CN110540230A - Modified porous cattail straw biochar with tooth whitening and antibacterial effects - Google Patents
Modified porous cattail straw biochar with tooth whitening and antibacterial effects Download PDFInfo
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Abstract
The invention provides a preparation method of modified porous cattail stem charcoal with tooth whitening and antibacterial effects, cattail stems are refined to 2000-3000 meshes through toughening and ball milling, zinc oxide nano particles with antibacterial effects are modified on the surface of the porous cattail stem charcoal, the charcoal taking cattail stems as raw materials is obtained through twice pyrolysis and zinc oxide modification, the prepared porous cattail stem charcoal modified by a nano zinc oxide layer is used as a novel tooth whitening antibacterial material, not only has similar whitening effects, but also obviously reduces damage to an enamel structure, the specific surface area of the porous cattail stem charcoal loaded with zinc oxide is high, active pigments and bacterial toxins tightly attached to the surfaces of teeth can be effectively adsorbed, and the charcoal also has good antibacterial capability.
Description
Technical Field
The invention relates to a tooth whitening charcoal with an antibacterial effect and a preparation method thereof, and belongs to the field of daily chemical materials.
Background
Tooth whitening materials have been widely used whitening health products in modern life. The discoloration of teeth can be classified as intrinsic, extrinsic or both, depending on their location and etiology. Extrinsic discoloration of teeth is caused by pigments produced by habitual ingestion of diets (e.g., coffee, tea, chocolate, beverages, smoking, etc.) or by deposition of pigments produced by bacteria in the mouth on the tooth surface, while intrinsic discoloration is usually formed during tooth development. Dental plaque is closely related to caries, gingival inflammation, bleeding and periodontal disease, so we must constantly prevent and treat dental plaque to keep it at a low level and prevent it from developing.
Techniques for tooth whitening are roughly classified into invasive whitening and non-invasive whitening. Clinical whitening procedures include full crown repair and laminated veneer repair. These procedures necessitate grinding and cutting of the enamel, which can cause irreversible damage to the teeth. Minimally invasive whitening generally refers to chemically bleaching teeth. Hydrogen peroxide or carbamide peroxide are the most commonly used tooth bleaching agents, but long-term use can cause a series of problems, such as enamel demineralization, tooth sensitivity, gum irritation, acute pulpitis and the like. Therefore, the tooth whitening powder which has no damage to the teeth and simultaneously has antibacterial effect is of great significance.
typha latifolia, also called water candle, is widely distributed and often grows in swamp lands on the bank of rivers, lakes and banks. Is a wild vegetable in China, and the pseudostem white and tender part (namely the great cattail) and the tender part (namely the grass buds) at the tip of the underground stolons can be eaten, and the taste is fresh and delicious. Pollen, called pollen Typhae, has the effects of diminishing inflammation, stopping bleeding and promoting urination; the female flower can be used as "cattail wool" and can be filled into bed pillow. The inflorescence can be used as cut flower or dried flower. The water candle is a traditional Chinese waterscape flower and is used for beautifying the water surface and the wetland. The leaves of the water candle can be used as a weaving material; the stem and leaf fiber can be used for making paper, the straw is often used for weaving, and the prior published technology has no report of using the straw for tooth whitening or antibiosis.
The invention content is as follows:
Aiming at the problems in the background technology, the invention provides a technology for preparing nano zinc oxide modified porous cattail straw biochar with tooth whitening and antibacterial effects.
The invention is realized by the following technical scheme: a preparation method of modified porous cattail straw biochar with tooth whitening and antibacterial effects comprises the following steps:
(1) Washing the cattail straw with distilled water for 2-5 times to remove dirt particles, then drying in an oven for 24 hours, then thinning the cattail straw, putting the cattail straw into a tubular furnace for carbonization for 2 hours at the temperature of 800 ℃ and at the heating rate of 10 ℃/min for first pyrolysis to obtain the cattail straw biochar.
(2) Soaking the straw biochar obtained in the step (1) in a potassium hydroxide solution with the concentration of 1 mol.L < -1 >, wherein the soaking ratio is 1: 1, the mixture is then dehydrated in an oven for 12 hours.
(3) Crushing the cattail straw biochar, placing the cattail straw biochar in a nitrogen tube type furnace with the purity of 99.995%, controlling the nitrogen flow rate to be 150cm3 & min < -1 > for second pyrolysis, pretreating at the temperature of 400 ℃ for 1 hour, heating to 800 ℃ for pyrolysis for 1 hour, and washing with deionized water to remove residual chemical impurities.
(4) and (4) transferring the charcoal powder obtained in the step (3) into a 250mL beaker, adding 0.1 mol. L < -1 > hydrochloric acid, stirring for 1 hour, washing with hot deionized water until the pH value of the washed solution is 6-7, and drying to obtain the porous cattail straw charcoal.
(5) Dissolving 1g of porous cattail straw biochar in 270mL of deionized water, performing ultrasonic treatment for 1 hour, adding 2.208g of zinc chloride and 0.135g of sodium carboxymethylcellulose, adding 216mL of concentrated nitric acid, and adjusting the pH value to 2; dissolving 1.532g of sodium borohydride in 135mL of deionized water, performing the process in an argon atmosphere, dropwise adding the sodium borohydride solution into a biochar solution at 90 ℃, keeping for 4 hours, taking out a sample, washing and drying to obtain the nano zinc oxide modified porous cattail stem biochar.
A preparation method of modified porous cattail straw biochar with tooth whitening and antibacterial effects comprises the following steps: the refining step in the step (1) is as follows: putting the dried cattail stalks sheared to 1mm into a 2L ball mill, mixing high-chromium steel ball grinding balls with the diameters of 1.0cm, 1.5cm and 2.0cm according to the weight ratio of 2:5:3, adding the high-chromium steel balls into the ball mill, grinding the ball mill for 90min, and grinding the cattail stalks to 700 plus 1000-mesh coarse powder; adding 50g of the prepared coarse powder into a 0.5L ball mill, adding water accounting for 5-10% of the weight of the cattail straw into the ball mill to prepare cattail straw pulp, mixing high-chromium steel ball grinding balls with the diameters of 6mm, 8mm and 10mm according to the weight ratio of 2:6:4, adding 0.3-0.5kg of the high-chromium steel balls into the high-chromium steel balls, grinding the mixture for 2-3h, and drying the mixture to remove water to obtain fine powder with the particle size of 3000 meshes of 2000 plus materials.
The biochar comprises the following components: it can be used for whitening teeth and resisting bacteria.
the invention has the advantages of
(1) The surface of the porous cattail straw biochar is modified with zinc oxide nano-particles with antibacterial effect, the tooth whitening effect, antibacterial property and biological safety of the product are deeply researched, and compared with the commercially available whitening toothpaste and antibacterial toothpaste, the results show that the whitening and antibacterial effects of the porous cattail straw biochar modified by the nano-zinc oxide are better than those of the commercially available whitening toothpaste and antibacterial toothpaste.
(2) Meanwhile, the use process of the nano zinc oxide modified porous cattail straw biochar does not damage the surface of tooth enamel, and the nano zinc oxide modified porous cattail straw biochar is biologically safe tooth antibacterial and whitening powder.
(3) Aiming at the characteristic of stronger toughness of the straw, the two-stage ball milling double refinement of the invention is adopted, so that the particle size of the straw can be refined to 2000-3000 meshes, and the straw has good adsorption when being used for whitening teeth.
(4) Compared with the traditional clinical whitening agent (peroxide), the nano zinc oxide layer modified porous cattail straw biochar serving as a novel tooth whitening antibacterial material has a similar whitening effect, obviously reduces damage to an enamel structure, has a high specific surface area, can effectively adsorb active pigments and bacterial toxins tightly attached to the surface of teeth, and has good antibacterial capacity.
drawings
FIG. 1(a-c) is a scanning electron microscope image of porous pythagoras biochar; (d-f) is a scanning electron microscope picture of the nano zinc oxide modified porous cattail straw biochar.
FIG. 2(a-b) is X-ray diffraction spectrum and Fourier infrared spectrum of zinc oxide particle, porous cattail straw charcoal and nano zinc oxide modified porous cattail straw charcoal.
Fig. 3 is a dental professional colorimetric card.
Fig. 4(a-d) is a graph showing the whitening effect of a toothbrush on teeth, wherein the nano zinc oxide modified porous cattail straw biochar, the porous cattail straw biochar and a commercially available whitening toothpaste are used independently.
FIG. 5(a-d) is a diagram showing the antibacterial effect of the blank set, the porous cattail straw biochar, the commercial antibacterial toothpaste and the nano-zinc oxide modified porous cattail straw biochar, respectively; (e-h) corresponding plate colony count map; (i) the antibacterial rate of the porous cattail straw biochar, the commercial antibacterial toothpaste and the nano zinc oxide modified porous cattail straw biochar.
Fig. 6 is a graph showing HE (hematoxylin-eosin) staining of heart, liver, spleen, lung and kidney of the control and experimental mice.
Detailed Description
Example 1
1. The preparation process of the nano zinc oxide modified porous cattail straw biochar comprises the following steps:
Washing the cattail straw with distilled water for 2-5 times to remove dirt particles, then drying in an oven for 24 hours, then thinning the cattail straw, putting the cattail straw into a tubular furnace for carbonization for 2 hours at the temperature of 800 ℃ and at the heating rate of 10 ℃/min for first pyrolysis to obtain the cattail straw biochar. Soaking the obtained straw biochar in a potassium hydroxide solution with the concentration of 1 mol.L < -1 >, wherein the soaking ratio is 1: 1, the mixture is then dehydrated in an oven for 12 hours. Crushing the cattail straw biochar, placing the cattail straw biochar in a nitrogen tube type furnace with the purity of 99.995%, controlling the nitrogen flow rate to be 150cm3 & min < -1 > for second pyrolysis, pretreating at the temperature of 400 ℃ for 1 hour, heating to 800 ℃ for pyrolysis for 1 hour, and washing with deionized water to remove residual chemical impurities. Transferring the obtained charcoal powder into a 250mL beaker, adding 0.1 mol/L-1 hydrochloric acid, stirring for 1 hour, washing with hot deionized water until the pH value of the washing is 6-7, and drying to obtain the porous cattail straw charcoal as shown in figure 1 (a-c).
The refining steps are as follows: putting the dried cattail straws sheared to 1mm into a 2L ball mill, mixing high-chromium steel ball grinding balls with the diameters of 1.0cm, 1.5cm and 2.0cm according to the weight ratio of 2:5:3, adding the high-chromium steel balls into the ball mill, wherein the total weight of the high-chromium steel balls is 2.5kg, grinding the high-chromium steel balls for 90min, and grinding the cattail straws into 800-mesh coarse powder; adding 50g of the prepared coarse powder into a 0.5L ball mill, adding water accounting for 10% of the weight of the cattail straw into the ball mill to prepare cattail straw pulp, mixing high-chromium steel ball grinding balls with the diameters of 6mm, 8mm and 10mm according to the weight ratio of 2:6:4, adding 0.3kg of the high-chromium steel balls into the high-chromium steel balls, grinding the mixture for 2 hours, and drying the mixture to remove water to obtain 2500-mesh fine powder.
Dissolving 1g of porous cattail straw biochar in 270mL of deionized water, performing ultrasonic treatment for 1 hour, adding 2.208g of zinc chloride and 0.135g of sodium carboxymethylcellulose, adding 216mL of concentrated nitric acid, and adjusting the pH value to 2; 1.532g of sodium borohydride was dissolved in 135mL of deionized water and the process was carried out under an argon atmosphere. The above sodium borohydride solution was added dropwise to the charcoal solution at 90 ℃ and held for 4 hours. Taking out the sample, washing and drying to obtain the nano zinc oxide modified porous cattail straw biochar as shown in figure 1 (d-f).
Fig. 2(a) shows the X-ray diffraction patterns of zinc oxide, porous pygma biochar and nano zinc oxide modified porous pygma biochar, with the peaks indicating good crystallinity of zinc oxide. The 5 peak patterns in the range of 30-60 ° on the abscissa are characteristic peaks of the ZnO polycrystalline hexagonal wurtzite structure. FIG. 2(b) shows the Fourier transform infrared spectra (wave number: 4000-. The shape of the IR spectrum of ZnO nanoparticles is generally affected by the particle size and morphology, the degree of particle aggregation, or the crystal structure of ZnO polycrystals, and the peak center of the infrared band of Zn-O bonds is shown to be located at 430 cm-1.
2. Whitening effect of nano-zinc oxide modified porous cattail straw biochar on teeth
Tens of teeth with equal size and similar color are soaked in the concentrated tea and coffee, taken out after three days, compared with a dental professional colorimetric card, and the teeth with 16 color levels are taken out for later use. Then dividing the colored teeth into four groups, one group is used as a blank group, brushing for 3min by independently dipping water in a toothbrush, and the other three groups are respectively and uniformly coated on the surfaces of the teeth by 1000 g.L < -1 > nanometer zinc oxide modified porous cattail straw charcoal powder, porous cattail straw charcoal powder and commercially available whitening toothpaste, and brushing for 3min by using the toothbrush. The rinsed crown portion was then compared to a dental professional color chart (fig. 3).
As shown in fig. 4, after all the 3-minute brushing experiments were completed, the color change before and after tooth brushing was compared with a dental professional color chart under the same illumination condition. According to the dental professional color card, the Vita color scale of the tooth color is improved from C4 to A4 by brushing the teeth with a toothbrush only, and only 1-grade whitening change occurs; when the whitening toothpaste is used for brushing teeth, the Vita color level of the tooth color is improved from C4 to A3.5, and the whitening change of level 4 is generated; when the teeth are brushed by using the porous cattail charcoal, the Vita color scale of the tooth color is improved from C4 to D4, and 6-grade whitening change occurs; after the nano zinc oxide modified porous cattail straw charcoal powder is used for brushing teeth, the Vita color scale of the tooth color is improved from C4 to B2, and the 13-grade whitening change is generated. Therefore, the nano-zinc oxide modified porous pythagoras bio-char has an ideal effect as a tooth whitening agent, and can effectively remove exogenous pigments (such as coffee, black tea, green tea, and the like) attached to the surface of teeth.
3. Antibacterial effect test of nano-zinc oxide modified porous cattail stem biochar
The 4 prepared teeth were washed clean, sterilized under high pressure and high pressure, and then co-cultured with staphylococcus aureus. One of the three materials is brushed for 3 minutes by a sterilized toothbrush, and the other 3 materials are respectively brushed for 3 minutes by a sterilized toothbrush after being added with nano zinc oxide modified porous cattail straw charcoal, porous cattail straw charcoal powder and commercially available antibacterial toothpaste. Next, 4 teeth were washed 2 times with phosphate buffered saline (PBS, pH 7.4), and Staphylococcus aureus remaining on the tooth surface was observed by a scanning electron microscope after the drying treatment.
After the 4 cleaned teeth were sterilized at high temperature and high pressure, they were co-cultured with staphylococcus aureus. One of the three materials is brushed for 3 minutes by using a sterilized toothbrush, and the other 3 materials are respectively brushed for 3 minutes by using nano zinc oxide modified porous cattail straw biochar, porous cattail straw biochar powder and commercially available antibacterial toothpaste. Then, the teeth are continuously co-cultured with staphylococcus aureus for 2 hours, and the antibacterial performance of three samples of nano zinc oxide modified porous cattail straw biochar, porous cattail straw biochar powder and commercially available antibacterial toothpaste on staphylococcus aureus is calculated by a plate-coating colony counting method.
As shown in figure 5, staphylococcus aureus can not be observed on the tooth surface brushed by the nano zinc oxide modified porous cattail straw biochar, and the material has excellent antibacterial activity on gram-positive bacteria staphylococcus aureus and has better antibacterial effect than the commercially available antibacterial toothpaste. From fig. 4.10(e-h), we quantitatively evaluate the antibacterial property of the toothpaste by using a plate colony counting method, and obtain fig. 4.10(i), wherein the bacteriostatic rate of the porous cattail straw biochar modified by the rice zinc oxide on staphylococcus aureus is close to 100% and is far higher than that of the antibacterial toothpaste.
4. Biological safety test of nano-zinc oxide modified porous cattail stem biochar
8 male Kunming mice (about 30g each) were prepared, 4 of which served as control groups and 4 of which served as test groups. After the mice are adapted for one week, oral gavage tests are carried out on the mice by using the nano zinc oxide modified porous cattail straw biochar solution at the dose of 35mg/kg every day, and the same gavage process is carried out on a control group by using normal saline. Five days after dosing, mice were dissected and histopathological examination was performed. The liver, kidney, lung, spleen and heart tissues of the experimental group and the control group were dissected and fixed with 4% paraformaldehyde solution, and the tissues were obtained by routine collection, dehydrated, paraffin-embedded, and sectioned (4 μm thick) and stained with hematoxylin-eosin. Then, we observed their histopathological features by light microscopy.
as shown in fig. 6, compared with the control group, the myocardial fibers in the visual field of the experimental group are closely arranged, the staining is uniform, the boundary is clear, the morphology is normal, a small amount of red blood cells are visible in the interstitial space of the myocardium, and the tissues are not obviously abnormal; the liver cell cytoplasm in the visual field is loose and lightly stained, and tissues have no obvious necrosis or inflammatory reaction; the red and white marrow in the visual field has clear division, white marrow lymphocytes are rich, and tissues have no obvious abnormality; the alveolus in the visual field is uniform in size, the alveolar wall is uniform in thickness, the bronchial epithelial cells are closely arranged and normal in shape, the alveolus and the bronchial lumen are clean, and the tissues are not obviously abnormal; the renal tubules are arranged closely in the visual field, the renal tubule epithelial cells are normal in shape, and no obvious abnormality is seen in the tissues. H & E (hematoxylin-eosin) staining results show that the heart, the liver, the spleen, the lung and the kidney of the mice are normal after being perfused with the porous cattail charcoal modified by the nano zinc oxide. In fact, only a trace amount of the tooth whitening agent is introduced into the stomach through the mouth during actual use. The experiment shows that even if a small amount of the nano zinc oxide modified porous cattail stem biochar is absorbed, the prepared nano zinc oxide modified porous cattail stem biochar does not bring obvious harm to tissues and organs.
Claims (3)
1. A preparation method of modified porous cattail straw biochar with tooth whitening and antibacterial effects is characterized by comprising the following steps:
(1) Washing the cattail straw with distilled water for 2-5 times to remove dirt particles, then drying in an oven for 24 hours, then thinning the cattail straw, putting the cattail straw into a tubular furnace for carbonization for 2 hours at the temperature of 800 ℃ and at the heating rate of 10 ℃/min for first pyrolysis to obtain cattail straw biochar;
(2) Soaking the straw biochar obtained in the step (1) in a potassium hydroxide solution with the concentration of 1 mol.L < -1 >, wherein the soaking ratio is 1: 1, then dehydrating the mixture in an oven for 12 hours;
(3) Crushing the cattail straw biochar, placing the cattail straw biochar in a nitrogen tube type furnace with the purity of 99.995%, controlling the nitrogen flow rate to be 150cm3 & min < -1 > for second pyrolysis at the temperature of 400 ℃, pretreating for 1 hour, then heating to 800 ℃ for pyrolysis for 1 hour, and washing with deionized water to remove residual chemical impurities;
(4) Transferring the charcoal powder obtained in the step (3) into a 250mL beaker, adding 0.1 mol. L-1 hydrochloric acid, stirring for 1 hour, washing with hot deionized water until the pH value of the washing is 6-7, and drying to obtain porous cattail straw charcoal;
(5) Dissolving 1g of porous cattail straw biochar in 270mL of deionized water, performing ultrasonic treatment for 1 hour, adding 2.208g of zinc chloride and 0.135g of sodium carboxymethylcellulose, adding 216mL of concentrated nitric acid, and adjusting the pH value to 2; dissolving 1.532g of sodium borohydride in 135mL of deionized water, performing the process in an argon atmosphere, dropwise adding the sodium borohydride solution into a biochar solution at 90 ℃, keeping for 4 hours, taking out a sample, washing and drying to obtain the nano zinc oxide modified porous cattail stem biochar.
2. The preparation method of the modified porous cattail straw biochar with tooth whitening and antibacterial effects as claimed in claim 1, is characterized in that: the refining step in the step (1) is as follows: putting the dried cattail stalks sheared to 1mm into a 2L ball mill, mixing high-chromium steel ball grinding balls with the diameters of 1.0cm, 1.5cm and 2.0cm according to the weight ratio of 2:5:3, adding the high-chromium steel balls into the ball mill, grinding the ball mill for 90min, and grinding the cattail stalks to 700 plus 1000-mesh coarse powder; adding 50g of the prepared coarse powder into a 0.5L ball mill, adding water accounting for 5-10% of the weight of the cattail straw into the ball mill to prepare cattail straw pulp, mixing high-chromium steel ball grinding balls with the diameters of 6mm, 8mm and 10mm according to the weight ratio of 2:6:4, adding 0.3-0.5kg of the high-chromium steel balls into the high-chromium steel balls, grinding the mixture for 2-3h, and drying the mixture to remove water to obtain fine powder with the particle size of 3000 meshes of 2000 plus materials.
3. the modified porous pythagoras biochar with tooth whitening and antibacterial effects as claimed in claim 1, is characterized in that: the charcoal is applied to whitening teeth and resisting bacteria.
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| CN112715606A (en) * | 2021-01-08 | 2021-04-30 | 中国药科大学 | Biscuit with anti-helicobacter pylori activity and preparation method thereof |
| CN114983849A (en) * | 2022-01-10 | 2022-09-02 | 宁波楚月新材料科技有限公司 | Single-component visible light catalysis tooth whitening gel with low hydrogen peroxide concentration as well as preparation and application thereof |
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| CN114983849A (en) * | 2022-01-10 | 2022-09-02 | 宁波楚月新材料科技有限公司 | Single-component visible light catalysis tooth whitening gel with low hydrogen peroxide concentration as well as preparation and application thereof |
| CN114983849B (en) * | 2022-01-10 | 2023-08-01 | 宁波楚月新材料科技有限公司 | Single-component low-hydrogen-peroxide-concentration visible light catalytic tooth whitening gel and preparation and application thereof |
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