CN108704624B - Preparation method of photocatalytic active gas adsorbent - Google Patents
Preparation method of photocatalytic active gas adsorbent Download PDFInfo
- Publication number
- CN108704624B CN108704624B CN201810463270.4A CN201810463270A CN108704624B CN 108704624 B CN108704624 B CN 108704624B CN 201810463270 A CN201810463270 A CN 201810463270A CN 108704624 B CN108704624 B CN 108704624B
- Authority
- CN
- China
- Prior art keywords
- solution
- preparation
- gas adsorbent
- mass fraction
- beaker
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/80—Type of catalytic reaction
- B01D2255/802—Photocatalytic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/704—Solvents not covered by groups B01D2257/702 - B01D2257/7027
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/06—Polluted air
Abstract
The invention discloses a preparation method of a gas adsorbent with photocatalytic activity, belonging to the technical field of preparation of adsorption materials. The invention uses the carbonized matrix of the nano-cellulose as the adsorbing material of the indoor volatile organic pollutants, and in the process of mixing the carbonized matrix with the nano-titanium dioxide, the carbonized matrix and the titanium dioxide generate a synergistic effect and a photosensitive effect among molecules, the nano-titanium dioxide can form a film in pores of the carbon aerogel, the carbon aerogel can quickly enrich the volatile organic pollutants with low concentration, and the method is favorable for increasing the enrichment area of the carbon aerogel on the organic pollutants under the condition of low concentration, thereby accelerating the catalytic reaction, so that the titanium dioxide shows stronger catalytic activity under visible light, the coordination effect generated among the titanium dioxide, the carbon aerogel and chitosan molecules improves the photocatalytic activity of the film, the titanium dioxide is more sensitive to the volatile organic gases, the catalytic degradation concentration of the organic pollutants can be reduced, and the application prospect is wide.
Description
Technical Field
The invention discloses a preparation method of a gas adsorbent with photocatalytic activity, belonging to the technical field of preparation of adsorption materials.
Background
The adsorbent is also called absorbent. The substance can make active ingredient adhere to the surface of the particle, and make the liquid trace compound additive change into solid compound, which is beneficial to uniform mixing. Is a solid substance that can effectively adsorb certain components from a gas or liquid. Has large specific surface, proper pore structure and surface structure; strong adsorption capacity to adsorbates; generally do not chemically react with the adsorbate and the media; the manufacturing is convenient and the regeneration is easy; has excellent adsorbability and mechanical property.
The adsorbents commonly used include various activated carbon adsorbents made of carbonaceous materials and metal and non-metal oxide adsorbents (such as silica gel, alumina, molecular sieves, natural clays, etc.). The most representative adsorbent is activated carbon, which has quite good adsorption performance but higher cost, and has been used for adsorbing toluene in water bodies in the event of Songhuajiang. And secondly molecular sieves, silica gel, activated aluminum, polymeric adsorbents, biological adsorbents, and the like.
Decoration pollution is known as indoor "invisible killer" in which harmful substances are more harmful to women, children and the elderly. In a non-industrial indoor environment, 50 to 300 kinds of volatile organic compounds can be seen. The five harmful substances in the newly-decorated house far exceed the standard and seriously harm the life health of people. In addition, various occupational diseases of China increase year by year, and the number of the occupational diseases generated by long-term exposure to chemical products occupies a large proportion. Some electronic production workshops often use chemical solvents, and the chemical solvents are volatilized into air to cause environmental pollution. With the development of world economy and the concern of various countries on industrial safety production, people continuously deepen the understanding of the harmfulness of poisonous and harmful gases, around the purification treatment of the poisonous and harmful gases, extensive researchers at home and abroad develop the spirit of coursing exploration, and continuously search for a reasonable and efficient solution, and a series of measures for purifying and treating the poisonous and harmful gases are used for emergency treatment and daily industrial production waste gas purification. Adsorbents commonly used in the industry include: activated carbon, activated alumina, silica gel, synthetic zeolite molecular sieves, organic resin adsorbents, and the like, and among them, activated carbon including granular activated carbon and activated carbon fibers is widely used because of its low cost and ready availability. However, the above adsorbents have the disadvantages of easy saturation of adsorption and easy dust emission to cause secondary pollution. Therefore, the invention of the photocatalytic active gas adsorbent has positive significance in the technical field of preparation of adsorption materials.
Disclosure of Invention
The invention mainly solves the technical problem that 50-300 volatile organic compounds can be seen in the current non-industrial indoor environment, the content of volatile organic compounds in newly-decorated houses is far beyond the standard, but the current adsorbent cannot effectively adsorb indoor toxic substances and decompose the indoor toxic substances into non-toxic micromolecular inorganic gas and water, and provides a preparation method of a photocatalytic active gas adsorbent.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a photocatalytic active gas adsorbent is characterized by comprising the following specific preparation steps:
(1) putting 200-300 g of poplar into a grinder, grinding for 1-2 h, sieving by using a standard sieve to obtain wood powder, weighing 100-150 g of wood powder, putting into a Soxhlet extractor, mixing phenethyl alcohol and water at normal temperature to obtain a phenethyl alcohol solution, pouring 300-400 mL of the phenethyl alcohol solution into the Soxhlet extractor, extracting, and removing an extract to obtain crude wood fiber powder;
(2) putting the crude wood fiber powder into a beaker, adding 50-60 mL of sodium chlorite solution into the beaker to obtain a mixed solution, adjusting the pH of the mixed solution by using a glacial acetic acid solution, carrying out heat preservation treatment, repeating the operation for 3-5 times, and removing lignin to obtain holocellulose;
(3) soaking holocellulose in 120-150 mL of sodium hydroxide solution at a certain temperature, preserving heat, soaking, filtering to remove filtrate to obtain purified cellulose, preparing the purified cellulose into aqueous suspension, and placing the aqueous suspension in an ultrasonic plant cell crusher for ultrasonic treatment to obtain the wood nanocellulose;
(4) adding 50-60 mL of absolute ethyl alcohol into a beaker filled with 6-8 mL of tetraethoxysilane, stirring for 10-15 min, adding 3-4 mL of water into the beaker, stirring for 10-12 min, adding hydrochloric acid into the beaker to adjust the pH value of the solution in the beaker, and standing to obtain silicon dioxide sol;
(5) adding 40-50 mL of absolute ethyl alcohol and 2-3 g of wood nano-cellulose into an ultrasonic disperser, performing ultrasonic dispersion to obtain a cellulose suspension, placing the cellulose suspension into a conical flask with a stirrer, adding 18-20 mL of tetrabutyl titanate into the conical flask by using a dropping funnel, starting the stirrer, and stirring at a rotating speed of 200-300 r/min for 10-15 min to obtain a mixed solution;
(6) adding 4-5 mL of acetic acid solution and 20-30 mL of silica sol into the mixed solution, stirring for 1-2 h to obtain nano-cellulose/titanium dioxide sol, standing and aging to obtain dry sol, drying the dry sol in a drying oven to obtain gel blocks, grinding the gel blocks in a mortar for 30-35 min, and sieving to obtain gel powder;
(7) soaking 100-120 g of clean and dry shrimp shells in 200-230 mL of dilute hydrochloric acid to obtain an acid leaching solution, adding 80-90 g of gel powder, 40-50 mL of sodium hypochlorite solution and 70-80 mL of sodium hydroxide solution into the acid leaching solution, heating, performing heat preservation reaction, drying in a supercritical drying system to obtain aerogel, putting the aerogel into a carbonization furnace, and carbonizing in an argon atmosphere to obtain the photocatalytic activity gas adsorbent.
The screened size in the step (1) is 200 meshes, the volume ratio of the phenethyl alcohol to the water is 2: 1 at normal temperature, the extraction temperature is 80-90 ℃, and the extraction time is 5-10 h.
The mass fraction of the sodium chlorite solution in the step (2) is 20%, the mass fraction of the glacial acetic acid solution is 98%, the pH of the mixed solution is adjusted to be 4-5, the heat preservation treatment temperature is 75-80 ℃, and the heat preservation treatment time is 5-7 h. The mass fraction of the sodium hydroxide solution in the step (3) is 20%, the soaking temperature is 90-100 ℃, the heat preservation soaking time is 2-3 h, the mass fraction of the aqueous suspension is 10-20%, the ultrasonic power is 1200-1500W, the ultrasonic treatment time is 30-45 min, and the ultrasonic frequency is 30-35 kHz.
The mass fraction of the hydrochloric acid in the step (4) is 15%, the pH value of the solution in the beaker is adjusted to be 1.8-2.2, and the standing time is 3-4 h.
And (5) controlling the ultrasonic power to be 150-200W, controlling the ultrasonic dispersion time to be 4-6 min, and controlling the dropping rate of a dropping funnel to be 2-3 mL/min.
The mass fraction of the acetic acid solution in the step (6) is 20%, the standing and aging time is 2-3 days, the set temperature of an oven is 60-70 ℃, the drying time is 10-12 hours, and the screened specification is 200 meshes.
The mass fraction of the dilute hydrochloric acid in the step (7) is 5%, the soaking time is 2-3 h, the mass fraction of the sodium hypochlorite solution is 2%, the mass fraction of the sodium hydroxide solution is 40%, the temperature after heating is 50-55 ℃, the heat preservation reaction time is 40-50 min, the drying temperature is 70-80 ℃, the drying time is 20-24 h, the carbonization temperature is 300-350 ℃, and the carbonization time is 20-25 min.
The invention has the beneficial effects that:
(1) the invention takes poplar as raw material, obtains wood powder after crushing and sieving, places the wood powder in a Soxhlet extractor, extracts the wood powder by taking phenylethanol solution as solvent, obtains crude wood fiber powder, treats the crude wood fiber powder by sodium chlorite solution and glacial acetic acid solution, removes lignin under heating condition, obtains holocellulose, soaks the holocellulose by sodium hydroxide solution at a constant temperature, obtains purified cellulose by filtering and separating, prepares the purified cellulose into aqueous suspension, carries out ultrasonic treatment to obtain wood nano-cellulose, mixes ethyl orthosilicate and absolute ethyl alcohol, adds dilute hydrochloric acid to acidify and hydrolyze to obtain silicon dioxide sol, mixes the absolute ethyl alcohol and the nano-cellulose, obtains nano-cellulose suspension by ultrasonic dispersion, adds the nano-cellulose suspension into ethyl titanate, stirs and mixes to obtain mixed solution, adds acetic acid and the silicon dioxide sol into the mixed solution, stirring to obtain nano-cellulose/titanium dioxide sol, standing, ageing, drying and grinding to obtain titanium dioxide gel powder, taking waste shrimp shells as raw materials, carrying out acid leaching, doping gel powder, carrying out acetylation by using alkali liquor, drying to obtain aerogel, and carrying out carbonization treatment on the aerogel to obtain a gas adsorbent with photocatalytic activity. Thereby effectively inhibiting the recombination of photo-generated electrons and holes and improving the photocatalytic efficiency;
(2) the nanometer titanium dioxide can form a film in the pores of the carbon aerogel, the carbon aerogel can quickly enrich low-concentration volatile organic pollutants, degrade the concentration of the organic pollutants on the surface of the nanometer titanium dioxide film and improve the indoor photocatalytic oxidation efficiency, the acid leaching solution of shrimp shells is subjected to alkalization and deacetylation to obtain chitosan, the titanium dioxide film is formed by taking chitosan as a carrier, and the chitosan plays a role in a cross-linking agent to disperse the composite film material in a matrix of the chitosan, so that the composite material catalytic film layer is favorable for forming a regular structure, the film structure in the pores of the carbon aerogel is more regular, the enrichment area of the carbon aerogel on the organic pollutants under the low-concentration condition is favorably increased, the catalytic reaction is accelerated, in addition, the forbidden energy gap of the titanium dioxide becomes narrow after the carbon aerogel is doped in the composite film material to generate red shift, the nano titanium dioxide film can absorb light with longer wavelength, so that the titanium dioxide shows stronger catalytic activity under visible light, the chitosan is used as a cross-linking agent to be doped into the composite film material, the specific surface area of the film is reduced, but the chitosan has positive influence on the photocatalytic activity of the catalyst, the coordination effect generated among the titanium dioxide, the carbon aerogel and the chitosan molecules improves the photocatalytic activity of the film, the titanium dioxide is more sensitive to organic gas volatile matters, the catalytic degradation concentration of organic pollutants can be reduced, and the application prospect is wide.
Detailed Description
Putting 200-300 g of poplar into a grinder, grinding for 1-2 h, sieving with a 200-mesh standard sieve to obtain wood powder, weighing 100-150 g of wood powder, putting into a Soxhlet extractor, mixing phenethyl alcohol and water at normal temperature according to a volume ratio of 2: 1 to obtain a phenethyl alcohol solution, pouring 300-400 mL of the phenethyl alcohol solution into the Soxhlet extractor, extracting at 80-90 ℃ for 5-10 h, and removing the extract to obtain crude wood fiber powder; putting the crude wood fiber powder into a beaker, adding 50-60 mL of a 20% sodium chlorite solution into the beaker to obtain a mixed solution, adjusting the pH of the mixed solution to 4-5 by using a 98% glacial acetic acid solution, carrying out heat preservation treatment for 5-7 h at the temperature of 75-80 ℃, repeating the operation for 3-5 times, and removing lignin to obtain the holocellulose; soaking holocellulose in 120-150 mL of 20% sodium hydroxide solution at 90-100 ℃, preserving heat, soaking for 2-3 h, filtering to remove filtrate to obtain purified cellulose, preparing the purified cellulose into 10-20% aqueous suspension, placing the aqueous suspension in an ultrasonic plant cell crusher, performing ultrasonic treatment for 30-45 min at 1200-1500W, and controlling the ultrasonic frequency to be 30-35 kHz to obtain the wood nanocellulose; adding 50-60 mL of absolute ethyl alcohol into a beaker containing 6-8 mL of tetraethoxysilane, stirring for 10-15 min, adding 3-4 mL of water into the beaker, stirring for 10-12 min, adding 15% by mass of hydrochloric acid into the beaker to adjust the pH of the solution in the beaker to 1.8-2.2, and standing for 3-4 h to obtain silica sol; adding 40-50 mL of anhydrous ethanol and 2-3 g of wood nano-cellulose into an ultrasonic disperser, controlling the ultrasonic power to be 150-200W, ultrasonically dispersing for 4-6 min to obtain a cellulose suspension, placing the cellulose suspension into a conical flask with a stirrer, adding 18-20 mL of tetrabutyl titanate into the conical flask at a dropping rate of 2-3 mL/min by using a dropping funnel, starting the stirrer at the same time, and stirring for 10-15 min at a rotating speed of 200-300 r/min to obtain a mixed solution; adding 4-5 mL of 20% mass acetic acid solution and 20-30 mL of silica sol into the mixed solution, stirring for 1-2 h to obtain nano-cellulose/titanium dioxide sol, standing and aging for 2-3 days to obtain dry sol, placing the dry sol in an oven with a set temperature of 60-70 ℃, drying for 10-12 h to obtain gel blocks, placing the gel blocks in a mortar for grinding for 30-35 min, and sieving with a 200-mesh sieve to obtain gel powder; soaking 100-120 g of clean and dry shrimp shells in 200-230 mL of dilute hydrochloric acid with the mass fraction of 5% for 2-3 hours to obtain an acid leaching solution, adding 80-90 g of gel powder, 40-50 mL of sodium hypochlorite solution with the mass fraction of 2% and 70-80 mL of sodium hydroxide solution with the mass fraction of 40% into the acid leaching solution, heating to 50-55 ℃, performing heat preservation reaction for 40-50 minutes, placing in a supercritical drying system, drying at 70-80 ℃ for 20-24 hours to obtain aerogel, placing the aerogel in a carbonization furnace, carbonizing in an argon atmosphere, controlling the carbonization temperature to be 300-350 ℃, and carbonizing for 20-25 minutes to obtain the photocatalytic activity gas adsorbent.
Example 1
Putting 200g of poplar into a pulverizer, pulverizing for 1h, sieving with a 200-mesh standard sieve to obtain wood powder, weighing 100g of wood powder, putting into a Soxhlet extractor, mixing phenethyl alcohol and water at normal temperature according to the volume ratio of 2: 1 to obtain a phenethyl alcohol solution, pouring 300mL of the phenethyl alcohol solution into the Soxhlet extractor, extracting for 5h at 80 ℃, and removing the extract to obtain crude wood fiber powder; putting the crude wood fiber powder into a beaker, adding 50mL of 20% sodium chlorite solution into the beaker to obtain a mixed solution, adjusting the pH of the mixed solution to 4 by using 98% glacial acetic acid solution, carrying out heat preservation treatment for 5h at 75 ℃, repeating the operation for 3 times, and removing lignin to obtain holocellulose; soaking holocellulose in 120mL of 20% sodium hydroxide solution at 90 ℃, preserving heat and soaking for 2h, filtering to remove filtrate to obtain purified cellulose, preparing the purified cellulose into 10% aqueous suspension, placing the aqueous suspension in an ultrasonic plant cell crusher, performing ultrasonic treatment for 30min at 1200W power, and controlling the ultrasonic frequency to be 30kHz to obtain the wood nanocellulose; adding 50mL of absolute ethyl alcohol into a beaker filled with 6mL of tetraethoxysilane, stirring for 10min, adding 3mL of water into the beaker, stirring for 10min, adding 15 mass percent hydrochloric acid into the beaker to adjust the pH of the solution in the beaker to 1.8, and standing for 3h to obtain silicon dioxide sol; adding 40mL of absolute ethyl alcohol and 2g of wood nano-cellulose into an ultrasonic disperser, controlling the ultrasonic power to be 150W, ultrasonically dispersing for 4min to obtain a cellulose suspension, placing the cellulose suspension into a conical flask with a stirrer, adding 18mL of tetrabutyl titanate into the conical flask at the dropping rate of 2mL/min by using a dropping funnel, starting the stirrer at the same time, and stirring for 10min at the rotating speed of 200r/min to obtain a mixed solution; adding 4mL of 20 mass percent acetic acid solution and 20mL of silica sol into the mixed solution, stirring for 1h to obtain nano-cellulose/titanium dioxide sol, standing and aging for 2 days to obtain dry sol, placing the dry sol in a drying oven with the set temperature of 60 ℃, drying for 10h to obtain gel blocks, placing the gel blocks into a mortar for grinding for 30min, and sieving by a 200-mesh sieve to obtain gel powder; soaking 100g of clean and dry shrimp shells in 200mL of dilute hydrochloric acid with the mass fraction of 5% for 2h to obtain an acid leaching solution, adding 80g of gel powder, 40mL of sodium hypochlorite solution with the mass fraction of 2% and 70mL of sodium hydroxide solution with the mass fraction of 40% into the acid leaching solution, heating to 50 ℃, carrying out heat preservation reaction for 40min, placing in a supercritical drying system, drying at 70 ℃ for 20h to obtain aerogel, placing the aerogel in a carbonization furnace, carbonizing in argon atmosphere, controlling the carbonization temperature at 300 ℃, and carbonizing for 20min to obtain the photocatalytic active gas adsorbent.
Example 2
Putting 250g of poplar into a grinder, grinding for 1.5h, sieving with a 200-mesh standard sieve to obtain wood powder, weighing 120g of wood powder, putting into a Soxhlet extractor, mixing phenethyl alcohol and water at normal temperature according to the volume ratio of 2: 1 to obtain a phenethyl alcohol solution, pouring 350mL of the phenethyl alcohol solution into the Soxhlet extractor, extracting for 7h at 85 ℃, and removing the extract to obtain crude wood fiber powder; putting the crude wood fiber powder into a beaker, adding 55mL of a 20% sodium chlorite solution into the beaker to obtain a mixed solution, adjusting the pH of the mixed solution to 4 by using a 98% glacial acetic acid solution, carrying out heat preservation treatment at 77 ℃ for 6h, repeating the operation for 4 times, and removing lignin to obtain holocellulose; soaking holocellulose in 135mL of 20% sodium hydroxide solution at 95 ℃, preserving heat and soaking for 2.5h, filtering to remove filtrate to obtain purified cellulose, preparing the purified cellulose into 15% aqueous suspension, placing the aqueous suspension in an ultrasonic plant cell crusher, performing ultrasonic treatment for 40min at 1350W power, and controlling the ultrasonic frequency to be 32kHz to obtain the wood nanocellulose; adding 55mL of absolute ethyl alcohol into a beaker filled with 7mL of tetraethoxysilane, stirring for 12min, adding 3mL of water into the beaker, stirring for 11min, adding 15 mass percent hydrochloric acid into the beaker to regulate the pH of the solution in the beaker to 2.0, and standing for 3.5h to obtain silicon dioxide sol; adding 45mL of absolute ethyl alcohol and 2g of wood nano-cellulose into an ultrasonic disperser, controlling the ultrasonic power to be 170W, ultrasonically dispersing for 5min to obtain a cellulose suspension, placing the cellulose suspension into a conical flask with a stirrer, adding 19mL of tetrabutyl titanate into the conical flask at the dropping rate of 2mL/min by using a dropping funnel, starting the stirrer at the same time, and stirring for 12min at the rotating speed of 250r/min to obtain a mixed solution; adding 4mL of 20 mass percent acetic acid solution and 25mL of silica sol into the mixed solution, stirring for 1.5h to obtain nano-cellulose/titanium dioxide sol, standing and aging for 2 days to obtain dry sol, placing the dry sol in a baking oven with the set temperature of 65 ℃, drying for 11h to obtain gel blocks, placing the gel blocks into a mortar for grinding for 32min, and sieving by a 200-mesh sieve to obtain gel powder; soaking 110g of clean and dry shrimp shells in 215mL of dilute hydrochloric acid with the mass fraction of 5% for 2.5h to obtain an acid leaching solution, adding 85g of gel powder, 45mL of sodium hypochlorite solution with the mass fraction of 2% and 75mL of sodium hydroxide solution with the mass fraction of 40% into the acid leaching solution, heating to 52 ℃, carrying out heat preservation reaction for 45min, placing in a supercritical drying system, drying at 75 ℃ for 22h to obtain aerogel, placing the aerogel in a carbonization furnace, carbonizing in argon atmosphere, controlling the carbonization temperature to 320 ℃, and carbonizing for 22min to obtain the photocatalytic activity gas adsorbent.
Example 3
Putting 300g of poplar into a pulverizer, pulverizing for 2h, sieving with a 200-mesh standard sieve to obtain wood powder, weighing 150g of wood powder, putting into a Soxhlet extractor, mixing phenethyl alcohol and water at normal temperature according to a volume ratio of 2: 1 to obtain a phenethyl alcohol solution, pouring 400mL of the phenethyl alcohol solution into the Soxhlet extractor, extracting at 90 ℃ for 10h, and removing an extract to obtain crude wood fiber powder; putting the crude wood fiber powder into a beaker, adding 60mL of 20% sodium chlorite solution into the beaker to obtain a mixed solution, adjusting the pH of the mixed solution to 5 by using 98% glacial acetic acid solution, carrying out heat preservation treatment for 7h at the temperature of 80 ℃, repeating the operation for 5 times, and removing lignin to obtain holocellulose; soaking holocellulose in 150mL of 20% sodium hydroxide solution at 100 ℃, preserving heat and soaking for 3h, filtering to remove filtrate to obtain purified cellulose, preparing the purified cellulose into 20% aqueous suspension, placing the aqueous suspension in an ultrasonic plant cell crusher, performing ultrasonic treatment for 45min at 1500W power, and controlling the ultrasonic frequency to be 35kHz to obtain the wood nanocellulose; adding 60mL of absolute ethyl alcohol into a beaker filled with 8mL of tetraethoxysilane, stirring for 15min, adding 4mL of water into the beaker, stirring for 12min, adding 15 mass percent hydrochloric acid into the beaker to regulate the pH of the solution in the beaker to 2.2, and standing for 4h to obtain silicon dioxide sol; adding 50mL of absolute ethyl alcohol and 3g of wood nano-cellulose into an ultrasonic disperser, controlling the ultrasonic power to be 200W, ultrasonically dispersing for 6min to obtain a cellulose suspension, placing the cellulose suspension into a conical flask with a stirrer, adding 20mL of tetrabutyl titanate into the conical flask at the dropping rate of 3mL/min by using a dropping funnel, starting the stirrer at the same time, and stirring for 15min at the rotating speed of 300r/min to obtain a mixed solution; adding 5mL of 20 mass percent acetic acid solution and 30mL of silica sol into the mixed solution, stirring for 2h to obtain nano-cellulose/titanium dioxide sol, standing and aging for 3 days to obtain dry sol, placing the dry sol in a baking oven with the set temperature of 70 ℃, drying for 12h to obtain gel blocks, placing the gel blocks into a mortar for grinding for 35min, and sieving by a 200-mesh sieve to obtain gel powder; soaking 120g of clean and dry shrimp shells in 230mL of dilute hydrochloric acid with the mass fraction of 5% for 3h to obtain an acid leaching solution, adding 90g of gel powder, 50mL of sodium hypochlorite solution with the mass fraction of 2% and 80mL of sodium hydroxide solution with the mass fraction of 40% into the acid leaching solution, heating to 55 ℃, carrying out heat preservation reaction for 50min, placing the obtained product in a supercritical drying system, drying for 24h at the temperature of 80 ℃ to obtain aerogel, placing the aerogel in a carbonization furnace, carbonizing in an argon atmosphere, controlling the carbonization temperature to be 350 ℃, and carbonizing for 25min to obtain the photocatalytic activity gas adsorbent.
Comparative example
The photocatalytically active gas adsorbent produced by Changzhou company was used as a comparative example to examine the performance of the photocatalytically active gas adsorbent produced by the present invention and the photocatalytically active gas adsorbent in the comparative example
The test method comprises the following steps:
and (3) testing the formaldehyde removal rate: taking 25g of the gas adsorbent in the examples 1-3 and the comparative example, putting the gas adsorbent into a drying bag, sealing the opening of the bag by using a clamp, and then placing the drying bag at any corner in a room, wherein 3 drying bags filled with the adsorbent are placed in each square meter, placing the drying bag for 10 hours, and measuring the formaldehyde content before 10 hours and the formaldehyde after 10 hours;
detecting the saturated adsorption quantity according to GB/T19587-;
testing the photocatalytic efficiency: the gas adsorbents in examples 1 to 3 and comparative examples were placed in a drying bag, and after the mouth of the bag was sealed with a clip, the bag was placed at any corner of the room, and the photocatalytic performance was evaluated by measuring the change in the degradation rate of formaldehyde under a fluorescent lamp.
The photocatalytic active gas adsorbent prepared by the method has the advantages of good adsorption effect on formaldehyde in indoor air, higher removal rate, no harm to human bodies and environment, high degradation rate, good photocatalytic effect and wide application prospect.
Claims (8)
1. A preparation method of a photocatalytic active gas adsorbent is characterized by comprising the following specific preparation steps:
(1) putting 200-300 g of poplar into a grinder, grinding for 1-2 h, sieving by using a standard sieve to obtain wood powder, weighing 100-150 g of wood powder, putting into a Soxhlet extractor, mixing phenethyl alcohol and water at normal temperature to obtain a phenethyl alcohol solution, pouring 300-400 mL of the phenethyl alcohol solution into the Soxhlet extractor, extracting, and removing an extract to obtain crude wood fiber powder;
(2) putting the crude wood fiber powder into a beaker, adding 50-60 mL of sodium chlorite solution into the beaker to obtain a mixed solution, adjusting the pH of the mixed solution by using a glacial acetic acid solution, carrying out heat preservation treatment, repeating the operation for 3-5 times, and removing lignin to obtain holocellulose;
(3) soaking holocellulose in 120-150 mL of sodium hydroxide solution at a certain temperature, preserving heat, soaking, filtering to remove filtrate to obtain purified cellulose, preparing the purified cellulose into aqueous suspension, and placing the aqueous suspension in an ultrasonic plant cell crusher for ultrasonic treatment to obtain the wood nanocellulose;
(4) adding 50-60 mL of absolute ethyl alcohol into a beaker filled with 6-8 mL of tetraethoxysilane, stirring for 10-15 min, adding 3-4 mL of water into the beaker, stirring for 10-12 min, adding hydrochloric acid into the beaker to adjust the pH value of the solution in the beaker, and standing to obtain silicon dioxide sol;
(5) adding 40-50 mL of absolute ethyl alcohol and 2-3 g of wood nano-cellulose into an ultrasonic disperser, performing ultrasonic dispersion to obtain a cellulose suspension, placing the cellulose suspension into a conical flask with a stirrer, adding 18-20 mL of tetrabutyl titanate into the conical flask by using a dropping funnel, starting the stirrer, and stirring at a rotating speed of 200-300 r/min for 10-15 min to obtain a mixed solution;
(6) adding 4-5 mL of acetic acid solution and 20-30 mL of silica sol into the mixed solution, stirring for 1-2 h to obtain nano-cellulose/titanium dioxide sol, standing and aging to obtain dry sol, drying the dry sol in a drying oven to obtain gel blocks, grinding the gel blocks in a mortar for 30-35 min, and sieving to obtain gel powder;
(7) soaking 100-120 g of clean and dry shrimp shells in 200-230 mL of dilute hydrochloric acid to obtain an acid leaching solution, adding 80-90 g of gel powder, 40-50 mL of sodium hypochlorite solution and 70-80 mL of sodium hydroxide solution into the acid leaching solution, heating, performing heat preservation reaction, drying in a supercritical drying system to obtain aerogel, putting the aerogel into a carbonization furnace, and carbonizing in an argon atmosphere to obtain the photocatalytic activity gas adsorbent.
2. A process for the preparation of a photocatalytically active gas adsorbent according to claim 1, characterized in that: the screened size in the step (1) is 200 meshes, the volume ratio of the phenethyl alcohol to the water is 2: 1 at normal temperature, the extraction temperature is 80-90 ℃, and the extraction time is 5-10 h.
3. A process for the preparation of a photocatalytically active gas adsorbent according to claim 1, characterized in that: the mass fraction of the sodium chlorite solution in the step (2) is 20%, the mass fraction of the glacial acetic acid solution is 98%, the pH of the mixed solution is adjusted to be 4-5, the heat preservation treatment temperature is 75-80 ℃, and the heat preservation treatment time is 5-7 h.
4. A process for the preparation of a photocatalytically active gas adsorbent according to claim 1, characterized in that: the mass fraction of the sodium hydroxide solution in the step (3) is 20%, the soaking temperature is 90-100 ℃, the heat preservation soaking time is 2-3 h, the mass fraction of the aqueous suspension is 10-20%, the ultrasonic power is 1200-1500W, the ultrasonic treatment time is 30-45 min, and the ultrasonic frequency is 30-35 kHz.
5. A process for the preparation of a photocatalytically active gas adsorbent according to claim 1, characterized in that: the mass fraction of the hydrochloric acid in the step (4) is 15%, the pH value of the solution in the beaker is adjusted to be 1.8-2.2, and the standing time is 3-4 h.
6. A process for the preparation of a photocatalytically active gas adsorbent according to claim 1, characterized in that: and (5) controlling the ultrasonic power to be 150-200W, controlling the ultrasonic dispersion time to be 4-6 min, and controlling the dropping rate of a dropping funnel to be 2-3 mL/min.
7. A process for the preparation of a photocatalytically active gas adsorbent according to claim 1, characterized in that: the mass fraction of the acetic acid solution in the step (6) is 20%, the standing and aging time is 2-3 days, the set temperature of an oven is 60-70 ℃, the drying time is 10-12 hours, and the screened specification is 200 meshes.
8. A process for the preparation of a photocatalytically active gas adsorbent according to claim 1, characterized in that: the mass fraction of the dilute hydrochloric acid in the step (7) is 5%, the soaking time is 2-3 h, the mass fraction of the sodium hypochlorite solution is 2%, the mass fraction of the sodium hydroxide solution is 40%, the temperature after heating is 50-55 ℃, the heat preservation reaction time is 40-50 min, the drying temperature is 70-80 ℃, the drying time is 20-24 h, the carbonization temperature is 300-350 ℃, and the carbonization time is 20-25 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810463270.4A CN108704624B (en) | 2018-05-15 | 2018-05-15 | Preparation method of photocatalytic active gas adsorbent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810463270.4A CN108704624B (en) | 2018-05-15 | 2018-05-15 | Preparation method of photocatalytic active gas adsorbent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108704624A CN108704624A (en) | 2018-10-26 |
| CN108704624B true CN108704624B (en) | 2021-07-20 |
Family
ID=63868890
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810463270.4A Active CN108704624B (en) | 2018-05-15 | 2018-05-15 | Preparation method of photocatalytic active gas adsorbent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108704624B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109603532A (en) * | 2019-01-10 | 2019-04-12 | 上海滢晶环保科技有限公司 | A kind of composite spraying agent and preparation method thereof of decomposing formaldehyde benzene homologues TVOC |
| CN109987861A (en) * | 2019-04-30 | 2019-07-09 | 江戴玉 | A kind of preparation method of aeroge glass |
| CN112808227B (en) * | 2020-12-28 | 2023-09-19 | 苏州城市学院 | Hybrid aerogel adsorbent, preparation method thereof and application thereof in wastewater treatment |
| CN112870965B (en) * | 2021-01-19 | 2021-12-21 | 杭州妙蓝环保科技有限公司 | Air purification material capable of rapidly degrading formaldehyde and preparation method thereof |
| CN113351174A (en) * | 2021-06-18 | 2021-09-07 | 东北电力大学 | Preparation method and application of HKUST-1/CNF composite membrane loaded with V/N doped nano titanium dioxide |
| CN113908652B (en) * | 2021-09-09 | 2023-02-10 | 济南市平阴县玛钢厂 | Process for reducing smoke dust emission of cupola furnace in foundry |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101690901A (en) * | 2009-03-06 | 2010-04-07 | 中国科学院等离子体物理研究所 | Photocatalysis material derived from biomass and preparation method |
| WO2014136073A1 (en) * | 2013-03-06 | 2014-09-12 | Ecole Polytechnique Federale De Lausanne (Epfl) | Titanium oxide aerogel composites |
| CN104741137A (en) * | 2013-12-31 | 2015-07-01 | 西北大学 | Preparation method of titanium dioxide and doped body of titanium dioxide |
| CN106000302A (en) * | 2016-05-28 | 2016-10-12 | 湖南细心信息科技有限公司 | Preparation method of composite carbon aerogel-baed air purifying agent |
| CN106365195A (en) * | 2016-08-26 | 2017-02-01 | 华南理工大学 | Three-dimensional porous titanium dioxide using biomass material as template and preparation method thereof |
| CN107684886A (en) * | 2017-09-29 | 2018-02-13 | 华纺股份有限公司 | One kind doping TiO2The compound carbon aerogels of cotton fiber preparation method |
-
2018
- 2018-05-15 CN CN201810463270.4A patent/CN108704624B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101690901A (en) * | 2009-03-06 | 2010-04-07 | 中国科学院等离子体物理研究所 | Photocatalysis material derived from biomass and preparation method |
| WO2014136073A1 (en) * | 2013-03-06 | 2014-09-12 | Ecole Polytechnique Federale De Lausanne (Epfl) | Titanium oxide aerogel composites |
| CN104741137A (en) * | 2013-12-31 | 2015-07-01 | 西北大学 | Preparation method of titanium dioxide and doped body of titanium dioxide |
| CN106000302A (en) * | 2016-05-28 | 2016-10-12 | 湖南细心信息科技有限公司 | Preparation method of composite carbon aerogel-baed air purifying agent |
| CN106365195A (en) * | 2016-08-26 | 2017-02-01 | 华南理工大学 | Three-dimensional porous titanium dioxide using biomass material as template and preparation method thereof |
| CN107684886A (en) * | 2017-09-29 | 2018-02-13 | 华纺股份有限公司 | One kind doping TiO2The compound carbon aerogels of cotton fiber preparation method |
Non-Patent Citations (1)
| Title |
|---|
| Fabricating 3D hierarchical porous TiO2 and SiO2 with high specific surface area by using nanofibril-interconnected cellulose aerogel as a new biotemplate;Xiaoting Zhang et al.;《Industrial Crops & Products》;20170927;第109卷;第791页第2节Experimental section部分 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108704624A (en) | 2018-10-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108704624B (en) | Preparation method of photocatalytic active gas adsorbent | |
| CN107029668B (en) | A kind of honeycomb type molecular sieve-active carbon compound adsorbent, preparation method and applications | |
| CN110813383B (en) | Wood fiber biomass loaded nano hydrated titanium dioxide composite material and preparation method and application thereof | |
| CN1293938C (en) | Methanal disintegrant and preparation thereof | |
| CN111359582A (en) | Graphene composite aerogel formaldehyde-removing material and preparation method thereof | |
| CN109894007B (en) | Environment-friendly air purification material and preparation process thereof | |
| CN106512974A (en) | Regeneration method of activated carbon | |
| CN104707588B (en) | A kind of material for air purification containing titania aerogel and preparation method thereof | |
| CN108479707A (en) | A kind of preparation method of material for air purification | |
| CN109126714B (en) | TiO 22/SiO2-banana peel biochar composite adsorption material and preparation method thereof | |
| CN105688660A (en) | Air purification material taking titanium dioxide photocatalyst as base material and preparation method thereof | |
| CN115197591A (en) | Visible light catalytic composite material and preparation method thereof | |
| CN113976166B (en) | Preparation method and application of nitrogen-doped ordered mesoporous carbon catalyst | |
| CN111729654A (en) | Preparation method and application of modified pagodatree leaf biochar | |
| CN114835477B (en) | Multifunctional water purification ceramic material | |
| CN107029674A (en) | A kind of rare earth modified medical stone and peanut shell composite adsorbing material and preparation method thereof | |
| CN114213140A (en) | Coal gangue-based ceramsite for phosphorus adsorption, preparation method thereof and water treatment equipment | |
| CN110180503A (en) | A kind of preparation method of high removal rate air filting material | |
| CN111977873B (en) | Method for using photoactivated sepiolite Si-OH for adsorption and photodegradation of water-soluble organic pollutants | |
| CN110590227A (en) | Diatom ooze capable of efficiently and durably removing formaldehyde and preparation method thereof | |
| CN116459795A (en) | Water treatment material for removing lead from wastewater and preparation method and application thereof | |
| CN108854524A (en) | A kind of preparation method of the oxidation modification support type bamboo charcoal of adsorbable degradation of formaldehyde | |
| CN110922158B (en) | Environment-friendly material for air purification and application thereof | |
| CN114392723A (en) | Carbon dioxide adsorbent, preparation method thereof, activation regeneration method and application | |
| CN106362686A (en) | Preparation method of composite material for gathering and degrading benzene series organic wastewater |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20210630 Address after: 541700 group 1, Ledong village, Chengguan village, Longsheng Town, Longsheng County, Guilin City, Guangxi Zhuang Autonomous Region Applicant after: Guangxi Guilin xigelun Technology Co.,Ltd. Address before: 213000 room 801, unit a, building 152, qinglongyuan, Tianning District, Changzhou City, Jiangsu Province Applicant before: Wang Cheng |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |