CN110124618B - Hydrotalcite-plant cellulose composite pellet and preparation method and application thereof - Google Patents
Hydrotalcite-plant cellulose composite pellet and preparation method and application thereof Download PDFInfo
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- CN110124618B CN110124618B CN201910298898.8A CN201910298898A CN110124618B CN 110124618 B CN110124618 B CN 110124618B CN 201910298898 A CN201910298898 A CN 201910298898A CN 110124618 B CN110124618 B CN 110124618B
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
Abstract
The invention discloses a hydrotalcite-plant cellulose composite pellet and a preparation method and application thereof. The preparation method comprises the following steps: adding plant cellulose powder and hydrotalcite into a mixed aqueous solution of polyvinyl alcohol and sodium alginate, uniformly mixing, adding the mixed aqueous solution into a mixed aqueous solution of boric acid and calcium chloride, and calcification to obtain the hydrotalcite-plant cellulose composite pellet. The plant cellulose and the hydrotalcite selected by the invention have wide sources, are safe and have no toxicity; the preparation process is simple, other pollutants are not doped, the spherical size is controllable, the experimental operation is easy, and the recovery is convenient; the prepared hydrotalcite-plant cellulose composite pellet can effectively adsorb and treat nano-scale plastics.
Description
Technical Field
The invention belongs to the technical field of sewage purification treatment in environmental protection, and particularly relates to a hydrotalcite-plant cellulose composite pellet as well as a preparation method and application thereof.
Background
Due to the unique layered structure, hydrotalcite (hydrotalcite) has wide application prospect in the fields of catalysis, medicine, ion exchange, adsorption and the like. Hydrotalcite is generally in powder form and, although effective in treating contaminants in water, is not conducive to recovery. The cellulose is extracted from pennisetum hydridum which is a plant with large biological quantity, has the characteristics of strong tillering property, high growth speed, high yield, rich nutrition, capability of being harvested for many years and the like, and pennisetum hydridum leaves can be used as feed for feeding herbivorous animals such as cows, sheep, rabbits, fishes and the like and also can be widely applied to the fields of papermaking, food and the like; meanwhile, pennisetum hydridum has developed fibrous root systems, strong drought resistance, low requirement on soil and the like, and is gradually applied to the ecological environment control and protection aspects such as the re-greening of barren mountains, water and soil balance maintenance, soil structure restoration and improvement, and the like in recent years, but a large amount of straws including pennisetum hydridum still face the situation of being discarded and burnt, pollute the environment and are not beneficial to resource utilization, so if pennisetum hydridum (or straws of other plants, such as corn straws, rice straws and the like) can be used for extracting cellulose, the ecological, environmental, social and economic benefits can be simultaneously realized, and the value is played in multiple aspects. Cellulose is a natural high molecular polysaccharide which is the most widely distributed in the nature, is a precious natural renewable resource owned by human beings, and has the characteristics of large surface area, large specific surface area and easy adsorption, and a large amount of hydroxyl groups are contained on the surface.
The cellulose adsorbent is powdery, and subsequent recovery work is difficult to carry out in practical application. In addition, for the removal of plastics below the micron level at present, a membrane bioreactor can be used for treating primary effluent and different three-level treatment technologies (reverse filtration, rapid sand filtration and dissolved air flotation) can be used for treating secondary effluent, so that the engineering is large and the process is complex.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention mainly aims to provide a preparation method of hydrotalcite-plant cellulose composite pellets.
Another object of the present application is to provide a hydrotalcite-plant cellulose composite pellet prepared by the above method.
Another object of the present invention is to provide an application of the above hydrotalcite-plant cellulose composite beads in the treatment of nano-scale plastics in water.
The purpose of the invention is realized by the following technical scheme:
a preparation method of hydrotalcite-plant cellulose composite pellets comprises the following steps:
(1) adding polyvinyl alcohol and sodium alginate into water, heating and stirring for dissolving to obtain a mixed solution, wherein the mass concentration of the polyvinyl alcohol in the mixed solution is 5-15%, and the mass concentration of the sodium alginate is 0.1-0.5%;
(2) adding plant cellulose powder and hydrotalcite into the mixed solution obtained in the step (1), and uniformly mixing, wherein the mass ratio of the plant cellulose powder to the hydrotalcite to the polyvinyl alcohol is 1: (1-2): (5-14);
(3) uniformly mixing the mixed solution obtained in the step (2) according to a volume ratio of 3: (3-5) dropwise adding the hydrotalcite-plant cellulose composite microspheres into a mixed aqueous solution of boric acid and calcium chloride, calcifying for 3-6h, and washing to obtain the hydrotalcite-plant cellulose composite microspheres.
The mass concentration of the polyvinyl alcohol in the step (1) is preferably 5-6%; the mass concentration of the sodium alginate is preferably 0.15-0.25%.
The specific preparation method of the mixed solution in the step (1) is preferably as follows: firstly, adding polyvinyl alcohol into water, stirring for 1.5h at 90 ℃ to obtain a polyvinyl alcohol solution, then cooling to be less than or equal to 80 ℃, adding a sodium alginate solution, and stirring for 1.5 h.
The specific preparation method of the mixed solution is more preferably: firstly, adding polyvinyl alcohol into water, stirring for 1.5h at 90 ℃ to obtain a polyvinyl alcohol solution, then cooling to 80 ℃, adding a sodium alginate solution, and stirring for 1.5 h.
The mass concentration of the polyvinyl alcohol solution is preferably 10-12%; the mass concentration of the sodium alginate solution is preferably 0.2-0.5%, and more preferably 0.3-0.5%.
The volume ratio of the polyvinyl alcohol solution to the sodium alginate solution is preferably 1: 1.
the plant cellulose powder in the step (2) is preferably pennisetum hydridum cellulose powder.
The preparation method of the pennisetum hydridum cellulose powder comprises the following steps: cutting and cleaning pennisetum hydridum, boiling in boiling water, drying, pulverizing, sieving, and drying to constant weight to obtain powder; mixing the powder according to the weight ratio of 1 g: adding 25ml of the mixture into a nitric acid ethanol solution, heating at 90 ℃ until the powder turns white, and then washing and drying to obtain the pennisetum hydridum cellulose powder.
The volume ratio of nitric acid to ethanol in the nital solution is preferably 1: (3-5), more preferably 1: 4; the concentration of the nitric acid is 65-68%.
The boiling time of the boiling water is preferably 2-4 h; the sieving is 100 mesh sieving.
The washing is preferably: washing with nital solution for 2 times, washing with hot water until the washing solution is neutral, and draining the filtrate.
The drying temperature is preferably 60 ℃, and the drying time is preferably 24-36 h.
The hydrotalcite of step (2) is preferably added to the mixed solution in the form of a hydrotalcite solution.
The mass concentration of the hydrotalcite solution is preferably 0.5-2%; more preferably 1-2%.
The hydrotalcite in the step (2) is calcined before use, the calcination temperature is preferably 500 ℃, and the calcination time is preferably 4 hours.
The hydrotalcite in the step (2) is preferably magnesium-aluminum type hydrotalcite.
The solvent of the hydrotalcite solution in the step (2) is preferably water.
Adding plant cellulose powder and hydrotalcite into the mixed solution obtained in the step (1) in the step (2), wherein the specific method comprises the following steps: uniformly dispersing plant cellulose powder in the mixed solution obtained in the step (1), and then adding hydrotalcite.
The method for uniformly dispersing is preferably to disperse by using an ultrasonic pulverizer.
The mass ratio of the plant cellulose powder, the hydrotalcite and the polyvinyl alcohol in the step (2) is preferably 1: (1-2): (10-12).
The preferable dripping condition of the step (3) is 30-40 drops/min and 0.02-1 ml/drop; more preferably 0.02 to 0.5 ml/drop. When the dropping condition is out of the range, the prepared small balls have uneven particle sizes, and the small balls are adsorbed due to the uneven difference of the particle sizes, so that the porosity among the particles is increased, and the adsorption effect is reduced.
The dropping method in the step (3) is preferably a liquid dropping method.
The liquid drop method is preferably carried out by using an injector, and the dropping speed is 30-40 drops/min and 0.02-1 ml/drop; more preferably, the injection is carried out using a 20ml syringe having a needle size of (1.2 to 1.6). times.31 mm.
The mass concentrations of the boric acid and the calcium chloride in the mixed aqueous solution of the boric acid and the calcium chloride in the step (3) are preferably 2-8% and 3-10% respectively; all more preferably 3-5%.
The calcification time in the step (3) is preferably 4-5 h.
The washing method in the step (3) is preferably: washing with water for 3-5 times.
The hydrotalcite-plant cellulose composite pellet prepared by the method.
The volume of the hydrotalcite-plant cellulose composite pellet is preferably 0.02-0.05 ml/pellet.
The application of the hydrotalcite-plant cellulose composite pellet in treating nano-scale plastics in water.
The application method comprises the following steps: adding hydrotalcite-plant cellulose composite pellets into water containing nano plastic particles, and carrying out constant-temperature oscillation treatment.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention selects polyvinyl alcohol and sodium alginate to obtain the hydrotalcite-plant cellulose composite bead with high specific surface area for adsorption.
(2) The plant cellulose and the hydrotalcite selected by the invention have wide sources, are safe and nontoxic, have main structures formed by combining two or more than two metal oxides, are in a layered structure with positive charges, and can improve the removal rate of the nano plastic and be beneficial to subsequent recovery treatment after being crosslinked with the cellulose into composite pellets.
(3) The hydrotalcite-plant cellulose composite bead adsorbent disclosed by the invention is simple in preparation process, free of other pollutants, controllable in spherical size, easy to operate in experiments and convenient to recover.
(4) The hydrotalcite-plant cellulose composite pellet prepared by the method can effectively adsorb and treat nano-scale plastics in water, and the removal rate can reach 68%.
Drawings
Fig. 1 is a scanning electron microscope surface image of the hydrotalcite-plant cellulose composite pellet prepared in example 1, wherein the magnification is 5000.
FIG. 2 is a scanning electron microscope sectional view of the hydrotalcite-plant cellulose composite pellet prepared in example 2, wherein the magnification is 5000.
FIG. 3 is a diagram of hydrotalcite-plant cellulose composite pellet prepared in example 2.
FIG. 4 is a schematic view (not formed into pellets) of the plant cellulose adsorbent obtained in comparative example 1.
Fig. 5 is a physical diagram (not capable of being compounded into pellets) of the hydrotalcite-plant cellulose composite prepared in comparative example 2.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
The nitric acid in the examples and the comparative examples of the application is a nitric acid solution with the concentration of 65-68%; the 20ml syringes each had a needle size of 1.2X 31 mm.
The volume of the hydrotalcite-plant cellulose composite pellets prepared by the embodiment of the invention is 0.02-0.05 ml/pellet.
The specific method for adsorbing water containing nano plastic by the hydrotalcite-plant cellulose composite pellets prepared in the embodiment of the application comprises the following steps:
3 parts (200 parts each) of the prepared hydrotalcite-plant cellulose composite bead adsorbent is weighed and respectively added into 50ml of adsorbate solution, and the mixture is subjected to constant-temperature oscillation in a constant-temperature oscillator for adsorption. The concentration of the nanoplastic in the water was measured at regular intervals.
The amount of adsorption (Qe) and the adsorption rate were calculated using the following formulas:
qe ═ Co-Ce) × V, and adsorption rate ═ Co-Ce)/Ce × 100%.
Wherein Co and Ce are respectively the initial concentration (mg. L) of adsorbate solution in water phase-1) And the concentration at equilibrium (mg. L)-1) (ii) a V is the volume of the liquid phase (L).
EXAMPLE 1 preparation of hydrotalcite-plant cellulose composite pellets
Pretreatment and cellulose extraction of pennisetum hydridum: cutting pennisetum hydridum into small sections, washing with tap water to remove dust on the surface, washing with ultrapure water twice, boiling in a pot filled with ultrapure water for 4h, oven drying, pulverizing with a pulverizer, sieving with a 100-mesh sieve, and drying in a drier to constant weight to obtain powder. Extracting cellulose by a nitric acid-ethanol method, and mixing the powder according to a mass-to-liquid ratio of 1 g: adding 25ml of the cellulose into 250ml of nitric acid ethanol solution (the volume ratio of nitric acid ethanol is 1:4), installing a condensation reflux device, heating in a water bath at 90 ℃ for 2 hours, washing the obtained cellulose powder with the nitric acid ethanol solution for 2 times, and washing with hot water until the washing liquid is neutral. And (4) draining the filtrate, and drying in an oven at 60 ℃ for 24h to obtain cellulose powder.
Preparation of hydrotalcite powder: adding magnesium-aluminum type hydrotalcite (Shaoyang Tiantang auxiliary chemical Co., Ltd.) into a muffle furnace, and sintering at 500 deg.C for 4 hr to obtain water-soluble hydrotalcite powder.
The preparation method of the hydrotalcite-plant cellulose composite pellet comprises the following steps: the hydrotalcite-plant cellulose composite pellet is prepared by an embedding method. Adding 12g of polyvinyl alcohol into 88ml of water, stirring in a water bath at 90 ℃ for 1.5h to completely dissolve the polyvinyl alcohol; adjusting the temperature to 80 ℃, adding 100ml of sodium alginate solution with the mass fraction of 0.5% into the polyvinyl alcohol aqueous solution, stirring for 1.5h to completely dissolve the sodium alginate, adding 1g of cellulose powder, and putting the mixture into an ultrasonic crusher to completely break the cellulose into the mixed solution. Adding 100ml of hydrotalcite solution with the mass fraction of 2% into the mixed solution, continuously stirring for 2 hours until the mixed solution is viscous, and carrying out a liquid drop method by using a 20ml syringe to mix the mixed solution according to the volume ratio of 3: 4, dripping (40 drops/min) into a cross-linking agent aqueous solution (wherein the mass concentration of boric acid is 3 percent, and the mass concentration of calcium chloride is 4 percent) prepared from boric acid and calcium chloride, forming hydrotalcite-plant cellulose composite pellets after calcification for 4 hours, washing for 3 times by using ultrapure water, storing in the ultrapure water for subsequent use.
The scanning electron microscope surface image of the hydrotalcite-plant cellulose composite beads (average diameter about 4mm) prepared in this example is shown in fig. 1.
EXAMPLE 2 preparation of hydrotalcite-plant cellulose composite pellets
Pretreatment and cellulose extraction of pennisetum hydridum: cutting pennisetum hydridum into small sections, washing with tap water to remove dust on the surface, washing with ultrapure water twice, boiling in a pot filled with ultrapure water for 4h, oven drying, pulverizing with a pulverizer, sieving with a 100-mesh sieve, and drying in a drier to constant weight to obtain powder. Extracting cellulose by a nitric acid-ethanol method, and mixing the powder according to a mass-to-liquid ratio of 1 g: adding 25ml of the cellulose powder into 250ml of a nitric acid ethanol solution (the volume ratio of nitric acid ethanol is 1:4), installing a condensation reflux device, heating in a water bath at 90 ℃ for 2 hours, washing the obtained cellulose powder with the nitric acid ethanol solution for 2 times, and washing with hot water until the washing liquid is neutral. And (4) draining the filtrate, and drying in an oven at 60 ℃ for 24h to obtain cellulose powder.
Preparation of hydrotalcite powder: adding magnesium-aluminum type hydrotalcite (Shaoyang Tiantang auxiliary chemical Co., Ltd.) into a muffle furnace, and sintering at 500 deg.C for 4 hr to obtain water-soluble hydrotalcite powder.
The preparation method of the hydrotalcite-plant cellulose composite pellet comprises the following steps: the hydrotalcite-plant cellulose composite pellet is prepared by an embedding method. Adding 10g of polyvinyl alcohol into 90ml of water, stirring in a water bath at 90 ℃ for 1.5h to completely dissolve the polyvinyl alcohol; adjusting the temperature to 80 ℃, adding 100ml of sodium alginate solution with the mass fraction of 0.3% into the polyvinyl alcohol solution, stirring for 1.5h to completely dissolve the sodium alginate, adding 1g of cellulose powder, and putting the mixture into an ultrasonic crusher to completely break up the cellulose into the mixed solution. Adding 100ml of hydrotalcite solution with the mass fraction of 1% into the mixed solution, continuously stirring for 2 hours until the mixed solution is viscous, and carrying out a liquid drop method by using a 20ml syringe to mix the mixed solution according to the volume ratio of 3: 4, dripping (40 drops/min) into a cross-linking agent aqueous solution (wherein the mass concentration of boric acid is 3 percent, and the mass concentration of calcium chloride is 4 percent) prepared from boric acid and calcium chloride, calcifying for 4 hours to form hydrotalcite-plant cellulose composite balls, washing for 3 times by pure water, storing in ultrapure water for subsequent use.
The sectional view and the physical view of the hydrotalcite-plant cellulose composite pellet (average diameter about 4mm) obtained in this example are shown in fig. 2 and 3, respectively.
Example 3 adsorption application of hydrotalcite-plant cellulose composite pellets to Nano-plastics
Adsorption: 3 parts (200 parts each) of the hydrotalcite-plant cellulose composite bead adsorbent prepared in example 1 was weighed and added to 50ml of water containing the nano-plastic, and the mixture was subjected to constant temperature oscillation at 25 ℃ for 24 hours in a constant temperature oscillator to measure the concentration of the nano-plastic (polystyrene as a main component, having a particle size of about 100 to 200nm) in the water. The initial concentration of the prepared nano plastic in water is 25mg/L, the initial concentration is reduced to 8mg/L after 24 hours, and the average adsorption rate is 68%.
Example 4 adsorption application of hydrotalcite-plant cellulose composite pellets to Nano-plastics
Adsorption: 3 parts (200 parts each) of the hydrotalcite-plant cellulose composite bead adsorbent prepared in example 2 was weighed and added to 50ml of water containing the nano-plastic, and the mixture was subjected to constant temperature oscillation at 25 ℃ for 24 hours in a constant temperature oscillator to measure the concentration of the nano-plastic (polystyrene as a main component, having a particle size of about 100 to 200nm) in the water. The initial concentration of the prepared nano plastic in water is 25mg/L, the initial concentration is reduced to 14mg/L after 24 hours, and the average adsorption rate is 44%.
Comparative example 1 Anhydrous Talc addition
Pretreatment and cellulose extraction of pennisetum hydridum: cutting pennisetum hydridum into small sections, washing with tap water to remove dust on the surface, washing with ultrapure water twice, boiling in a pot filled with ultrapure water for 4h, oven drying, pulverizing with a pulverizer, sieving with a 100-mesh sieve, and drying in a drier to constant weight to obtain powder. Extracting cellulose by a nitric acid-ethanol method, and mixing the powder according to a mass-to-liquid ratio of 1 g: adding 25ml of the cellulose into 250ml of nitric acid ethanol solution (the volume ratio of nitric acid ethanol is 1:4), installing a condensation reflux device, heating in a water bath at 90 ℃ for 2 hours, washing the obtained cellulose powder with the nitric acid ethanol solution for 2 times, and washing with hot water until the washing liquid is neutral. And (4) draining the filtrate, and drying in an oven at 60 ℃ for 24h to obtain cellulose powder.
The preparation method of the plant cellulose pellet comprises the following steps: embedding process is used to prepare plant cellulose balls. Adding 12g of polyvinyl alcohol into 88ml of water, stirring in a water bath at 90 ℃ for 1.5h to completely dissolve the polyvinyl alcohol; adjusting the temperature to 80 ℃, adding 100ml of sodium alginate solution with the mass fraction of 0.5% into the polyvinyl alcohol solution, stirring for 1.5h to completely dissolve the sodium alginate, adding 1g of cellulose powder, and putting the mixture into an ultrasonic crusher to completely break the cellulose into the mixed solution. And continuously stirring for 2 hours until the mixed solution is viscous, and performing a liquid drop method by using a 20ml syringe to mix the mixed solution according to a volume ratio of 3: 4, dripping (40 drops/min) into a cross-linking agent aqueous solution (wherein the mass concentration of the boric acid is 3 percent, and the mass concentration of the calcium chloride is 4 percent) prepared from boric acid and calcium chloride, and calcifying for 4 hours. The mixture solution was not formed into a spherical shape, and the result is shown in FIG. 4.
Comparative example 2
Pretreatment and cellulose extraction of pennisetum hydridum: cutting pennisetum hydridum into small sections, washing with tap water to remove dust on the surface, washing with ultrapure water twice, boiling in a pot filled with ultrapure water for 4h, oven drying, pulverizing with a pulverizer, sieving with a 100-mesh sieve, and drying in a drier to constant weight to obtain powder. Extracting cellulose by a nitric acid-ethanol method, and mixing the powder according to a mass-to-liquid ratio of 1 g: adding 25ml of the cellulose into 250ml of nitric acid ethanol solution (the volume ratio of nitric acid ethanol is 1:4), installing a condensation reflux device, heating in a water bath at 90 ℃ for 2 hours, washing the obtained cellulose powder with the nitric acid ethanol solution for 2 times, and washing with hot water until the washing liquid is neutral. And (4) draining the filtrate, and drying in an oven at 60 ℃ for 24h to obtain cellulose powder.
Preparation of hydrotalcite powder: adding magnesium-aluminum type hydrotalcite (Shaoyang Tiantang auxiliary chemical Co., Ltd.) into a muffle furnace, and sintering at 500 deg.C for 4 hr to obtain water-soluble hydrotalcite powder.
The preparation method of the plant cellulose pellet comprises the following steps: the hydrotalcite-plant cellulose compound is prepared by an embedding method. Adding 3g of polyvinyl alcohol into 97ml of water, stirring in a water bath at 90 ℃ for 1.5h to completely dissolve the polyvinyl alcohol; adjusting the temperature to 80 ℃, adding 100ml of sodium alginate solution with the mass fraction of 0.05% into the polyvinyl alcohol solution, stirring for 1.5h to completely dissolve the sodium alginate, adding 0.2g of cellulose powder, and putting the mixture into an ultrasonic crusher to completely disperse the cellulose into the mixed solution. Adding 100ml of hydrotalcite solution with the mass fraction of 0.3% into the mixed solution, continuously stirring for 2 hours until the mixed solution is viscous, and carrying out a liquid drop method by using a 20ml syringe to mix the mixed solution according to the volume ratio of 3: 4 dropping (40 drops/min) into 200ml of mixed solution of a cross-linking agent prepared from boric acid and calcium chloride (wherein the mass concentration of the boric acid is 3 percent, and the mass concentration of the calcium chloride is 4 percent), and calcifying for 4 hours. The mixture solution was not formed into a spherical shape, and the result is shown in FIG. 5.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The preparation method of the hydrotalcite-plant cellulose composite pellets is characterized by comprising the following steps:
(1) adding polyvinyl alcohol and sodium alginate into water, heating and stirring for dissolving to obtain a mixed solution, wherein the mass concentration of the polyvinyl alcohol in the mixed solution is 5-15%, and the mass concentration of the sodium alginate is 0.1-0.5%;
(2) adding plant cellulose powder and hydrotalcite into the mixed solution obtained in the step (1), and uniformly mixing, wherein the mass ratio of the plant cellulose powder to the hydrotalcite to the polyvinyl alcohol is 1: (1-2): (5-14);
(3) uniformly mixing the mixed solution obtained in the step (2) according to a volume ratio of 3: (3-5) dropwise adding the mixture into a mixed aqueous solution of boric acid and calcium chloride, calcifying for 3-6h, and washing to obtain hydrotalcite-plant cellulose composite pellets;
adding the hydrotalcite obtained in the step (2) into the mixed solution in a hydrotalcite solution mode; the mass concentration of the hydrotalcite solution is 0.5-2%.
2. The method for preparing hydrotalcite-plant cellulose composite pellets according to claim 1, wherein the mass ratio of the plant cellulose powder, hydrotalcite and polyvinyl alcohol in step (2) is 1: (1-2): (10-12).
3. The method for preparing hydrotalcite-plant cellulose composite pellets according to claim 1 or 2, wherein the mass concentration of the polyvinyl alcohol in the step (1) is 5-6%; the mass concentration of the sodium alginate is 0.15-0.25%.
4. The method for preparing hydrotalcite-plant cellulose composite pellets according to claim 3, wherein the mass concentrations of boric acid and calcium chloride in the mixed aqueous solution of boric acid and calcium chloride in step (3) are 2-8% and 3-10%, respectively.
5. The method for preparing hydrotalcite-plant cellulose composite pellets according to claim 4, wherein the mass concentration of the hydrotalcite solution is 1-2%; the mass concentration of the boric acid and the calcium chloride in the mixed aqueous solution of the boric acid and the calcium chloride is 3-5%.
6. The method for preparing hydrotalcite-plant cellulose composite pellets according to claim 3, wherein the hydrotalcite of step (2) is magnesium-aluminum type hydrotalcite; the hydrotalcite is calcined before use, the calcining temperature is 500 ℃, and the calcining time is 4 hours.
7. The method for preparing hydrotalcite-plant cellulose composite pellets according to claim 3, wherein the dropping conditions in step (3) are 30-40 drops/min and 0.02-1 ml/drop.
8. The method for preparing hydrotalcite-plant cellulose composite pellets according to claim 1 or 2, wherein the mixed solution of step (1) is prepared by the following specific method: firstly, adding polyvinyl alcohol into water, stirring for 1.5h at 90 ℃ to obtain a polyvinyl alcohol solution, then cooling to be less than or equal to 80 ℃, adding a sodium alginate solution, and stirring for 1.5 h;
the mass concentration of the polyvinyl alcohol solution is 10-12%; the mass concentration of the sodium alginate solution is 0.2-0.5%;
adding plant cellulose powder and hydrotalcite into the mixed solution obtained in the step (1) in the step (2), wherein the specific method comprises the following steps: uniformly dispersing plant cellulose powder in the mixed solution obtained in the step (1), and then adding hydrotalcite;
the plant cellulose powder in the step (2) is pennisetum hydridum cellulose powder;
the preparation method of the pennisetum hydridum cellulose powder comprises the following steps: cutting and cleaning pennisetum hydridum, boiling in boiling water, drying, pulverizing, sieving, and drying to constant weight to obtain powder; mixing the powder according to the weight ratio of 1 g: adding 25ml of the mixture into a nitric acid ethanol solution, heating at 90 ℃ until the powder turns white, and then washing and drying to obtain pennisetum hydridum cellulose powder;
and (4) the dripping method in the step (3) is a liquid dripping method.
9. A hydrotalcite-plant cellulose composite pellet obtainable by the process according to any one of claims 1 to 8.
10. The use of the hydrotalcite-plant cellulose composite beads according to claim 9 for the treatment of plastics of nanometric size in water.
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| CN101348782A (en) * | 2008-08-30 | 2009-01-21 | 兰州大学 | Macroreticular polyvinyl alcohol bead carrier and preparation thereof |
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