removal performance of the prepared vermiculite-based formaldehyde adsorbent is improved.
Example 2
Influence of solid-liquid ratio of vermiculite powder to acidified chitosan solution on formaldehyde removal performance of prepared vermiculite-based formaldehyde adsorbent
Preparing a vermiculite-based formaldehyde adsorbent: dissolving chitosan into water according to a solid-to-liquid ratio of chitosan to water of 5:100(mg: mL) to obtain a chitosan solution, and dripping hydrochloric acid into the chitosan solution to obtain an acidified chitosan solution, wherein the concentration of the hydrochloric acid in the solution is 2 mol/L; grinding vermiculite, sieving with a 300-mesh sieve to obtain vermiculite powder, mixing the vermiculite powder and the acidified chitosan solution according to the solid-to-liquid ratio of the vermiculite powder to the acidified chitosan solution of 1.5:1, 2:1, 2.5:1, 3:1, 6:1, 9:1, 9.5:1, 10:1 and 10.5:1(mg: mL), continuously stirring at 240rpm, and simultaneously performing low-temperature plasma irradiation on the mixed slurry for 1.5 hours to obtain carbon chain loaded vermiculite flake slurry, wherein the low-temperature plasma action voltage is 16.5kV, the action atmosphere is oxygen, drying the carbon chain loaded vermiculite flake slurry at 100 ℃, grinding, and sieving with a 300-mesh sieve to obtain vermiculite carbon chain loaded flake powder; and (3) irradiating the carbon chain loaded vermiculite flake powder for 1.5 hours by using low-temperature plasma to obtain the vermiculite-based formaldehyde adsorbent, wherein the action voltage of the low-temperature plasma is 16.5kV, the action atmosphere is a mixed gas of ammonia gas and argon gas, and the volume ratio of the ammonia gas to the argon gas is 10: 100.
The formaldehyde adsorption test, the detection of formaldehyde in the aqueous solution, the measurement of the formaldehyde mass in the experimental box, and the calculation of the formaldehyde removal rate were the same as those in example 1. The test results are shown in Table 2.
TABLE 2 influence of the solid-liquid ratio of vermiculite powder to acidified chitosan solution on the formaldehyde removing performance of the prepared vermiculite-based formaldehyde adsorbent
As can be seen from table 2, when the solid-to-liquid ratio of the vermiculite powder to the acidified chitosan solution is less than 3:1(mg: mL) (as shown in table 2, the solid-to-liquid ratio of the vermiculite powder to the acidified chitosan solution is 2.5:1, 2:1, 1.5:1, and lower ratios not listed in table 2), the vermiculite powder is less, the vermiculite flake is not sufficiently gelatinized, the carbon chain loading effect is poor, and the formaldehyde removal rate is significantly reduced as the solid-to-liquid ratio of the vermiculite powder to the acidified chitosan solution is reduced. When the solid-to-liquid ratio of the vermiculite powder to the acidified chitosan solution is 3-9: 1(mg: mL) (as shown in Table 2, the solid-to-liquid ratio of the vermiculite powder to the acidified chitosan solution is 3:1, 6:1 and 9:1), the hydroxyl radical and the oxygen radical can accelerate the dissolution of vermiculite interlayer ions through oxidation, expand vermiculite interlayer spacing and promote the intercalation of chitosan molecules, so as to realize vermiculite stripping, meanwhile, the hydroxyl radical and the oxygen radical can enable partial chitosan molecule carbon chains to be broken to generate carbon chain molecules, the carbon chain molecules are loaded on the surface of the vermiculite stripping through a plasma grafting mode, the hydroxyl radical and the hydrated electrons can induce the gelation of the vermiculite stripping loaded carbon chains under an acid catalysis environment, so as to strengthen the stability of the loaded carbon chains, and the amine radical and the nitrogen radical can further react with the loaded carbon chain molecules on the surface of the vermiculite stripping to generate organic amine, thereby realizing carbon chain amination. Finally, the formaldehyde removal rate of the prepared vermiculite-based formaldehyde adsorption material is greater than 94%. When the solid-to-liquid ratio of the vermiculite powder to the acidified chitosan solution is greater than 9:1(mg: mL) (as shown in table 2, the solid-to-liquid ratio of the vermiculite powder to the acidified chitosan solution is 9.5:1, 10:1, 10.5:1 and higher ratios not listed in table 2), the vermiculite powder is excessive, the vermiculite flaking and carbon chain loading effects are poor, and the formaldehyde removal rate is remarkably reduced as the solid-to-liquid ratio of the vermiculite powder to the acidified chitosan solution is further increased. In general, the benefit and the cost are combined, and when the solid-to-liquid ratio of the vermiculite powder to the acidified chitosan solution is 3-9: 1(mg: mL), the formaldehyde removal performance of the prepared vermiculite-based formaldehyde adsorbent is improved.
Example 3
Influence of volume ratio of ammonia gas to argon gas on formaldehyde removal performance of prepared vermiculite-based formaldehyde adsorbent
Preparing a vermiculite-based formaldehyde adsorbent: dissolving chitosan into water according to a solid-to-liquid ratio of chitosan to water of 8:100(mg: mL) to obtain a chitosan solution, and dripping hydrochloric acid into the chitosan solution to obtain an acidified chitosan solution, wherein the concentration of the hydrochloric acid in the solution is 3 mol/L; grinding vermiculite, sieving with a 400-mesh sieve to obtain vermiculite powder, mixing the vermiculite powder with an acidified chitosan solution according to a solid-to-liquid ratio of 9:1(mg: mL) of the vermiculite powder to the acidified chitosan solution, continuously stirring at 360rpm, and simultaneously irradiating the mixed slurry with low-temperature plasma for 2 hours to obtain carbon chain loaded vermiculite flake slurry, wherein the low-temperature plasma has an action voltage of 30kV and an action atmosphere of oxygen, drying and grinding the carbon chain loaded vermiculite flake slurry at 150 ℃, and sieving with a 400-mesh sieve to obtain carbon chain loaded vermiculite flake powder; and (3) irradiating the carbon chain loaded vermiculite flake powder for 2 hours at low temperature by using plasma to obtain the vermiculite-based formaldehyde adsorbing material, wherein the action voltage of the low-temperature plasma is 30kV, the action atmosphere is a mixed gas of ammonia gas and argon gas, and the product ratio of the ammonia gas to the argon gas is 2.5:100, 3.5:100, 4.5:100, 5:100, 10:100, 15:100, 15.5:100, 16.5:100 and 17.5:100 respectively.
The formaldehyde adsorption test, the detection of formaldehyde in the aqueous solution, the measurement of the formaldehyde mass in the experimental box, and the calculation of the formaldehyde removal rate were the same as those in example 1. The test results are shown in Table 3.
TABLE 3 influence of the volume ratio of ammonia and argon on the formaldehyde removal performance of the prepared vermiculite-based formaldehyde adsorbent
| Volume ratio of ammonia to argon | q％ | Relative error |
| 2.5:100 | 76.94％ | ±0.1％ |
| 3.5:100 | 84.65％ | ±0.1％ |
| 4.5:100 | 91.31％ | ±0.1％ |
| 5:100 | 97.46％ | ±0.1％ |
| 10:100 | 98.12％ | ±0.1％ |
| 15:100 | 98.89％ | ±0.1％ |
| 15.5:100 | 93.24％ | ±0.2％ |
| 16.5:100 | 87.53％ | ±0.1％ |
| 17.5:100 | 81.62％ | ±0.1％ |
As can be seen from table 3, when the volume ratio of ammonia gas to argon gas is less than 5:100 (as shown in table 3, the volume ratio of ammonia gas to argon gas is 4.5:100, 3.5:100, 2.5:100 and lower ratios not listed in table 3), less ammonia gas is generated, so that the dissociation of ammonia gas generates less hydrogen radicals, amine radicals and nitrogen radicals, and the amination of the carbon chain is insufficient, resulting in a significant decrease in the formaldehyde removal rate as the volume ratio of ammonia gas to argon gas decreases. When the volume ratio of ammonia gas to argon gas is 5-15: 100 (as shown in table 3, the volume ratio of ammonia gas to argon gas is 5:100, 10:100 and 15:100), appropriate amount of ammonia gas is adopted, carbon chain amination is sufficient, and an amine free radical and a nitrogen free radical can further react with a carbon chain molecule loaded on the surface of the exfoliated vermiculite to generate organic amine. Finally, the formaldehyde removal rate of the prepared vermiculite-based formaldehyde adsorption material is greater than 97%. When the volume ratio of ammonia gas to argon gas is greater than 15:100 (as shown in table 3, the volume ratio of ammonia gas to argon gas is 15.5:100, 16.5:100, 17.5:100 and higher ratios not listed in table 3), ammonia gas is excessive, hydrogen radicals, amine radicals and nitrogen radicals generated by ammonia gas dissociation are excessive, the carbon chain loading effect is poor, and the formaldehyde removal rate is remarkably reduced as the volume ratio of ammonia gas to argon gas is further increased. In general, the benefit and the cost are combined, and when the volume ratio of ammonia gas to argon gas is 5-15: 100, the formaldehyde removal performance of the prepared vermiculite-based formaldehyde adsorbent is improved.
Claims (9)
1. A preparation method of a vermiculite-based formaldehyde adsorbent is characterized by comprising the following steps:
(1) dissolving chitosan in water, and adding hydrochloric acid to obtain an acidified chitosan solution;
(2) mixing vermiculite powder and an acidified chitosan solution, stirring and irradiating low-temperature plasma to obtain carbon chain loaded vermiculite flake slurry, drying, grinding and sieving to obtain carbon chain loaded vermiculite flake powder;
(3) and (3) irradiating the carbon chain loaded vermiculite flake powder by low-temperature plasma to obtain the vermiculite-based formaldehyde adsorbent.
2. The preparation method of the vermiculite-based formaldehyde adsorbent according to claim 1, wherein the solid-to-liquid ratio of chitosan to water in the step (1) is 2-8: 100.
3. The preparation method of the vermiculite-based formaldehyde adsorbent according to claim 1, wherein the solid-to-liquid ratio of the vermiculite powder to the acidified chitosan solution in the step (2) is 3-9.5: 1.
4. The preparation method of the vermiculite-based formaldehyde adsorbent according to claim 3, wherein the solid-to-liquid ratio of the vermiculite powder to the acidified chitosan solution in the step (2) is 3-9: 1.
5. The preparation method of the vermiculite-based formaldehyde adsorbent according to claim 1, wherein the action atmosphere of the low-temperature plasma irradiation in the step (3) is a mixed gas of ammonia gas and argon gas, and the volume ratio of the ammonia gas to the argon gas is 4.5-15.5: 100.
6. The preparation method of the vermiculite-based formaldehyde adsorbent according to claim 5, wherein the volume ratio of the ammonia gas to the argon gas is 5-15: 100.
7. The method for preparing the vermiculite-based formaldehyde adsorbent according to claim 1, wherein the concentration of hydrochloric acid in the step (1) is 1-3 mol/L.
8. The preparation method of the vermiculite-based formaldehyde adsorbent according to claim 1, wherein the time of low-temperature plasma irradiation in the step (2) and the step (3) is 1-2 h, the action voltage is 3-30 kV, and the action atmosphere in the step (2) is oxygen.
9. The preparation method of the vermiculite-based formaldehyde adsorbent according to claim 1, wherein the drying temperature of the carbon chain-loaded vermiculite flake slurry in the step (2) is 50-150 ℃, and the slurry is sieved with a 200-400 mesh sieve after being ground.
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