CN111039289A - Preparation method of alkali-activated porous carbon and application of alkali-activated porous carbon in adsorption of toluene in liquid paraffin - Google Patents
Preparation method of alkali-activated porous carbon and application of alkali-activated porous carbon in adsorption of toluene in liquid paraffin Download PDFInfo
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
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Abstract
The invention belongs to the technical field of synthesis of inorganic functional materials, and particularly relates to a preparation method of alkali activated porous carbon and application of the alkali activated porous carbon in adsorption of toluene in liquid paraffin. According to the invention, biomass sodium lignosulfonate is used as a carbon source, a mixed hard template sodium chloride is pre-carbonized, an activating agent sodium hydroxide is added, a sodium lignosulfonate-based alkali activated porous carbon adsorbent is obtained after carbonization, and a series of porous carbon materials are obtained by controlling different alkali-carbon ratios. The synthesis method provided by the invention is simple, low in cost, strong in controllability and mild in condition, and researches show that the prepared alkali-activated porous carbon has a good application prospect in adsorbing toluene in liquid paraffin.
Description
Technical Field
The invention belongs to the technical field of synthesis of inorganic functional materials, and particularly relates to a preparation method of alkali activated porous carbon and application of the alkali activated porous carbon in adsorption of toluene in liquid paraffin.
Background
Liquid wax is an important basic raw material for petroleum products, chemical industry, also called paraffin oil, is colorless, odorless, tasteless and non-fluorescent oily liquid, and is obtained by reduced pressure distillation of heavy oil. In recent years, low aromatic content has been the direction of high quality liquid wax. On one hand, when liquid wax is used as a reaction intermediate, the existence of aromatic hydrocarbon increases reaction byproducts, and influences reaction selectivity; on the other hand, the by-products have a severe effect on the color of downstream products, thereby affecting product quality. However, the liquid wax prepared in the prior art contains high concentration of aromatic compounds (30% -50%) which limits the application thereof, so that the research on a method for removing aromatic hydrocarbons from liquid paraffin, which is efficient, economical, good in circulation and environment-friendly, is urgent.
The prior dearomatization methods comprise a sulfonation method, an extraction method, a hydrogenation catalysis method and an adsorption method, but the defects of large three-waste discharge, low efficiency, high equipment cost, complex and dangerous operation process and the like of the former methods limit the wide application of the methods. Porous carbon adsorption is applied to selective separation of gas phase and liquid phase with high efficiency in recent years, and common adsorption materials include molecular sieves, silica gel, alumina, MOF materials, porous carbon materials and the like. The porous carbon has good mechanical and chemical stability, is easy to prepare, low in cost, small in pollution, large in specific surface area, rich in pores, controllable in pore size, strong in adsorption capacity and easy to modify, and becomes the first choice of industrial adsorption.
Sodium lignosulfonates are a by-product of the pulp and paper industry, currently producing over 100 million tons of lignin product per year for commercial use, but are relatively low value applications such as concrete additives, dye dispersants, adhesives, even when handled as low cost fuels, and lignin has the potential to become an important component of value added products. The method takes sodium lignosulfonate as a carbon source and sodium hydroxide as an activating agent, obtains a series of adsorbents with excellent performance by controlling the alkali-carbon ratio, takes toluene which is a typical aromatic hydrocarbon as a representative, is used for removing the toluene in the liquid paraffin, develops researches on an activation mechanism and an adsorption mechanism, and can provide a basis for industrial application.
Disclosure of Invention
The invention aims to provide a preparation method of alkali activated porous carbon and application of the alkali activated porous carbon in adsorption of aromatic hydrocarbon in liquid paraffin, so as to solve the problems of complex and dangerous operation, high cost and great environmental pollution of the aromatic hydrocarbon in the current liquid paraffin.
The invention adopts the following technical scheme for solving the problems:
a preparation method of alkali activated porous carbon comprises the following specific steps:
(1) weighing sodium lignosulfonate and a hard template, adding a small amount of water into the sodium lignosulfonate and the hard template, stirring until the sodium lignosulfonate and the hard template are completely dissolved to obtain a mixed solution, drying the mixed solution at the temperature of 100-200 ℃ (preferably drying at the temperature of 160 ℃), carbonizing the mixed solution for 2-3h at the temperature of 600 ℃ under the protection of nitrogen, naturally cooling the carbonized solution (preferably carbonizing the mixed solution for 2h at the temperature of 500 ℃), fully dissolving the hard template and soluble substances with water, filtering and drying to obtain a pre-carbonized product;
(2) mixing and grinding sodium hydroxide and the pre-carbonized product prepared in the step (1) uniformly, carbonizing the mixture for 2 to 3 hours at the temperature of 700-;
the mass ratio of the sodium hydroxide to the pre-carbonized product prepared in the step (1) is (0-4): 1, preferably (1-3): 1, most preferably 1: 1.
further, the hard template is sodium chloride, and the mass ratio of the sodium chloride to the sodium lignosulfonate is (2-5): 1, preferably 4: 1.
further, the carbonization in the step (1)The process is as follows: in N2Raising the temperature to 400-600 ℃ at the temperature raising rate of 5 ℃/min under protection, and preserving the temperature for 2-3h at the temperature of 400-600 ℃.
Further, the carbonization process in the step (2) is as follows: in N2Raising the temperature to 700 ℃ and 1000 ℃ at the temperature raising rate of 5 ℃/min under protection, and preserving the temperature for 2-3h at the temperature of 700 ℃ and 1000 ℃.
Further, the acid solution in the step (2) is dilute hydrochloric acid with the concentration of 4 wt% to 7 wt%, and preferably dilute hydrochloric acid with the concentration of 5 wt%.
The invention also provides application of the alkali activated porous carbon prepared by the preparation method in adsorbing toluene in liquid paraffin.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the synthesis method provided by the invention is simple, low in cost, strong in controllability, mild in condition, stable in toluene adsorption rate, far superior to that of a commercial adsorbent in adsorption effect, and easy to regenerate and use under the elution of isooctane, so that the adsorbent has excellent structural stability and economic performance, and accords with a green chemical concept.
Drawings
FIG. 1 is a scanning electron micrograph of a pre-carbonized product prepared in example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of SPCN-1 prepared in example 2 of the present invention;
FIG. 3 is a scanning electron micrograph of SPCN-4 prepared in example 2 of the present invention;
FIG. 4 is an XRD pattern of each porous carbon material prepared in example 2 of the present invention;
fig. 5 is a raman spectrum of each porous carbon material prepared in example 2 of the present invention;
FIG. 6 is an infrared spectrum of each porous carbon material prepared in example 2 of the present invention;
FIG. 7 is a graph showing toluene adsorption by each porous carbon material in example 3 of the present invention;
FIG. 8 is a nitrogen adsorption-desorption isothermal curve for each porous carbon material in example 3 of the present invention;
FIG. 9 is a graph showing the change in the amount of toluene adsorbed in the adsorption-desorption cycle experiment of the porous carbon material SPCN-1 in example 4 of the present invention;
FIG. 10 is a graph comparing the adsorption amounts of the porous carbon material SPCN-1 of the present invention to toluene adsorbed by commercial column chromatography silica gel, 10X molecular sieve and granular activated carbon in example 4.
Detailed Description
In order to make the objects, features and characteristics of the present invention comprehensible, embodiments accompanied with the present invention are further described below.
Example 1: the preparation of the pre-carbonized product comprises the following steps:
weighing a certain amount of Sodium Lignosulfonate (SLS), adding sodium chloride as a hard template according to the weight ratio of SLS to NaCl (1: 4), adding a small amount of deionized water, stirring until the sodium chloride is completely dissolved to obtain a mixed solution, drying the mixed solution in an electrothermal drying oven at 160 ℃, fully grinding to obtain solid mixed powder, putting the solid mixed powder into a tubular furnace, and putting the solid mixed powder into an N-shaped tube furnace2Raising the temperature to 500 ℃ at a heating rate of 5 ℃/min under protection, preserving the heat at 500 ℃ for 120min, naturally cooling, fully dissolving the hard template and the soluble substances with a large amount of deionized water, filtering, and drying at 150 ℃ to obtain a pre-carbonized product, wherein a scanning electron microscope image of the pre-carbonized product is shown in figure 1.
Example 2: the preparation method of the alkali activated porous carbon comprises the following steps:
sodium hydroxide and the pre-carbonized product prepared in example 1 were mixed and ground to uniformity in the alkali-carbon ratio of x:1, and then placed in a tube furnace under N2Raising the temperature to 850 ℃ at a heating rate of 5 ℃/min under protection, then preserving the temperature at 850 ℃ for 120min, cooling to room temperature, adding dilute hydrochloric acid with the mass percentage concentration of 5% into the mixture until no bubbles are generated and the pH value of the system is measured to be acidic, then magnetically stirring for 12h, filtering, repeatedly washing the mixture with deionized water until the mixture is neutral (the pH value of the washing solution is 7), drying the mixture in an electrothermal drying box at 110 ℃ to obtain a porous carbon product SPCN-x, and storing the porous carbon product SPCN-x in the electrothermal drying box at 120 ℃ for later use.
Porous carbon products SPCN-0, SPCN-1, SPCN-2, SPCN-3 and SPCN-4 with different alkali-carbon ratios are prepared by respectively selecting x as 0, 1, 2, 3 and 4.
FIGS. 2 and 3 are scanning electron micrographs of SPCN-1 and SPCN-4, respectively; as can be seen from the comparison between fig. 2 and fig. 3, the surface of the material is rich and varied in pore structure, and when the alkali-carbon ratio is further increased to 4:1, the pore diameter of the carbon material becomes finer and denser, and the pore volume is greatly reduced, because the excessive sodium hydroxide promotes the gasification reaction, so that the accessible area of alkali is reduced, and the activation stays on the surface.
Fig. 4 is an XRD spectrum of each porous carbon material, and fig. 5 is a raman spectrum of each porous carbon material. Fig. 4 shows the crystal structure of the material, in which the (002) crystal plane corresponds to the honeycomb hybridized carbon atom, while the (100) crystal plane shows the presence of short-range and parallel stacked graphite crystallites, and the broader low intensity peak shows that the sample has a lower graphitization degree and is an amorphous carbon structure.
Fig. 5 shows that the degree of graphitization of the material is low, and the result is consistent with the result of a scanning electron microscope, the crystal structure of the carbon material is not changed by different alkali-carbon ratios, and the chemical activation of the carbon material generates more graphene fragments and defect sites, so that the adsorption can be promoted.
FIG. 6 is an infrared spectrum of each porous carbon material, and it can be seen from FIG. 6 that the carbonization and activation process makes the surface of the adsorbent still have active chemical properties, and abundant chemical groups are favorable for adsorption.
Example 3: the experiment for adsorbing toluene by using the alkali-activated porous carbon prepared in example 2 as an adsorbent comprises the following steps:
weighing 0.02g of adsorbent, putting the adsorbent into a triangular flask with a plug containing 50mL of liquid paraffin containing 5g/L of toluene, then placing the triangular flask in a constant-temperature water bath oscillator at 45 ℃ and oscillating for more than 12h at the frequency of 130r/min until the adsorption balance is reached, sampling and centrifuging to obtain a supernatant, transferring 50 mu L of the supernatant into a 25mL volumetric flask by using a liquid transfer gun, diluting the supernatant with anhydrous isooctane to a constant volume, measuring the absorbance after adsorption at 206nm by using an ultraviolet visible spectrophotometer, measuring three times for each group, averaging, and detecting the adsorption capacity of the alkali activated porous carbon prepared under different alkali carbon ratios in example 2 as the adsorbent, wherein the adsorption capacity of the alkali activated porous carbon is 1684.74mg g g.g.the adsorption capacity of SPCN-0, SPCN-1, SPCN-2, SPCN-3 and SPCN-4 is respectively shown in figure 7-1、2875.17mg·g-1、2465.53mg·g-1、2427.71mg·g-1、1729.64mg·g-1。
Relationship between standard solution (C) and absorbance (a): preparing a series of liquid paraffin standard solutions containing toluene (the concentration of toluene in the standard solutions is respectively 0.5g/L, 1g/L, 2g/L, 3g/L, 4g/L, 5g/L and 6g/L), respectively measuring the absorbances of the standard solutions at 206nm, obtaining a formula (1) by knowing that the absorbance (A) and the solution concentration (C) are in a direct proportion relation according to Lambert-Beer law, and calculating the adsorption capacity by using the formula (2).
A＝0.1494*C-8.6×10-4(1)
In the formula, A (a.u.) is absorbance, C (g/L) is concentration of toluene in the solution, and the linear correlation coefficient R of the formula (1)2＝0.9996，Qe(mg/g) is the amount of toluene adsorbed by the adsorbent when the adsorption reached equilibrium, C0(g/L) is the initial concentration of toluene in the solution, Ce(g/L) is the adsorption equilibrium concentration of the solution, V (mL) represents the volume of the solution to be tested, and m (mg) is the mass of the adsorbent.
The nitrogen adsorption-desorption isotherms using SPCN-0, SPCN-1, SPCN-2, SPCN-3 and SPCN-4 prepared in example 2 as adsorbents, respectively, are shown in FIG. 8. from FIG. 8, it can be seen that all the samples conform to the typical type IV isotherm, have a hysteresis loop of type H4, and exhibit a micro-mesoporous property2Adsorption profile in the low pressure region (P/P)0Less than 0.05) and a rapid adsorption phenomenon occurs.
Example 4: reproducibility test
Taking SPCN-1 as an example, a static cycle experiment was carried out under the same adsorption conditions as in example 3 until an adsorption equilibrium was reached, which was a first adsorption, followed by desorption with anhydrous isooctane as a desorbent and then adsorption reaction again, the adsorption was repeated 5 times, and the change in the amount of adsorbed toluene per adsorption was calculated and compared, and the results are shown in FIG. 9, in which FIG. 9 shows that the adsorption capacities of the first to 5 th adsorbings were 3108.94 mg. cndot.g-1、2976.57mg·g-1、2932.31mg·g-1、2888.24mg·g-1、2875.72mg·g-1After repeated adsorption for 5 times, the adsorption performance of the adsorbent can still be kept above 92.5%, and the adsorption rate is kept stable.
Several commercial adsorbents commonly used in the market continue to be selected: the results of the regeneration experiments performed under the same experimental conditions as described above on the commercial column chromatography silica gel, the 10X molecular sieve and the granular activated carbon are shown in FIG. 10, and as can be seen from FIG. 10, the adsorption capacities of the 10X molecular sieve, the commercial column chromatography silica gel, the granular activated carbon and the SPCN-1 are shown from left to right, respectively, and after 5 times of adsorption, the adsorption capacities are 1548.15mg g-1、1718.16mg·g-1、2287.61mg·g-1、3018.53mg·g-1The adsorption effect of the SPCN-1 is far greater than that of a common commercial adsorbent, and the porous carbon material SPCN series prepared in the example 2 has better industrialization potential and application prospect.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the claims of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (6)
1. A preparation method of alkali activated porous carbon comprises the following specific steps:
(1) weighing sodium lignosulfonate and a hard template, adding a small amount of water into the sodium lignosulfonate and the hard template, stirring until the sodium lignosulfonate and the hard template are completely dissolved to obtain a mixed solution, drying the mixed solution at the temperature of 100-200 ℃, carbonizing the mixed solution at the temperature of 400-600 ℃ under the protection of nitrogen for 2-3h, naturally cooling the carbonized solution, fully dissolving the hard template and soluble substances by using water, filtering and drying the carbonized solution to obtain a pre-carbonized product;
(2) mixing and grinding sodium hydroxide and the pre-carbonized product prepared in the step (1) uniformly, carbonizing the mixture for 2 to 3 hours at the temperature of 700-;
the mass ratio of the sodium hydroxide to the pre-carbonized product prepared in the step (1) is (0-4): 1.
2. the preparation method according to claim 1, wherein the hard template is sodium chloride, and the mass ratio of the sodium chloride to the sodium lignosulfonate is (2-5): 1.
3. the production method according to claim 1, wherein the carbonization process in step (1) is: in N2Raising the temperature to 400-600 ℃ at the temperature raising rate of 5 ℃/min under protection, and preserving the temperature for 2-3h at the temperature of 400-600 ℃.
4. The production method according to claim 1, wherein the carbonization process in the step (2) is: in N2Raising the temperature to 700 ℃ and 1000 ℃ at the temperature raising rate of 5 ℃/min under protection, and preserving the temperature for 2-3h at the temperature of 700 ℃ and 1000 ℃.
5. The preparation method according to claim 1, wherein the acidic solution in the step (2) is diluted hydrochloric acid with a concentration of 4-7% by mass.
6. Use of the alkali-activated porous carbon obtained by the preparation method according to any one of claims 1 to 5 for adsorbing toluene in liquid paraffin.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112194126A (en) * | 2020-10-14 | 2021-01-08 | 中国华能集团清洁能源技术研究院有限公司 | Preparation method of lithium ion battery cathode porous carbon material |
| CN113149005A (en) * | 2021-04-29 | 2021-07-23 | 长安大学 | Biomass porous carbon material with high specific surface area, and preparation method and application thereof |
| CN114870801A (en) * | 2022-05-10 | 2022-08-09 | 南方科技大学 | Preparation method and application of modified charcoal adsorbent |
| CN115282924A (en) * | 2022-06-30 | 2022-11-04 | 南京林业大学 | Method for adsorbing cationic dye in wastewater |
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| EP2707327A1 (en) * | 2011-05-11 | 2014-03-19 | FPInnovations Inc. | Chiral or achiral, mesoporous carbon |
| CN105664848A (en) * | 2016-01-14 | 2016-06-15 | 江苏大学 | Preparation method of lignin hierarchical porous carbon material with endellite as template |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP2707327A1 (en) * | 2011-05-11 | 2014-03-19 | FPInnovations Inc. | Chiral or achiral, mesoporous carbon |
| CN105664848A (en) * | 2016-01-14 | 2016-06-15 | 江苏大学 | Preparation method of lignin hierarchical porous carbon material with endellite as template |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112194126A (en) * | 2020-10-14 | 2021-01-08 | 中国华能集团清洁能源技术研究院有限公司 | Preparation method of lithium ion battery cathode porous carbon material |
| CN113149005A (en) * | 2021-04-29 | 2021-07-23 | 长安大学 | Biomass porous carbon material with high specific surface area, and preparation method and application thereof |
| CN114870801A (en) * | 2022-05-10 | 2022-08-09 | 南方科技大学 | Preparation method and application of modified charcoal adsorbent |
| CN115282924A (en) * | 2022-06-30 | 2022-11-04 | 南京林业大学 | Method for adsorbing cationic dye in wastewater |
| CN115282924B (en) * | 2022-06-30 | 2024-02-09 | 南京林业大学 | Adsorption method of cationic dye in wastewater |
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