Dandelion adsorbent as well as preparation method and application thereof
The dandelion adsorbent prepared by treating dandelion with α-amylase and potassium hydroxide solves the problems of poor nicotine adsorption effect and short duration, achieving efficient nicotine adsorption and economy.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- YUNCHENG UNIVERSITY
- Filing Date
- 2023-11-21
- Publication Date
- 2026-04-17
AI Technical Summary
Existing nicotine adsorbents have poor adsorption effects, and suffer from problems such as adsorption saturation, secondary pollution, and short adsorption duration.
Dandelion adsorbent was prepared by soaking dandelion in a water bath with α-amylase solution, followed by ultrasonic treatment with potassium hydroxide solution, washing, drying and pulverizing.
It improves the adsorption effect of nicotine, solves the problems of short adsorption duration and secondary pollution of adsorbents, and is relatively economical.
Smart Images

Figure CN121869302A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of harmful gas adsorbent technology, specifically to a dandelion adsorbent, its preparation method, and its application. Background Technology
[0002] Cigarettes are now ubiquitous in the market, and smoking addiction has become a serious problem. Cigarettes are extremely harmful to the human body. The main harmful substances in cigarette smoke are tar, nicotine, and carbon monoxide. Nicotine is a stimulant and numbing substance that keeps the nervous system in an excited state, causing vasospasm and high blood pressure. Smoking can damage multiple organs and lead to cancer, high blood pressure, chronic bronchitis, and other lung diseases.
[0003] Nicotine, also known as tobacco alkaloid, is a liquid, colorless or slightly yellow in color, and is volatile. Nicotine is highly toxic; it is a narcotic. Even small amounts can keep the central nervous system excited and raise blood pressure; large doses can suppress the central nervous system, paralyze the heart, and even lead to death—a process that takes only 5 to 30 minutes. Clinical observations show that just a few milligrams of pure nicotine can cause headaches and confusion, thus, heavy smokers can suffer from chronic poisoning. The harm of nicotine to the human body is not only manifested in addiction but also in "nicotine-induced optic neuropathy." Long-term smoking can cause vision loss, and in severe cases, optic nerve atrophy, ultimately leading to blindness. Therefore, reducing the harm of nicotine has become a critical technical problem urgently needing to be solved in this field.
[0004] Existing materials for removing nicotine include activated carbon and some indoor plants. Activated carbon can reduce and filter smoke toxins or nicotine; indoor plants include plants such as Milan, spider plants, ivy, snake plants, daffodils, and cacti. However, the above-mentioned adsorbents all have technical problems such as poor adsorption effect and short adsorption duration. Therefore, this invention provides a dandelion adsorbent, its preparation method, and its application. Summary of the Invention
[0005] This invention provides a dandelion adsorbent, its preparation method, and its application, effectively solving the technical problems of poor adsorption effect, adsorption saturation, secondary pollution, and short adsorption duration of existing nicotine adsorbents. At the same time, it provides a dandelion adsorbent with a significantly better adsorption capacity for nicotine than existing nicotine adsorbents and capable of cyclic adsorption and desorption.
[0006] The first objective of this invention is to provide a method for preparing a dandelion adsorbent, comprising the following steps:
[0007] S1. Wash the dandelion, boil it in boiling water for 20 minutes, rinse it with running water, add α-amylase solution, treat it in a water bath at 85-90℃ for 30 minutes, wash it, and obtain enzymatically hydrolyzed dandelion.
[0008] S2: Add potassium hydroxide solution to the enzymatically hydrolyzed dandelion from S1, sonicate at 65-70℃ for 30 minutes, wash, dry at constant temperature, and pulverize to obtain dandelion adsorbent.
[0009] In a preferred embodiment, in S1, the concentration of the α-amylase solution is 0.001–0.0026 mol / L.
[0010] In a preferred embodiment, in S1, the ratio of dandelion to α-amylase solution is 1g:80-100mL.
[0011] In a preferred embodiment, in S2, the concentration of the potassium hydroxide solution is 0.1–0.5 mol / L.
[0012] In a preferred embodiment, in S2, the ratio of the enzymatically hydrolyzed dandelion to potassium hydroxide solution is 1-2 g: 100 mL.
[0013] In a preferred embodiment, in S2, the ultrasonic power is 150W.
[0014] In a preferred embodiment, in S2, after pulverization, the dandelion adsorbent has a mesh size of 40.
[0015] The second objective of this invention is to provide a dandelion adsorbent prepared by the above-described preparation method.
[0016] A third objective of this invention is to provide the application of the above-mentioned dandelion adsorbent in the removal of nicotine.
[0017] In a preferred embodiment, the application specifically involves: removing the fibers from the cigarette filter, placing the dandelion adsorbent inside the cigarette filter, and then absorbing the smoke through the cigarette filter after lighting the cigarette.
[0018] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0019] This invention provides a dandelion adsorbent, its preparation method, and its application. The invention involves soaking dandelion in a water bath with an α-amylase solution to obtain enzymatically hydrolyzed dandelion. The hydrolyzed dandelion is then ultrasonically treated in a potassium hydroxide solution, washed, dried, and pulverized to obtain the dandelion adsorbent. Compared with raw dandelion, activated carbon, diatomaceous earth, and cellulose acetate, the dandelion adsorbent of this invention exhibits the best adsorption effect for nicotine. Furthermore, the dandelion adsorbent residue prepared by this invention is relatively the most economical. This invention effectively solves the technical problems of existing nicotine adsorbents, such as poor adsorption effect, secondary pollution, and short adsorption duration. Attached Figure Description
[0020] Figure 1 This is a curve of the nicotine standard solution of the present invention;
[0021] Figure 2 This is a graph showing the effect of sodium hydroxide solution concentration and high-temperature resistant α-amylase concentration on adsorption rate in this invention.
[0022] Figure 3 This is a graph showing the effect of high-temperature resistant α-amylase concentration and ultrasonic time on the adsorption rate in this invention.
[0023] Figure 4 This is a graph showing the relationship between nicotine concentration and adsorption amount in this invention;
[0024] Figure 5 This invention relates to the Langmuir model;
[0025] Figure 6 This is the Freundlich model of the present invention;
[0026] Figure 7 This is a graph showing the effect of dandelion adsorbent particle size on nicotine adsorption rate in this invention.
[0027] Figure 8 This is a graph showing the effect of the amount of dandelion adsorbent added on the adsorption of nicotine in this invention.
[0028] Figure 9 This is a graph showing the effect of adsorption temperature on nicotine adsorption in this invention.
[0029] Figure 10 This is a graph showing the relationship between adsorption temperature and adsorption amount in this invention;
[0030] Figure 11 The adsorption temperature and lnK of this invention D Relationship diagram;
[0031] Figure 12 This is a graph showing the relationship between adsorption time and adsorption amount in this invention;
[0032] Figure 13This is the quasi-first-order kinetic diagram of the present invention (t and lnq). e -q t );
[0033] Figure 14 The pseudo-second-order kinetic diagram of this invention (t and t / q) t );
[0034] Figure 15 This is a comparison chart of the adsorption rates of different materials in this invention;
[0035] Figure 16 The images show the XRD patterns of the dandelion adsorbent after nicotine adsorption, the original dandelion, and the dandelion adsorbent before nicotine adsorption according to the present invention; where A represents the dandelion adsorbent after adsorption, B represents the dandelion adsorbent before adsorption, and C represents the original dandelion.
[0036] Figure 17 The infrared spectra of the dandelion adsorbent after nicotine adsorption, the original dandelion, and the dandelion adsorbent before nicotine adsorption are shown in this invention. Detailed Implementation
[0037] To enable those skilled in the art to better understand and implement the technical solutions of this invention, the invention will be further described below with reference to specific embodiments and accompanying drawings. However, the embodiments described are not intended to limit the invention. Unless otherwise specified, the following test methods and detection methods are conventional methods; unless otherwise specified, the reagents and raw materials are commercially available.
[0038] Example 1
[0039] A method for preparing a dandelion adsorbent includes the following steps:
[0040] S1. Wash the dandelion, boil it in boiling water for 20 minutes, rinse it under running water, add 0.001mol / L α-amylase solution at a ratio of 1g dandelion to 100mL, treat it in a water bath at 87℃ for 30 minutes, wash it, and obtain enzymatically hydrolyzed dandelion.
[0041] S2: Add 0.2 mol / L potassium hydroxide solution to the enzymatically hydrolyzed dandelion in S1 according to the ratio of 1 g to 100 mL of potassium hydroxide solution. Sonicate at 68℃ and 150 W for 40 min, wash, dry at constant temperature, and pulverize through a 40-mesh sieve to obtain dandelion adsorbent.
[0042] Example 2
[0043] A method for preparing a dandelion adsorbent includes the following steps:
[0044] S1. Wash the dandelion, boil it in boiling water for 20 minutes, rinse it under running water, add 0.0026mol / L α-amylase solution at a ratio of 1g dandelion to 80mL, treat it in a water bath at 85℃ for 30 minutes, wash it, and obtain enzymatically hydrolyzed dandelion.
[0045] S2: Add 0.1 mol / L potassium hydroxide solution to the enzymatically hydrolyzed dandelion in S1 according to the ratio of 2 g to 100 mL of potassium hydroxide solution. Sonicate at 65°C and 150 W for 30 min, wash, dry at constant temperature, and pulverize through a 40-mesh sieve to obtain dandelion adsorbent.
[0046] Example 3
[0047] A method for preparing a dandelion adsorbent includes the following steps:
[0048] S1. Wash the dandelion, boil it in boiling water for 20 minutes, rinse it with running water, add 0.002mol / L α-amylase solution at a ratio of 1g dandelion to 90mL, treat it in a 90℃ water bath for 30 minutes, wash it, and obtain enzymatically hydrolyzed dandelion.
[0049] S2: Add 0.5 mol / L potassium hydroxide solution to the enzymatically hydrolyzed dandelion in S1 according to the ratio of 1.5 g to 100 mL of potassium hydroxide solution. Sonicate at 70 °C and 150 W for 30 min, wash, dry at constant temperature, and pulverize through a 40-mesh sieve to obtain dandelion adsorbent.
[0050] Example 4
[0051] A method for preparing a dandelion adsorbent includes the following steps:
[0052] S1. Wash the dandelion, boil it in boiling water for 20 minutes, rinse it under running water, add 0.0015mol / L α-amylase solution at a ratio of 1g dandelion to 100mL, treat it in a water bath at 87℃ for 30 minutes, wash it, and obtain enzymatically hydrolyzed dandelion.
[0053] S2: Add 0.3 mol / L potassium hydroxide solution to the enzymatically hydrolyzed dandelion in S1 according to the ratio of 1 g to 100 mL of potassium hydroxide solution. Sonicate at 68℃ and 150 W for 30 min, wash, dry at constant temperature, and pulverize through a 40-mesh sieve to obtain dandelion adsorbent.
[0054] Comparative Examples 1-4
[0055] The difference from Example 1 is that the 40-mesh sieve was changed to an 8-mesh sieve, an 18-mesh sieve, a 60-mesh sieve, and an 80-mesh sieve, respectively.
[0056] A method for preparing a dandelion adsorbent includes the following steps:
[0057] S1. Wash the dandelion, boil it in boiling water for 20 minutes, rinse it under running water, add 0.001mol / L α-amylase solution at a ratio of 1g dandelion to 100mL, treat it in a water bath at 87℃ for 30 minutes, wash it, and obtain enzymatically hydrolyzed dandelion.
[0058] S2: Add 0.2 mol / L potassium hydroxide solution to the enzymatically hydrolyzed dandelion in S1 according to the ratio of 1 g to 100 mL of potassium hydroxide solution. Sonicate at 68℃ and 150 W for 40 min, wash, dry at constant temperature, and pulverize through 8-mesh, 18-mesh, 60-mesh and 80-mesh sieves to obtain dandelion adsorbent.
[0059] The dandelion adsorbents prepared in Examples 1-4 and Comparative Examples 1-4 were applied to adsorb nicotine, and their adsorption effects were compared with those of activated carbon, diatomaceous earth, and cellulose acetate. Specific application examples are as follows:
[0060] Application Example 1
[0061] (1) Weigh 0.1g of the dandelion adsorbent prepared in Example 1 using a balance. After pulling out the cellulose acetate from the filter of the Hongqiqu brand cigarette, cut off 1cm and leave the remaining 1.5cm of cellulose acetate in the filter paper sleeve. Then stuff 0.1g of the dandelion adsorbent into the filter paper sleeve.
[0062] (2) Place the cigarette prepared in step (1) on the adsorption device in the laboratory and clamp it with a water stop clamp. Turn on the vacuum pump. When the vacuum pump pressure reaches 0.01 MPa, small bubbles will appear. Open the water stop clamp, light the cigarette, and conduct the adsorption experiment at 26°C. When the cigarette is completely burned, turn off the vacuum pump and the water stop clamp, and let the smoke completely dissolve in 150 mL of distilled water. Pour the solution into a 250 mL volumetric flask, let it stand for 20 min, take the supernatant, measure the absorbance repeatedly, and calculate the nicotine adsorption rate.
[0063] Application Example 2
[0064] (1) Weigh 0.1g of the dandelion adsorbent prepared in Example 2 using a balance. After pulling out the cellulose acetate from the filter tip of the Hongqiqu brand cigarette, cut off 1cm and leave the remaining 1.5cm of cellulose acetate in the filter paper sleeve. Then stuff 0.1g of the dandelion adsorbent into the filter paper sleeve.
[0065] (2) Place the cigarette prepared in step (1) on the adsorption device in the laboratory and clamp it with a water stop clamp. Turn on the vacuum pump. When the vacuum pump pressure reaches 0.01 MPa, small bubbles will appear. Open the water stop clamp, light the cigarette, and conduct the adsorption experiment at 26°C. When the cigarette is completely burned, turn off the vacuum pump and the water stop clamp, and let the smoke completely dissolve in 150 mL of distilled water. Pour the solution into a 250 mL volumetric flask, let it stand for 20 min, take the supernatant, measure the absorbance repeatedly, and calculate the nicotine adsorption rate.
[0066] Application Example 3
[0067] (1) Weigh 0.1g of the dandelion adsorbent prepared in Example 3 using a balance. After pulling out the cellulose acetate from the filter of the Hongqiqu brand cigarette, cut off 1cm and leave the remaining 1.5cm of cellulose acetate in the filter paper sleeve. Then stuff 0.1g of the dandelion adsorbent into the filter paper sleeve.
[0068] (2) Place the cigarette prepared in step (1) on the adsorption device in the laboratory and clamp it with a water stop clamp. Turn on the vacuum pump. When the vacuum pump pressure reaches 0.01 MPa, small bubbles will appear. Open the water stop clamp, light the cigarette, and conduct the adsorption experiment at 26°C. When the cigarette is completely burned, turn off the vacuum pump and the water stop clamp, and let the smoke completely dissolve in 150 mL of distilled water. Pour the solution into a 250 mL volumetric flask, let it stand for 20 min, take the supernatant, measure the absorbance repeatedly, and calculate the nicotine adsorption rate.
[0069] Application Example 4
[0070] (1) Weigh 0.1g of the dandelion adsorbent prepared in Example 4 using a balance. After pulling out the cellulose acetate from the filter of the Hongqiqu brand cigarette, cut off 1cm and leave the remaining 1.5cm of cellulose acetate in the filter paper sleeve. Then stuff 0.1g of the dandelion adsorbent into the filter paper sleeve.
[0071] (2) Place the cigarette prepared in step (1) on the adsorption device in the laboratory and clamp it with a water stop clamp. Turn on the vacuum pump. When the vacuum pump pressure reaches 0.01 MPa, small bubbles will appear. Open the water stop clamp, light the cigarette, and conduct the adsorption experiment at 26°C. When the cigarette is completely burned, turn off the vacuum pump and the water stop clamp, and let the smoke completely dissolve in 150 mL of distilled water. Pour the solution into a 250 mL volumetric flask, let it stand for 20 min, take the supernatant, measure the absorbance repeatedly, and calculate the nicotine adsorption rate.
[0072] Application Comparative Examples 1-4
[0073] The difference compared to Application Example 1 is that the adsorption experiment temperature was adjusted to 18℃, 20℃, 22℃, and 24℃.
[0074] (1) Weigh 0.1g of the dandelion adsorbent prepared in Example 1 using a balance. After pulling out the cellulose acetate from the filter of the Hongqiqu brand cigarette, cut off 1cm and leave the remaining 1.5cm of cellulose acetate in the filter paper sleeve. Then stuff 0.1g of the dandelion adsorbent into the filter paper sleeve.
[0075] (2) Place the cigarette prepared in step (1) on the adsorption device in the laboratory and clamp it with a water stop clamp. Turn on the vacuum pump. When the vacuum pump pressure reaches 0.01 MPa, small bubbles will appear. Open the water stop clamp, light the cigarette, and conduct adsorption experiments at 18℃, 20℃, 22℃, and 24℃. When the cigarette is completely burned, turn off the vacuum pump and the water stop clamp, and let the smoke completely dissolve in 150 mL of distilled water. Pour the solution into a 250 mL volumetric flask, let it stand for 20 min, take the supernatant, measure the absorbance repeatedly, and calculate the nicotine adsorption rate.
[0076] Application Comparative Examples 5-8
[0077] The difference compared to Application Example 1 is that the mass of the dandelion adsorbent was adjusted to 0.06g, 0.08g, 0.12g, and 0.14g.
[0078] (1) Weigh 0.06g, 0.08g, 0.12g and 0.14g of the dandelion adsorbent prepared in Example 1 using a balance. After pulling out the cellulose acetate from the filter tip of each of the four Hongqiqu brand cigarettes, cut off 1cm and leave the remaining 1.5cm of cellulose acetate in the filter paper sleeve. Then, stuff 0.06g, 0.08g, 0.12g and 0.14g of the dandelion adsorbent into the corresponding filter paper sleeve.
[0079] (2) Place the cigarette prepared in step (1) on the adsorption device in the laboratory and clamp it with a water stop clamp. Turn on the vacuum pump. When the vacuum pump pressure reaches 0.01 MPa, small bubbles will appear. Open the water stop clamp, light the cigarette, and conduct the adsorption experiment at 26°C. When the cigarette is completely burned, turn off the vacuum pump and the water stop clamp, and let the smoke completely dissolve in 150 mL of distilled water. Pour the solution into a 250 mL volumetric flask, let it stand for 20 min, take the supernatant, measure the absorbance repeatedly, and calculate the nicotine adsorption rate.
[0080] Application Comparative Examples 9-12
[0081] The difference compared to Application Example 1 is that the mesh size of the pulverized dandelion adsorbent is adjusted to 8 mesh, 18 mesh, 60 mesh, and 80 mesh.
[0082] (1) Weigh 0.1g of the dandelion adsorbent prepared in Comparative Examples 1 to 4 using a balance. Pull out the cellulose acetate from the filter tips of four Hongqiqu brand cigarettes, cut off 1cm, leaving the remaining 1.5cm of cellulose acetate in the filter paper sleeve, and stuff 0.1g of the dandelion adsorbent into the filter paper sleeve.
[0083] (2) Place the cigarette prepared in step (1) on the adsorption device in the laboratory and clamp it with a water stop clamp. Turn on the vacuum pump. When the vacuum pump pressure reaches 0.01 MPa, small bubbles will appear. Open the water stop clamp, light the cigarette, and conduct adsorption experiments at 18℃, 20℃, 22℃, and 24℃. When the cigarette is completely burned, turn off the vacuum pump and the water stop clamp, and let the smoke completely dissolve in 150 mL of distilled water. Pour the solution into a 250 mL volumetric flask, let it stand for 20 min, take the supernatant, measure the absorbance repeatedly, and calculate the nicotine adsorption rate.
[0084] Application Comparative Example 13
[0085] (1) Weigh 0.1g of diatomaceous earth using a balance, pull out the cellulose acetate from the filter tip of the Hongqiqu brand cigarette, cut off 1cm, leaving the remaining 1.5cm of cellulose acetate in the filter paper sleeve, and stuff 0.1g of the dandelion adsorbent into the filter paper sleeve.
[0086] (2) Place the cigarette prepared in step (1) on the adsorption device in the laboratory and clamp it with a water stop clamp. Turn on the vacuum pump. When the vacuum pump pressure reaches 0.01 MPa, small bubbles will appear. Open the water stop clamp, light the cigarette, and conduct the adsorption experiment at 26°C. When the cigarette is completely burned, turn off the vacuum pump and the water stop clamp, and let the smoke completely dissolve in 150 mL of distilled water. Pour the solution into a 250 mL volumetric flask, let it stand for 20 min, take the supernatant, measure the absorbance repeatedly, and calculate the nicotine adsorption rate.
[0087] Application Comparative Example 14
[0088] (1) Weigh 0.1g of activated carbon using a balance. After pulling out the cellulose acetate from the filter tip of the Hongqiqu brand cigarette, cut off 1cm and leave the remaining 1.5cm of cellulose acetate in the filter paper sleeve. Then, stuff 0.1g of the dandelion adsorbent into the filter paper sleeve.
[0089] (2) Place the cigarette prepared in step (1) on the adsorption device in the laboratory and clamp it with a water stop clamp. Turn on the vacuum pump. When the vacuum pump pressure reaches 0.01 MPa, small bubbles will appear. Open the water stop clamp, light the cigarette, and conduct the adsorption experiment at 26°C. When the cigarette is completely burned, turn off the vacuum pump and the water stop clamp, and let the smoke completely dissolve in 150 mL of distilled water. Pour the solution into a 250 mL volumetric flask, let it stand for 20 min, take the supernatant, measure the absorbance repeatedly, and calculate the nicotine adsorption rate.
[0090] Application Comparative Example 15
[0091] (1) Weigh 0.1g of cellulose acetate using a balance. After pulling out the cellulose acetate from the filter of a Hongqiqu brand cigarette, cut off 1cm and leave the remaining 1.5cm of cellulose acetate in the filter paper sleeve. Then, stuff 0.1g of the dandelion adsorbent into the filter paper sleeve.
[0092] (2) Place the cigarette prepared in step (1) on the adsorption device in the laboratory and clamp it with a water stop clamp. Turn on the vacuum pump. When the vacuum pump pressure reaches 0.01 MPa, small bubbles will appear. Open the water stop clamp, light the cigarette, and conduct the adsorption experiment at 26°C. When the cigarette is completely burned, turn off the vacuum pump and the water stop clamp, and let the smoke completely dissolve in 150 mL of distilled water. Pour the solution into a 250 mL volumetric flask, let it stand for 20 min, take the supernatant, measure the absorbance repeatedly, and calculate the nicotine adsorption rate.
[0093] Application Comparative Example 16
[0094] (1) Weigh 0.1g of raw dandelion with a balance, crush it to 40 mesh, pull out the cellulose acetate from the filter of the Hongqiqu brand cigarette, cut off 1cm, leaving the remaining 1.5cm of cellulose acetate in the filter paper sleeve, and stuff 0.1g of the dandelion adsorbent into the filter paper sleeve;
[0095] (2) Place the cigarette prepared in step (1) on the adsorption device in the laboratory and clamp it with a water stop clamp. Turn on the vacuum pump. When the vacuum pump pressure reaches 0.01 MPa, small bubbles will appear. Open the water stop clamp, light the cigarette, and conduct the adsorption experiment at 26°C. When the cigarette is completely burned, turn off the vacuum pump and the water stop clamp, and let the smoke completely dissolve in 150 mL of distilled water. Pour the solution into a 250 mL volumetric flask, let it stand for 20 min, take the supernatant, measure the absorbance repeatedly, and calculate the nicotine adsorption rate.
[0096] The specific experimental process of this invention is as follows:
[0097] 1. Experimental materials
[0098] The dandelions used in this experiment were collected from rural land in Wanrong County, Yuncheng City.
[0099] 2. Experimental reagents and chemicals
[0100] Distilled water (laboratory preparation), sodium hydroxide (analytical grade), potassium hydroxide (analytical grade), hydrochloric acid (analytical grade), potassium permanganate (analytical grade), heat-resistant α-amylase, anhydrous calcium chloride (analytical grade), glacial acetic acid (analytical grade), activated carbon (granules) (analytical grade), diatomaceous earth (analytical grade), bamboo charcoal (granules), cellulose acetate.
[0101] 3. Plot the nicotine standard solution curve.
[0102] (1) Take 120ug, 190ug, 260ug, 330ug, 400ug and 470ug respectively from the pure nicotine solution with a pipette, add them to 150mL of distilled water respectively, add 5g of sodium hydroxide respectively, and after they are fully dissolved, add 0.02765g of potassium permanganate respectively, and then make up to 250mL respectively.
[0103] (2) Pour the six prepared solutions into six test tubes, label them, and incubate them in a water bath at 100℃ for 8 minutes. After cooling to room temperature, take the supernatant and filter it. Repeatedly measure its absorbance using a spectrophotometer to plot the nicotine curve, such as... Figure 1 As shown.
[0104] Depend on Figure 1 It can be concluded that the linear correlation between nicotine concentration and absorbance is significant in the plotted curve, indicating that the nicotine curve exhibits good linearity within the specified concentration range. The regression equation is y = 0.8225x - 0.1061, with a correlation coefficient R0. 2 It is 0.9996.
[0105] 5. Determination and calculation of the adsorption rate of nicotine by dandelion adsorbent
[0106] (1) Weigh a certain amount (0.1g) of dandelion adsorbent using a balance and put it into the filter paper sleeve that has been pulled out of the cellulose acetate (the tobacco used is Hongqiqu). Leave 1.5cm of cellulose acetate and then stuff it into the paper sleeve.
[0107] (2) Place the cigarette prepared by the above steps on the adsorption device, clamp it with a water stop clamp, turn on the vacuum pump, and wait until the vacuum pump pressure reaches 0.01MPa (at which point small bubbles will appear). Then open the water stop clamp, light the cigarette, and turn off the vacuum pump and water stop clamp when the cigarette has burned out. Let the smoke completely dissolve in 150mL of distilled water, pour it into a 250mL volumetric flask, and let it stand for 20 minutes.
[0108] (3) After 20 minutes, add 5g of sodium hydroxide and 0.02765g of potassium permanganate, and finally bring the volume to the 250mL mark to achieve a sodium hydroxide concentration of 0.5mol / L and a potassium permanganate concentration equilibrium of 7×10⁻⁶. -4 mol / L;
[0109] (4) Heat the liquid in a water bath at 100℃ for 7.5 min, cool it to room temperature, and then filter the upper layer of liquid. Collect the filtrate.
[0110] (5) Measure its absorbance at 612 nm using a spectrophotometer and obtain the nicotine concentration according to the nicotine standard curve.
[0111] (6) The formula for calculating the nicotine adsorption rate of dandelion is:
[0112] Adsorption rate = (M1 - M1') / M1
[0113] Where: M1 is the total amount of nicotine in the solution of the filtration device (1.5 + blank); M1' is the content of nicotine in the solution of the filtration device each time the experiment is conducted.
[0114] The nicotine content of various cigarette brands is shown in Table 1.
[0115] Table 1. Cigarette Brands by Brand
[0116]
[0117] 6. Quadratic orthogonal regression combination experimental design
[0118] (1) Using three factors, namely KOH solution concentration X1, α-amylase solution concentration X2, and ultrasonic time X3, the conditions of these three factors were set to zero level, and a three-factor five-level coding table was compiled as shown in Table 2. The nicotine adsorption rate was used as the evaluation index to conduct an experiment on nicotine adsorption.
[0119] Table 2 Three-Factor Five-Level Coding Table
[0120]
[0121] Based on Table 1, the experimental design table of three-factor, five-level quadratic orthogonal regression rotation combination can be obtained by using DPS software for data analysis and processing, as shown in Table 3.
[0122] Table 3. Quadratic Orthogonal Regression Combination Design Table
[0123]
[0124]
[0125] The analysis of variance was obtained from the adsorption rate results in Table 3 above, as shown in Table 4.
[0126] Table 4. Analysis of Variance Table
[0127]
[0128] (2) Model building and testing
[0129] The results were processed using DPS data processing software, resulting in a mathematical model of the regression equation between the three factors (X1, X2, X3) and the adsorption rate Y:
[0130] Y = 31.59918 + 0.98099X1 - 1.55738X2 - 0.00368X3 + 0.15356X 12 + 1.31675X 22 + 0.9225
[0131] 4X 32 + 1.59250X1X2 - 1.11000X1X3 - 1.83250X2X3
[0132] Under the condition that the significance level is 0.01, in this model, F lack of fit = 5.21680 < F0.01(5,8) = 6.63. This result indicates that the experimental error is very small and can be ignored, and some unknown factors have been taken into account in the experimental design; F regression = 4.27012 > F0.01(9,13) = 4.19, indicating that the regression equation has reached a very significant level, the reliability of the experimental speculation is extremely high, the prediction is accurate, and the model is established.
[0133] Conduct a significance test on the regression equation. After removing the insignificant terms at the significance level of α = 0.10, the simplified regression equation is obtained: <
[0140]
[0141]
[0142] From Table 5 and Figure 2 It can be seen that the highest point is (-1.682, -1.6818), that is, when the potassium hydroxide concentration is 0.2 mol / L and the thermostable α-amylase concentration is 0.001 mol / L, the adsorption rate is the highest, which is 40.80%.
[0143] The effects of heat-resistant α-amylase concentration (mol / L) and ultrasonic time (min) on adsorption rate are shown in Table 6 and Figure 3 .
[0144] Table 6. Effects of high-temperature resistant α-amylase concentration and ultrasonic time on adsorption rate.
[0145]
[0146] From Table 6 and Figure 3 Analysis shows that the highest point is (-1.682, 1.6818), which means that when the concentration of heat-resistant α-amylase is 0.001 mol / L and the ultrasonic time is 40 min, the highest adsorption rate is 45.74%.
[0147] After processing with DPS software, it can be seen that when the Y value is Max, the levels of the three factors X1, X2, and X3 are (-1.682, -1.682, 1.682), which corresponds to a potassium hydroxide concentration of 0.2 mol / L, a heat-resistant α-amylase concentration of 0.001 mol / L, an ultrasonic time of 40 min, and a Ymax of 48.48%. The actual measured value is 47.93%, and the actual value / predicted value = 0.9887, which is close to 1, indicating that the model is reliable.
[0148] 7. Adsorption isotherm
[0149] This experiment used two adsorption isotherm models, the Langmuir model and the Freundlich model, for fitting.
[0150] The adsorption isotherm equation for the Langmuir model is: C e / Q e =C e / Q m +1 / (Q m b);
[0151] The adsorption isotherm equation of the Freundlich model is: q e =k*C e 1 / n ;
[0152] Taking the logarithmic transformation yields lnq e =lnk+1 / nlnC e .
[0153] Among them, C e Equilibrium concentration (mg / L); q e Q represents the equilibrium adsorption amount (mg / g) during adsorption; m σ is the saturated adsorption capacity (mg / g); b is the adsorption equilibrium constant; σ represents the magnitude of the binding force between the adsorbent and the adsorbate. k and n are constants at a given temperature.
[0154] At room temperature, a graph was plotted with nicotine concentration on the x-axis and adsorption amount on the y-axis; lnC... e lnq is the x-axis. e Plot the graph using C as the vertical axis; e As the x-axis, with C e / q e Plot the graph on the ordinate; then fit it to the Langmuir isotherm, and the result is as follows. Figures 4-6 .
[0155] Depend on Figure 4 Therefore, the equation at 22℃ is: y = 0.6717x + 0.0166R 2 =0.9957
[0156] The equation at 24℃ is: y = 0.6963x + 0.0134R 2 =0.9968
[0157] The equation at 26℃ is: y = 0.7017x + 0.0131R 2 =0.998
[0158] Depend on Figure 5 Therefore, the equation at 22℃ is: y = 0.6677x + 0.7099R 2 =0.8817
[0159] The equation at 24℃ is: y = 0.5125x + 0.7058R 2 =0.8918
[0160] The equation at 26℃ is: y = 0.5264x + 0.696R 2 =0.9437
[0161] Depend on Figure 6 Therefore, the equation at 22℃ is: y = 0.8889x + 0.0035R 2 =0.9957
[0162] The equation at 24℃ is: y = 0.9136x + 0.0752R 2 =0.9976
[0163] The equation at 26℃ is: y = 0.9076x + 0.0737R 2 =0.9987
[0164] The isothermal parameters for nicotine adsorption by dandelion adsorbent are shown in Table 7.
[0165] Table 7 Adsorption isotherm parameters
[0166]
[0167]
[0168] The Langmuir and Freundlich isotherm models were used to fit the data at the three temperatures. The correlation coefficient R in Table 7 is used to obtain the results. 2 It can be seen that this adsorption process is more in line with the Freundlich isotherm model, that is, non-uniform multi-site adsorption.
[0169] 8. Single-factor experiment
[0170] After orthogonal processing, the optimal combination was selected to prepare dandelion adsorbent. Single-factor experiments were conducted to study the adsorption effects of dandelion residue particle size, addition amount, and temperature on nicotine.
[0171] (1) Effect of dandelion residue particle size on nicotine adsorption: Dried dandelion was pulverized using a pulverizer and passed through 8-mesh, 18-mesh, 40-mesh, 60-mesh, and 80-mesh sieves to obtain residues of different mesh sizes. 0.1g of residue from each mesh size was weighed and inserted into cigarettes for nicotine adsorption. The experiment was repeated three times, and the absorbance was measured to calculate the adsorption rate. Figure 7 As shown.
[0172] Depend on Figure 7 Observations revealed that as the particle size of dandelion residue increased, the nicotine adsorption rate initially increased and then decreased. The highest nicotine adsorption rate (43.48%) was observed when the dandelion residue was 40 mesh. Therefore, the optimal particle size for dandelion residue was determined to be 40 mesh. The resulting analysis of variance is shown in Table 8.
[0173] Table 8. Analysis of First-Order Variance Table
[0174]
[0175] Duncan's multiple comparisons are shown in Table 9.
[0176] Table 9. Multiple comparisons of nicotine adsorption by dandelion residue particle size.
[0177]
[0178] The data in Tables 8 and 9 show that different mesh sizes affect the adsorption efficiency of nicotine. The adsorption rate is worst at 8 mesh (35.27%), while the adsorption rate is highest at 40 mesh (43.48%).
[0179] (2) Effect of dandelion residue addition amount on nicotine adsorption: Based on the particle size of dandelion residue, the best adsorption effect for nicotine was observed when the residue was 40 mesh. Therefore, 8-mesh and 18-mesh residue were pulverized to the optimal mesh size, and 0.06g, 0.08g, 0.10g, 0.12g, and 0.14g of the 40-mesh dandelion residue were weighed for adsorption. The absorbance was repeatedly measured, and the adsorption rate for different addition amounts was calculated. Figure 8 As shown.
[0180] Depend on Figure 8 It can be seen that as the amount of dandelion adsorbent added increases, its adsorption rate for nicotine generally shows an upward trend. When the amount added reaches 0.14g, its adsorption rate for nicotine is 44.44%. Therefore, the optimal amount of dandelion residue to add is 0.14g.
[0181] The variance analysis of the added amount is shown in Table 10.
[0182] Table 10 Analysis of First-Order Variance Table
[0183]
[0184] Duncan's multiple comparisons are shown in Table 11.
[0185] Table 11 Multiple comparisons of nicotine adsorption by dandelion residue addition amount
[0186]
[0187] Tables 10 and 11 show that different amounts of nicotine added affect the adsorption effect. The adsorption rate is the worst at 35.75% when the amount added is 0.06g; the adsorption rate is the highest at 44.44% when the amount added increases to 0.14g.
[0188] (3) Effect of temperature on nicotine adsorption: Experiments were conducted at 18℃, 20℃, 22℃, 24℃, and 26℃, and the absorbance was measured to obtain the adsorption rate. Figure 9 As shown.
[0189] Depend on Figure 9It can be seen that as the temperature gradually increases, the adsorption rate of nicotine by dandelion adsorbent gradually increases, and the adsorption rate reaches its maximum value of 42.26% when the temperature reaches 26℃.
[0190] The temperature variance analysis table is shown in Table 12.
[0191] Table 12 Analysis of First-Order Variance Table
[0192]
[0193] Duncan's multiple comparisons are shown in Table 13:
[0194] Table 13 Multiple comparisons of the effects of temperature on nicotine adsorption
[0195]
[0196] As can be observed from Tables 12 and 13, temperature has a relatively small effect on nicotine adsorption. The adsorption rate is lowest at 18℃, at 41.28%, while the adsorption rate is highest at 26℃, at 42.26%.
[0197] Adsorption thermodynamics
[0198] According to the commonly used calculation method for adsorption thermodynamic parameters adopted by Saltal et al., the formulas for calculating thermodynamic parameters are as follows:
[0199] △G0=-RTlnK D
[0200] K D =q e / C e
[0201] △G0=△H0-T△S0
[0202] lnK D = -△H0 / R*(1 / T)+△S0 / R
[0203] Where ΔG0 is the standard Gibbs free energy, in kJ / mol; R is the thermodynamic gas constant, with a value of 8.314 J / (mol*K); T(K) is the thermodynamic temperature; q e The equilibrium adsorption amount during adsorption is expressed in mg / g; C e ΔH0 is the concentration at equilibrium, in mg / L; ΔH0 is the enthalpy change of the reaction, in kJ / mol; ΔS0 is the entropy change, in J / (mol·K).
[0204] The relationship between temperature and adsorption capacity is as follows: Figure 10 As shown, temperature and lnK D Relationship such as Figure 11 As shown.
[0205] Table 14 Thermodynamic parameters of nicotine adsorption by dandelion adsorbent
[0206]
[0207] Depend on Figures 10-11 As shown in Table 14, ΔH0 > 0, therefore this adsorption process is endothermic; ΔG0 < 0, this adsorption is spontaneous; as shown in the figure, the correlation coefficient R between temperature and thermodynamics is... 2 The value is 0.937, which is close to 1, indicating that the process fits thermodynamics very well and conforms to this law.
[0208] 9. Adsorption kinetics
[0209] In adsorption kinetic studies, pseudo-first-order and pseudo-second-order kinetic equations are typically used to fit experimental data to analyze the relationship between adsorption performance and time, thereby designing efficient adsorption systems. Pseudo-first-order adsorption is dominated by physisorption with chemisorption as a secondary process; pseudo-second-order adsorption is dominated by chemisorption with physisorption as a secondary process.
[0210] The equation of the pseudo-first-order dynamic model is: lg(q) e -q t )=lnq e -k1t;
[0211] The equation for the pseudo-second-order dynamic model is: t / q t =1 / k2q e 2 )+t / q e .
[0212] Where: q e To balance the adsorption capacity (mg / g); q t k is the amount of adsorption at adsorption time t (mg / g); k1 is the first-order adsorption rate constant (min). -1 k2 is the second-order adsorption rate constant (g·mg). -1 ·min -1 ).
[0213] In the adsorption kinetics experiment, the change in adsorption amount is studied with time t as the horizontal axis; with time t as the horizontal axis, ln(q) is used as the vertical axis. e -q t Using t as the ordinate, fit the first-order dynamic equation; using time t as the abscissa, and t / q as the ordinate. t Using y as the ordinate, the second-order dynamic equations were fitted. The results are shown below (see attached table). Figures 12-14 .
[0214] The adsorption kinetic parameters of nicotine by dandelion adsorbent are shown in Table 15.
[0215] Table 15 Adsorption kinetic parameters
[0216]
[0217]
[0218] As shown in Table 15, the correlation coefficient R of the pseudo-first-order kinetic curves is... 2 (0.8982) is much smaller than the R of the pseudo-second-order dynamic curve. 2 The value of (0.9819) indicates that the adsorption of nicotine by the treated dandelion is more inclined to a pseudo-second-order kinetic curve, meaning that the adsorption process is mainly chemical adsorption with physical adsorption as a secondary process.
[0219] 10. Horizontal comparison experiment
[0220] The optimal combination of dandelion residue obtained from the comprehensive single-factor analysis results was compared with the results measured by commercially available activated carbon, diatomaceous earth, and cellulose acetate under the same conditions. Since the dandelion adsorbents prepared in Examples 1-4 have similar nicotine adsorption effects, the adsorption effect of the dandelion adsorbent in Example 1 is used as an example for illustration, and compared with the adsorption effects of diatomaceous earth, activated carbon, and cellulose acetate on nicotine. The results are as follows: Figure 15 As shown.
[0221] Depend on Figure 15 Observations show that within this experimental range, under the condition of 80 mesh and with other factors (such as the amount added and the time being the same), the adsorption effect, from best to worst, is as follows: dandelion adsorbent > diatomaceous earth > activated carbon > raw dandelion > cellulose acetate. The dandelion adsorbent is more effective than other materials, and the dandelion adsorbent residue prepared by this invention is relatively the most economical.
[0222] The variance analysis of the different materials is shown in Table 16.
[0223] Table 16. Analysis of Variance for Different Materials
[0224]
[0225] The multiple comparisons among the different materials are shown in Table 17.
[0226] Table 17 Multiple Comparison Table Among Different Materials (Duncan Method)
[0227]
[0228]
[0229] Multiple comparisons at different times are shown in Table 18.
[0230] Table 18 Multiple Comparison Table at Different Times (Duncan's Method)
[0231]
[0232] Tables 16-18 show that different adsorption times and different materials have a significant impact on the adsorption effect, and the interaction between the two also affects the adsorption effect. The tables reveal that the treated dandelion residue exhibits a better adsorption effect for nicotine than the other four materials.
[0233] 11. Mechanism Characterization Analysis
[0234] (1) The X-ray diffractometer for the dandelion adsorbent of this invention is as follows: Figure 16
[0235] Depend on Figure 16 As can be seen, A represents the dandelion adsorbent after adsorption, B represents the dandelion adsorbent prepared in this invention, and C represents the original dandelion. The positions of the diffraction peaks of the original dandelion, the dandelion adsorbent, and the dandelion adsorbent after adsorption did not change significantly, with a strong characteristic diffraction peak appearing at around 22.5°, representing the crystalline region of cellulose. The figure shows that the diffraction peaks are: post-adsorption residue > post-treatment residue > original residue, indicating that after a series of treatments, the structure of cellulose becomes more ordered, and the stability of its physical structure increases.
[0236] (2) Infrared spectroscopy analysis, such as Figure 17 As shown
[0237] exist Figure 17 In the diagram, A represents the dandelion adsorbent after adsorption, B represents the dandelion adsorbent before adsorption, and C represents the original dandelion. At a wavenumber of 3508 cm⁻¹... -1 The presence of stretching vibrations of -OH groups at a certain point indicates that the -OH group plays a role in the adsorption process; at a wavenumber of 1637.92 cm⁻¹... -1 The change in waveform indicates that the C / C bonds play a role in the adsorption process. Furthermore, the CO and CH bonds also show corresponding changes, indicating that these groups also play a role in adsorption. Therefore, chemisorption plays a crucial role in this adsorption process.
[0238] (3) The elemental analysis results of dandelion adsorbent are shown in Table 19.
[0239] Table 19 Elemental Analysis of Three Materials
[0240]
[0241] As shown in Table 19, dandelion mainly contains C, N, H and S elements. Observation of each element shows that after treatment, the C, N and H elements of the original dandelion all show an increasing trend, while the S element shows a decreasing trend. After the dandelion adsorbent prepared in this invention adsorbs nicotine, the C, N and H elements all increase, while the S element decreases.
[0242] Obviously, those skilled in the art can make various modifications and variations to this invention without departing from its spirit and scope. Therefore, if these modifications and variations fall within the scope of the claims of this invention and their equivalents, this invention also intends to include these modifications and variations.
Claims
1. A method for preparing a dandelion adsorbent, characterized by, Includes the following steps: Wash the dandelion, boil it in boiling water until it is neutral, add α-amylase solution, treat it in a water bath at 85-90℃, wash it, and you will get enzymatically hydrolyzed dandelion. An alkaline solution was added to the enzymatically hydrolyzed dandelion, and the mixture was ultrasonically treated at 65–70°C, washed, dried at a constant temperature, and pulverized to obtain the dandelion adsorbent.
2. The production method according to claim 1, characterized by, The concentration of the α-amylase solution is 0.001–0.0026 mol / L.
3. The preparation method according to claim 1, characterized in that, The ratio of dandelion to α-amylase solution is 1g:80-100mL.
4. The production method according to claim 1, characterized by, The alkaline solution is a potassium hydroxide solution with a concentration of 0.1–0.5 mol / L.
5. The preparation method according to claim 1, characterized in that, The ratio of enzymatically hydrolyzed dandelion to alkaline solution is 1-2 g: 100 mL.
6. The method of claim 1, wherein, The ultrasonic power is 150W.
7. The preparation method according to claim 1, characterized in that, After being pulverized, the dandelion adsorbent has a mesh size of 20-60 mesh.
8. A dandelion adsorbent prepared by the preparation method according to any one of claims 1 to 7.
9. The use of the dandelion adsorbent according to claim 8 in the removal of nicotine.
10. Use according to claim 9, characterized in that, The specific application involves removing the fibers from a cigarette filter, placing the dandelion adsorbent inside the cigarette filter, and then absorbing the smoke through the cigarette filter after lighting the cigarette.