CN108704624A - A kind of preparation method of photocatalytic activity adsorbent - Google Patents

A kind of preparation method of photocatalytic activity adsorbent Download PDF

Info

Publication number
CN108704624A
CN108704624A CN201810463270.4A CN201810463270A CN108704624A CN 108704624 A CN108704624 A CN 108704624A CN 201810463270 A CN201810463270 A CN 201810463270A CN 108704624 A CN108704624 A CN 108704624A
Authority
CN
China
Prior art keywords
photocatalytic activity
added
obtains
solution
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.)
Granted
Application number
CN201810463270.4A
Other languages
Chinese (zh)
Other versions
CN108704624B (en
Inventor
王成
何伟仁
陈可
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangxi Guilin Xigelun Technology Co ltd
Original Assignee
Individual
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201810463270.4A priority Critical patent/CN108704624B/en
Publication of CN108704624A publication Critical patent/CN108704624A/en
Application granted granted Critical
Publication of CN108704624B publication Critical patent/CN108704624B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid 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
    • B01J20/28047Gels
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/02Separation 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86Catalytic processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86Catalytic processes
    • B01D53/8668Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054Solid 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
    • B01J20/28057Surface area, e.g. B.E.T specific surface area
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18Carbon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2255/00Catalysts
    • B01D2255/80Type of catalytic reaction
    • B01D2255/802Photocatalytic
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/70Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/704Solvents not covered by groups B01D2257/702 - B01D2257/7027
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/70Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/708Volatile organic compounds V.O.C.'s
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2258/00Sources of waste gases
    • B01D2258/06Polluted air

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Dispersion Chemistry (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Disinfection, Sterilisation Or Deodorisation Of Air (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses a kind of preparation methods of photocatalytic activity adsorbent, belong to technical field of adsorption material preparation.The present invention uses the charing matrix of nano-cellulose as the sorbing material of degradation of indoor air VOCs, by it and during nano-titanium dioxide mixes, synergistic effect and photosensitization will occurs in it between titania molecule, nano-titanium dioxide can form film in charcoal-aero gel hole in the present invention, charcoal-aero gel can make the volatile organic contaminant fast enriching of low concentration, be conducive to increase charcoal-aero gel under low consistency conditions to the enrichment area of organic pollution, to accelerate catalysis reaction, so that titanium dioxide shows stronger catalytic activity under visible light, titanium dioxide, the coordinating effect generated between charcoal-aero gel and chitosan molecule improves the photocatalytic activity of film, keep titanium dioxide more sensitive to organic gas volatile matter, organic pollution catalytic degradation concentration can be reduced, it has a extensive future.

Description

A kind of preparation method of photocatalytic activity adsorbent
Technical field
The invention discloses a kind of preparation methods of photocatalytic activity adsorbent, belong to sorbing material technology of preparing neck Domain.
Background technology
Adsorbent is also referred to as absorbent.This substance can make active constituent be attached to its particle surface, make the micro chemical combination of liquid Object additive becomes solid compounds, is conducive to implement uniformly to mix.It is one kind can effectively adsorb from gas or liquid The solid matter of some of which ingredient.With big specific surface, suitable pore structure and surface texture;Have to adsorbate strong Adsorption capacity;It is not chemically reacted with adsorbate and medium generally;Easily manufactured, regenerating easily;Have fabulous adsorptivity and Mechanicalness characteristic.
Common adsorbent has to be adsorbed by the various acticarbons and metal of raw material, nonmetal oxide class of carbonaceous Agent(Such as silica gel, aluminium oxide, molecular sieve, natural clay).Most representative adsorbent is activated carbon, and absorption property is suitable It is good, but cost is relatively high, once applies the toluene being used in the event of Song Hua River in adsorbed water body.Secondly there are molecular sieve, silicon Glue, activated aluminum, polymer absorbant and biological adsorption agent etc..
Finishing pollution is referred to as indoor " stealthy killer ", and harmful substance therein is to women, children and the injury of old man It is more serious.In subcommercial indoor environment, 50~300 kinds of volatile organic compounds can be seen.Newly-decorated house This interior five classes harmful substance is much exceeded, seriously endangers the life and health of people.In addition, the various occupational diseases in China increase year by year Add, and the occupational disease number that Long Term Contact chemical products generate occupies prodigious ratio.Some electronics workshops are commonly used Chemical solvent, chemical solvent, which is evaporate into air, causes environmental pollution.As the development and various countries of world economy are to industry security The concern of production, people are also constantly deepening the understanding of toxic and harmful gas harmfulness, surround the purification of toxic and harmful gas Disposition, domestic and international numerous researchers have developed the spirit for daring to exploring, and constantly look for reasonable efficient solution, a system The measure for showing malicious cleaning harmful gas processing is used in emergency disposal and the purification of daily industrial production waste gas.It is industrial common Adsorbent include:Activated carbon, activated alumina, silica gel, synthesis zeolite, organic resin adsorbent etc., wherein including Activated carbon including granular active carbon and activated carbon fibre is widely used because its is cheap and easy to get.But above-mentioned adsorbent It is easily saturated in the presence of absorption, is easy the shortcomings that airborne dust causes secondary pollution.Therefore, a kind of photocatalytic activity gas absorption is invented Agent has positive effect to technical field of adsorption material preparation.
Invention content
Present invention mainly solves the technical issues of, in current subcommercial indoor environment, 50~300 can be seen Volatile organic compounds is planted, the volatile organic content in newly-decorated house is much exceeded, however current adsorbent Noxious material and the defect of nontoxic small molecule inorganic gas and water can not be decomposed into effective adsorption chamber, provide a kind of light The preparation method of catalytic activity adsorbent.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of preparation method of photocatalytic activity adsorbent, it is characterised in that specifically preparation process is:
(1)It takes 200~300g poplars to be put into pulverizer, crushes 1~2h, cross standard screen, obtain wooden powder, weigh 100~ 150g wooden powders are placed in Soxhlet extractor, and benzyl carbinol and water are mixed to get benzyl carbinol solution at normal temperatures, then by 300~ 400mL benzyl carbinol solution pours into Soxhlet extractor, and extracting obtains thick wood fiber powder after removing extract;
(2)Thick wood fiber powder is put into beaker, 50~60mL sodium chlorite solutions are added into beaker, obtain mixed liquor, and The pH of mixed liquor is adjusted with glacial acetic acid solution, isothermal holding repeats aforesaid operations 3~5 times, removes lignin, obtains comprehensive fiber Element;
(3)With 120~150mL sodium hydroxide solutions, holocellulose, heat-insulation soaking, filtering removal are impregnated under the conditions of certain temperature Filtrate obtains purifying cellulose, and purifying cellulose is made into water slurry, is placed in ultrasonic wave plant cell pulverizer at ultrasound Wooden nano-cellulose is made in reason;
(4)50~60mL absolute ethyl alcohols are added in the beaker equipped with 6~8mL ethyl orthosilicates, 10~15min is stirred, by 3~ 4mL water is added in beaker, after stirring 10~12min, then hydrochloric acid is added into beaker and adjusts pH value of solution in beaker, stand, obtain Silicon dioxide gel;
(5)40~50mL absolute ethyl alcohols are added into ultrasonic disperse instrument and the wooden nano-celluloses of 2~3g, ultrasonic disperse obtain Cellulose suspension is placed in the conical flask with blender by cellulose suspension, is added into conical flask with dropping funel 18~20mL butyl titanates, while starting blender, stirring 10~15min with the rotating speed of 200~300r/min is mixed Liquid;
(6)4~5mL acetic acid solutions are added into mixed liquor, 20~30mL silicon dioxide gels stir 1~2h, obtain Nanowire Element/TiO 2 sol is tieed up, it is still aging, dry colloidal sol is obtained, dry colloidal sol is placed in drying in baking oven, gel piece is obtained, will coagulate Blob of viscose is put into 30~35min of grinding in mortar, and sieving obtains gel powder;
(7)It takes the shrimp shell of 100~120g clean drieds to be placed in 200~230mL dilute hydrochloric acid to impregnate, obtains pickle liquor, to acidleach 80~90g gel powders, 40~50mL liquor natrii hypochloritis and 70~80mL sodium hydroxide solutions are added in liquid, heat temperature raising is protected Temperature reaction is placed on drying in supercritical drying drying system, obtains aeroge, aeroge is put into retort, in argon gas atmosphere It is carbonized, obtains photocatalytic activity adsorbent.
Step(1)The be sieved specification is 200 mesh, and mixed volume ratio is 2 ︰ 1, extracting to benzyl carbinol at normal temperatures with water Temperature is 80~90 DEG C, and extraction times are 5~10h.
Step(2)Sodium chlorite solution's mass fraction is 20%, and glacial acetic acid solution mass fraction is 98%, is adjusted mixed The pH for closing liquid is 4~5, and isothermal holding temperature is 75~80 DEG C, and the isothermal holding time is 5~7h.Step(3)The hydroxide The mass fraction of sodium solution is 20%, and soaking temperature is 90~100 DEG C, and the heat-insulation soaking time is 2~3h, the quality of water slurry Score be 10~20%, ultrasonic power be 1200~1500W, sonication treatment time be 30~45min, supersonic frequency be 30~ 35kHz。
Step(4)The mass fraction of the hydrochloric acid is 15%, and it is 1.8~2.2 to adjust pH value of solution in beaker, time of repose For 3~4h.
Step(5)The control ultrasonic power is 150~200W, and the ultrasonic disperse time is 4~6min, dropping funel drop Rate of acceleration is 2~3mL/min.
Step(6)The mass fraction of the acetic acid solution is 20%, and the still aging time is 2~3 days, baking oven setting temperature Degree is 60~70 DEG C, and drying time is 10~12h, and be sieved specification is sieved for 200 mesh.
Step(7)The mass fraction of the dilute hydrochloric acid is 5%, and soaking time is 2~3h, the quality of liquor natrii hypochloritis Score is 2%, and the mass fraction of sodium hydroxide solution is 40%, and temperature is 50~55 DEG C after heat temperature raising, and the insulation reaction time is 40~50min, drying temperature be 70~80 DEG C, drying time be 20~for 24 hours, control carbonization temperature be 300~350 DEG C, charing Time is 20~25min.
The beneficial effects of the invention are as follows:
(1)The present invention obtains wooden powder after pulverizing and sieving, wooden powder is placed in Soxhlet extractor using poplar as raw material, Using benzyl carbinol solution as solvent extraction, thick wood fiber powder is obtained, by thick wood fiber powder with sodium chlorite solution, at glacial acetic acid solution It manages, removes lignin under heating condition, obtain holocellulose, by holocellulose sodium hydroxide solution heat-insulation soaking, filtering point From purifying cellulose is obtained, purifying cellulose is configured to water slurry, is ultrasonically treated, wooden nano-cellulose is made, it will just Silester is mixed with absolute ethyl alcohol, and dilute hydrochloric acid acidification hydrolization is added to obtain silicon dioxide gel, by absolute ethyl alcohol and nanofiber Element mixing, nano-cellulose suspension is obtained through ultrasonic disperse, and nano-cellulose suspension is added in tetraethyl titanate, and stirring is mixed Conjunction obtains mixed liquor, and acetic acid, silicon dioxide gel are added dropwise into mixed liquor, stirs to get nano-cellulose/TiO 2 sol, Titania gel powder is obtained by still aging, dry, grinding, it is solidifying by acidleach, incorporation using discarded shrimp shell as raw material Rubber powder simultaneously obtains photocatalytic activity gas absorption with being dried to obtain aeroge after lye acetylation, then by aeroge charing process Agent, the present invention uses the charing matrix of nano-cellulose as the sorbing material of degradation of indoor air VOCs, due to Nanowire The charcoal-aero gel formed after dimension element charing has high-specific surface area, has very to gas trace heavy metal element and certain organic matters Strong adsorption capacity, by it and during nano-titanium dioxide mixes, synergistic effect will occurs in it between titania molecule And photosensitization, the photocatalytic activity of nano-titanium dioxide film can be improved, receptor of the nano-cellulose as electronics is easy The light induced electron that titanium dioxide generates is received, to effectively inhibit compound, the raising photocatalysis efficiency of light induced electron and hole;
(2)Nano-titanium dioxide can form film in charcoal-aero gel hole in the present invention, and charcoal-aero gel can make low concentration Volatile organic contaminant fast enriching, the organic pollution concentration on degradation nano-titanium dioxide film surface improves to room The pickle liquor of interior photocatalytic oxidation efficiency, shrimp shell obtains chitosan, the formation of titanium deoxid film by alkalization is deacetylated Using chitosan as carrier, and chitosan serves among composite film material is dispersed in the matrix of chitosan by crosslinking agent, has It is catalyzed the structure of film layer formation rule conducive to composite material, makes in charcoal-aero gel hole that membrane structure is more regular, is conducive to increase Big charcoal-aero gel, to the enrichment area of organic pollution, reacts, in addition, charcoal-aero gel under low consistency conditions to accelerate catalysis Titanium dioxide forbidden band energy gap narrows after being doped in composite film material, generates red shift, nano-titanium dioxide film is allow to absorb The light of more long wavelength, so that titanium dioxide shows stronger catalytic activity under visible light, chitosan is mixed as crosslinking agent Enter in composite film material, although the specific surface area of film is caused to reduce, product is produced to the photocatalytic activity of catalyst The influence of pole, the coordinating effect generated between titanium dioxide, charcoal-aero gel and chitosan molecule improve the photocatalytic activity of film, Keep titanium dioxide more sensitive to organic gas volatile matter, organic pollution catalytic degradation concentration can be reduced, application prospect is wide It is wealthy.
Specific implementation mode
It takes 200~300g poplars to be put into pulverizer, crushes 1~2h, cross 200 mesh standard sieves, obtain wooden powder, weigh 100~150g wooden powders are placed in Soxhlet extractor, are that 2 ︰ 1 are mixed to get benzene by volume at normal temperatures by benzyl carbinol and water Ethanol solution, then 300~400mL benzyl carbinol solution is poured into Soxhlet extractor, 5~10h, removing are extracted at 80~90 DEG C After extract, thick wood fiber powder is obtained;Thick wood fiber powder is put into beaker, 50~60mL mass fractions are added into beaker is 20% sodium chlorite solution, obtains mixed liquor, be used in combination mass fraction be 98% glacial acetic acid solution adjust mixed liquor pH to 4~ 5,5~7h of isothermal holding under the conditions of 75~80 DEG C, repeat aforesaid operations 3~5 times, remove lignin, obtain holocellulose;With The sodium hydroxide solution that 120~150mL mass fractions are 20%, impregnates holocellulose, heat-insulation soaking 2 under the conditions of 90~100 DEG C ~3h, filtering removal filtrate obtain purifying cellulose, purifying cellulose are made into the water slurry that mass fraction is 10~20%, It is placed in ultrasonic wave plant cell pulverizer the power ultrasonic with 1200~1500W and handles 30~45min, control supersonic frequency is Wooden nano-cellulose is made in 30~35kHz;The beaker equipped with 6~8mL ethyl orthosilicates is added in 50~60mL absolute ethyl alcohols In, 10~15min is stirred, 3~4mL water is added in beaker, after stirring 10~12min, then mass fraction is added into beaker It is 1.8~2.2 for pH value of solution in 15% hydrochloric acid adjusting beaker, stands 3~4h, obtain silicon dioxide gel;To ultrasonic disperse instrument Middle addition 40~50mL absolute ethyl alcohols and the wooden nano-celluloses of 2~3g, control ultrasonic power are 150~200W, ultrasonic disperse 4 ~6min, obtains cellulose suspension, and cellulose suspension is placed in the conical flask with blender, with dropping funel with 2 18~20mL butyl titanates are added into conical flask for the drop rate of~3mL/min, while starting blender, with 200~ The rotating speed of 300r/min starts 10~15min of stirring and obtains mixed liquor;It is 20% that 4~5mL mass fractions are added into mixed liquor Acetic acid solution, 20~30mL silicon dioxide gels stir 1~2h, obtain nano-cellulose/TiO 2 sol, and still aging 2 ~3 days, dry colloidal sol is obtained, dry colloidal sol is placed in the baking oven that set temperature is 60~70 DEG C, dry 10~12h obtains gel Gel piece is put into 30~35min of grinding in mortar, crosses 200 mesh and sieve to obtain gel powder by block;Take 100~120g clean drieds Shrimp shell, which is placed in the dilute hydrochloric acid that 200~230mL mass fractions are 5%, impregnates 2~3h, obtains pickle liquor, 80 are added into pickle liquor The hydrogen-oxygen that the liquor natrii hypochloritis and 70~80mL mass fractions that~90g gel powders, 40~50mL mass fractions are 2% are 40% Change sodium solution, is heated to 50~55 DEG C, 40~50min of insulation reaction is placed in supercritical drying drying system, 70~80 Dry 20 under the conditions of DEG C~for 24 hours, aeroge is obtained, aeroge is put into retort, is carbonized in argon gas atmosphere, is controlled Carbonization temperature is 300~350 DEG C, and carbonization time is 20~25min, obtains photocatalytic activity adsorbent.
Example 1
It takes 200g poplars to be put into pulverizer, crushes 1h, cross 200 mesh standard sieves, obtain wooden powder, weigh 100g wooden powders It is placed in Soxhlet extractor, benzyl carbinol and water is mixed to get benzyl carbinol solution for 2 ︰ 1 by volume at normal temperatures, then will 300mL benzyl carbinol solution pours into Soxhlet extractor, and 5h is extracted at 80 DEG C, after removing extract, obtains thick wood fiber powder;It will Thick wood fiber powder is put into beaker, and the sodium chlorite solution that 50mL mass fractions are 20% is added into beaker, obtains mixed liquor, It is used in combination the glacial acetic acid solution that mass fraction is 98% to adjust pH to 4, isothermal holding 5h under the conditions of 75 DEG C of mixed liquor, in repetition Operation 3 times is stated, lignin is removed, obtains holocellulose;The sodium hydroxide solution for being 20% with 120mL mass fractions, in 90 DEG C of items Holocellulose, heat-insulation soaking 2h are impregnated under part, filtering removal filtrate obtains purifying cellulose, purifying cellulose is made into quality point Number is 10% water slurry, is placed in ultrasonic wave plant cell pulverizer the power ultrasonic processing 30min with 1200W, and control is super Acoustic frequency is 30kHz, and wooden nano-cellulose is made;50mL absolute ethyl alcohols are added in the beaker equipped with 6mL ethyl orthosilicates, 10min is stirred, 3mL water is added in beaker, after stirring 10min, then the hydrochloric acid that mass fraction is 15% is added into beaker and adjusts PH value of solution is 1.8 in beaker, stands 3h, obtains silicon dioxide gel;40mL absolute ethyl alcohols and 2g are added into ultrasonic disperse instrument Wooden nano-cellulose, control ultrasonic power are 150W, and ultrasonic disperse 4min obtains cellulose suspension, cellulose is suspended Liquid is placed in the conical flask with blender, and 18mL titaniums are added into conical flask with the drop rate of 2mL/min with dropping funel Sour four butyl esters, while starting blender, starting stirring 10min with the rotating speed of 200r/min obtains mixed liquor;Add into mixed liquor Enter the acetic acid solution that 4mL mass fractions are 20%, 20mL silicon dioxide gels stir 1h, obtain nano-cellulose/titanium dioxide Colloidal sol still aging 2 days, obtains dry colloidal sol, dry colloidal sol is placed in the baking oven that set temperature is 60 DEG C, and dry 10h is coagulated Gel piece is put into mortar and grinds 30min by blob of viscose, crosses 200 mesh and sieves to obtain gel powder;The shrimp shell of 100g clean drieds is taken to be placed in 2h is impregnated in the dilute hydrochloric acid that 200mL mass fractions are 5%, obtains pickle liquor, 80g gel powders, 40mL mass are added into pickle liquor The sodium hydroxide solution that the liquor natrii hypochloritis and 70mL mass fractions that score is 2% are 40% is heated to 50 DEG C, heat preservation Reaction 40min is placed in supercritical drying drying system, and dry 20h, obtains aeroge, aeroge is put into charcoal under the conditions of 70 DEG C Change in stove, carbonized in argon gas atmosphere, control carbonization temperature is 300 DEG C, carbonization time 20min, obtains photocatalysis work Property adsorbent.
Example 2
It takes 250g poplars to be put into pulverizer, crushes 1.5h, cross 200 mesh standard sieves, obtain wooden powder, weigh 120g wood powders End is placed in Soxhlet extractor, benzyl carbinol and water is mixed to get benzyl carbinol solution for 2 ︰ 1 by volume at normal temperatures, then will 350mL benzyl carbinol solution pours into Soxhlet extractor, and 7h is extracted at 85 DEG C, after removing extract, obtains thick wood fiber powder;It will Thick wood fiber powder is put into beaker, and the sodium chlorite solution that 55mL mass fractions are 20% is added into beaker, obtains mixed liquor, It is used in combination the glacial acetic acid solution that mass fraction is 98% to adjust pH to 4, isothermal holding 6h under the conditions of 77 DEG C of mixed liquor, in repetition Operation 4 times is stated, lignin is removed, obtains holocellulose;The sodium hydroxide solution for being 20% with 135mL mass fractions, in 95 DEG C of items Holocellulose, heat-insulation soaking 2.5h are impregnated under part, filtering removal filtrate obtains purifying cellulose, purifying cellulose is made into quality The water slurry that score is 15% is placed in ultrasonic wave plant cell pulverizer the power ultrasonic processing 40min with 1350W, control Supersonic frequency is 32kHz, and wooden nano-cellulose is made;The beaker equipped with 7mL ethyl orthosilicates is added in 55mL absolute ethyl alcohols In, 12min is stirred, 3mL water is added in beaker, after stirring 11min, then the hydrochloric acid that mass fraction is 15% is added into beaker It is 2.0 to adjust pH value of solution in beaker, stands 3.5h, obtains silicon dioxide gel;The anhydrous second of 45mL is added into ultrasonic disperse instrument Alcohol and the wooden nano-celluloses of 2g, control ultrasonic power are 170W, and ultrasonic disperse 5min obtains cellulose suspension, by fiber Plain suspension is placed in the conical flask with blender, is added into conical flask with the drop rate of 2mL/min with dropping funel 19mL butyl titanates, while starting blender, starting stirring 12min with the rotating speed of 250r/min obtains mixed liquor;To mixing In liquid be added 4mL mass fractions be 20% acetic acid solution, 25mL silicon dioxide gels, stir 1.5h, obtain nano-cellulose/ TiO 2 sol still aging 2 days, obtains dry colloidal sol, dry colloidal sol is placed in the baking oven that set temperature is 65 DEG C, dry 11h obtains gel piece, and gel piece is put into mortar and grinds 32min, crosses 200 mesh and sieves to obtain gel powder;Take 110g clean drieds Shrimp shell be placed in the dilute hydrochloric acid that 215mL mass fractions are 5% and impregnate 2.5h, obtain pickle liquor, it is solidifying that 85g be added into pickle liquor The sodium hydroxide solution that the liquor natrii hypochloritis and 75mL mass fractions that rubber powder, 45mL mass fractions are 2% are 40%, heating rise To 52 DEG C, insulation reaction 45min is placed in supercritical drying drying system temperature, and dry 22h, obtains aeroge under the conditions of 75 DEG C, Aeroge is put into retort, is carbonized in argon gas atmosphere, control carbonization temperature is 320 DEG C, and carbonization time is 22min obtains photocatalytic activity adsorbent.
Example 3
It takes 300g poplars to be put into pulverizer, crushes 2h, cross 200 mesh standard sieves, obtain wooden powder, weigh 150g wooden powders It is placed in Soxhlet extractor, benzyl carbinol and water is mixed to get benzyl carbinol solution for 2 ︰ 1 by volume at normal temperatures, then will 400mL benzyl carbinol solution pours into Soxhlet extractor, and 10h is extracted at 90 DEG C, after removing extract, obtains thick wood fiber powder; Thick wood fiber powder is put into beaker, the sodium chlorite solution that 60mL mass fractions are 20% is added into beaker, is mixed Liquid is used in combination the glacial acetic acid solution that mass fraction is 98% to adjust pH to 5, isothermal holding 7h under the conditions of 80 DEG C of mixed liquor, is repeated Aforesaid operations 5 times remove lignin, obtain holocellulose;The sodium hydroxide solution for being 20% with 150mL mass fractions, 100 Holocellulose, heat-insulation soaking 3h are impregnated under the conditions of DEG C, filtering removal filtrate obtains purifying cellulose, purifying cellulose is made into matter The water slurry that score is 20% is measured, the power ultrasonic processing 45min with 1500W, control are placed in ultrasonic wave plant cell pulverizer Supersonic frequency processed is 35kHz, and wooden nano-cellulose is made;The burning equipped with 8mL ethyl orthosilicates is added in 60mL absolute ethyl alcohols In cup, 15min is stirred, 4mL water is added in beaker, after stirring 12min, then the salt that mass fraction is 15% is added into beaker It is 2.2 that acid, which adjusts pH value of solution in beaker, stands 4h, obtains silicon dioxide gel;The anhydrous second of 50mL is added into ultrasonic disperse instrument Alcohol and the wooden nano-celluloses of 3g, control ultrasonic power are 200W, and ultrasonic disperse 6min obtains cellulose suspension, by fiber Plain suspension is placed in the conical flask with blender, is added into conical flask with the drop rate of 3mL/min with dropping funel 20mL butyl titanates, while starting blender, starting stirring 15min with the rotating speed of 300r/min obtains mixed liquor;To mixing The acetic acid solution that 5mL mass fractions are 20% is added in liquid, 30mL silicon dioxide gels stir 2h, obtain nano-cellulose/bis- Titanium oxide sol still aging 3 days, obtains dry colloidal sol, dry colloidal sol is placed in the baking oven that set temperature is 70 DEG C, dry 12h, Gel piece is obtained, gel piece is put into mortar and grinds 35min, 200 mesh is crossed and sieves to obtain gel powder;Take the shrimp of 120g clean drieds Shell, which is placed in the dilute hydrochloric acid that 230mL mass fractions are 5%, impregnates 3h, obtains pickle liquor, be added into pickle liquor 90g gel powders, The sodium hydroxide solution that the liquor natrii hypochloritis and 80mL mass fractions that 50mL mass fractions are 2% are 40%, is heated to 55 DEG C, insulation reaction 50min is placed in supercritical drying drying system, is dried for 24 hours under the conditions of 80 DEG C, aeroge is obtained, by airsetting Glue is put into retort, is carbonized in argon gas atmosphere, and control carbonization temperature is 350 DEG C, and carbonization time 25min is obtained Photocatalytic activity adsorbent.
Comparative example
With the photocatalytic activity adsorbent of Changzhou company production as a comparison case to photocatalytic activity produced by the present invention Photocatalytic activity adsorbent in adsorbent and comparative example carries out performance detection
Test method:
Formaldehyde removal rate is tested:It takes the adsorbent 25g in example 1~3 and comparative example to be put into dry bag, is used in combination clip close After bag mouth sealing, any corner indoors is placed, wherein every square metre is placed 3 dry bags that adsorbent is housed, 10h is placed, surveys Formaldehyde after content of formaldehyde and 10h before 10h;
Saturated extent of adsorption test is detected by GB/T 19587-2004 standards;
Photocatalysis efficiency is tested:Adsorbent in example 1~3 and comparative example is put into dry bag, clip is used in combination to seal After sack, any corner indoors is placed, by measuring its photocatalytic of the Assessment of Changes of degradation speed of formaldehyde under fluorescent lamp Energy.
Photocatalytic activity adsorbent produced by the present invention is good for the formaldehyde absorbing effect in room air, removal rate It is relatively high, and there is no any harm for human body and environment, degradation rate is high, and photocatalysis effect is good, has broad application prospects.

Claims (8)

1. a kind of preparation method of photocatalytic activity adsorbent, it is characterised in that specifically preparation process is:
(1)It takes 200~300g poplars to be put into pulverizer, crushes 1~2h, cross standard screen, obtain wooden powder, weigh 100~ 150g wooden powders are placed in Soxhlet extractor, and benzyl carbinol and water are mixed to get benzyl carbinol solution at normal temperatures, then by 300~ 400mL benzyl carbinol solution pours into Soxhlet extractor, and extracting obtains thick wood fiber powder after removing extract;
(2)Thick wood fiber powder is put into beaker, 50~60mL sodium chlorite solutions are added into beaker, obtain mixed liquor, and The pH of mixed liquor is adjusted with glacial acetic acid solution, isothermal holding repeats aforesaid operations 3~5 times, removes lignin, obtains comprehensive fiber Element;
(3)With 120~150mL sodium hydroxide solutions, holocellulose, heat-insulation soaking, filtering removal are impregnated under the conditions of certain temperature Filtrate obtains purifying cellulose, and purifying cellulose is made into water slurry, is placed in ultrasonic wave plant cell pulverizer at ultrasound Wooden nano-cellulose is made in reason;
(4)50~60mL absolute ethyl alcohols are added in the beaker equipped with 6~8mL ethyl orthosilicates, 10~15min is stirred, by 3~ 4mL water is added in beaker, after stirring 10~12min, then hydrochloric acid is added into beaker and adjusts pH value of solution in beaker, stand, obtain Silicon dioxide gel;
(5)40~50mL absolute ethyl alcohols are added into ultrasonic disperse instrument and the wooden nano-celluloses of 2~3g, ultrasonic disperse obtain Cellulose suspension is placed in the conical flask with blender by cellulose suspension, is added into conical flask with dropping funel 18~20mL butyl titanates, while starting blender, stirring 10~15min with the rotating speed of 200~300r/min is mixed Liquid;
(6)4~5mL acetic acid solutions are added into mixed liquor, 20~30mL silicon dioxide gels stir 1~2h, obtain Nanowire Element/TiO 2 sol is tieed up, it is still aging, dry colloidal sol is obtained, dry colloidal sol is placed in drying in baking oven, gel piece is obtained, will coagulate Blob of viscose is put into 30~35min of grinding in mortar, and sieving obtains gel powder;
(7)It takes the shrimp shell of 100~120g clean drieds to be placed in 200~230mL dilute hydrochloric acid to impregnate, obtains pickle liquor, to acidleach 80~90g gel powders, 40~50mL liquor natrii hypochloritis and 70~80mL sodium hydroxide solutions are added in liquid, heat temperature raising is protected Temperature reaction is placed on drying in supercritical drying drying system, obtains aeroge, aeroge is put into retort, in argon gas atmosphere It is carbonized, obtains photocatalytic activity adsorbent.
2. a kind of preparation method of photocatalytic activity adsorbent according to claim 1, it is characterised in that:Step (1)The be sieved specification is 200 mesh, and mixed volume ratio is 2 ︰ 1 to benzyl carbinol at normal temperatures with water, and extraction temperature is 80~90 DEG C, extraction times are 5~10h.
3. a kind of preparation method of photocatalytic activity adsorbent according to claim 1, it is characterised in that:Step (2)Sodium chlorite solution's mass fraction is 20%, and glacial acetic acid solution mass fraction is 98%, and the pH for adjusting mixed liquor is 4 ~5, isothermal holding temperature is 75~80 DEG C, and the isothermal holding time is 5~7h.
4. a kind of preparation method of photocatalytic activity adsorbent according to claim 1, it is characterised in that:Step (3)The mass fraction of the sodium hydroxide solution is 20%, and soaking temperature is 90~100 DEG C, and the heat-insulation soaking time is 2~3h, The mass fraction of water slurry is 10~20%, and ultrasonic power is 1200~1500W, and sonication treatment time is 30~45min, is surpassed Acoustic frequency is 30~35kHz.
5. a kind of preparation method of photocatalytic activity adsorbent according to claim 1, it is characterised in that:Step (4)The mass fraction of the hydrochloric acid is 15%, and it is 1.8~2.2 to adjust pH value of solution in beaker, and time of repose is 3~4h.
6. a kind of preparation method of photocatalytic activity adsorbent according to claim 1, it is characterised in that:Step (5)The control ultrasonic power be 150~200W, the ultrasonic disperse time be 4~6min, dropping funel drop rate be 2~ 3mL/min。
7. a kind of preparation method of photocatalytic activity adsorbent according to claim 1, it is characterised in that:Step (6)The mass fraction of the acetic acid solution is 20%, and the still aging time is 2~3 days, and baking oven set temperature is 60~70 DEG C, Drying time is 10~12h, and be sieved specification is sieved for 200 mesh.
8. a kind of preparation method of photocatalytic activity adsorbent according to claim 1, it is characterised in that:Step (7)The mass fraction of the dilute hydrochloric acid is 5%, and soaking time is 2~3h, and the mass fraction of liquor natrii hypochloritis is 2%, hydrogen-oxygen The mass fraction for changing sodium solution is 40%, and temperature is 50~55 DEG C after heat temperature raising, and the insulation reaction time is 40~50min, is done Dry temperature be 70~80 DEG C, drying time be 20~for 24 hours, control carbonization temperature be 300~350 DEG C, carbonization time be 20~ 25min。
CN201810463270.4A 2018-05-15 2018-05-15 Preparation method of photocatalytic active gas adsorbent Active CN108704624B (en)

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 true CN108704624A (en) 2018-10-26
CN108704624B 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)

Cited By (6)

* Cited by examiner, † Cited by third party
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
CN112808227A (en) * 2020-12-28 2021-05-18 苏州启创新材料科技有限公司 Hybrid aerogel adsorbent, preparation method thereof and application of hybrid aerogel adsorbent in wastewater treatment
CN112870965A (en) * 2021-01-19 2021-06-01 黎新安 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
CN113908652A (en) * 2021-09-09 2022-01-11 济南市平阴县玛钢厂 Process for reducing smoke dust emission of cupola furnace in foundry

Citations (6)

* Cited by examiner, † Cited by third party
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

Patent Citations (6)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
Title
XIAOTING ZHANG ET AL.: "Fabricating 3D hierarchical porous TiO2 and SiO2 with high specific surface area by using nanofibril-interconnected cellulose aerogel as a new biotemplate", 《INDUSTRIAL CROPS & PRODUCTS》 *

Cited By (7)

* Cited by examiner, † Cited by third party
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
CN112808227A (en) * 2020-12-28 2021-05-18 苏州启创新材料科技有限公司 Hybrid aerogel adsorbent, preparation method thereof and application of hybrid aerogel adsorbent in wastewater treatment
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
CN112870965A (en) * 2021-01-19 2021-06-01 黎新安 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
CN113908652A (en) * 2021-09-09 2022-01-11 济南市平阴县玛钢厂 Process for reducing smoke dust emission of cupola furnace in foundry

Also Published As

Publication number Publication date
CN108704624B (en) 2021-07-20

Similar Documents

Publication Publication Date Title
CN108704624A (en) A kind of preparation method of photocatalytic activity adsorbent
CN107029668B (en) A kind of honeycomb type molecular sieve-active carbon compound adsorbent, preparation method and applications
CN104289179B (en) Method for preparing attapulgite/carbon composite adsorbent by one-step carbonization-activation
CN102580703B (en) Method for preparing efficient air purification material
CN104549370B (en) Photocatalysis cellular activated carbon net
CN107362788A (en) A kind of graphene oxide/titanium dioxide activated carbon three-dimensional composite material and preparation method thereof
CN108479707A (en) A kind of preparation method of material for air purification
CN108579721B (en) Preparation method of photocatalyst for air VOC treatment
CN103977755B (en) A kind of high catalytic oxidation activity material for air purification
CN103752287B (en) A kind of construction and decoration pollutant inorganic agent and preparation method thereof
CN105688660B (en) Using photocatalyst of titanium dioxide as material for air purification of base material and preparation method thereof
CN106185921A (en) A kind of method and purposes preparing porous carbon materials with NaCl for hard template
CN104707588B (en) A kind of material for air purification containing titania aerogel and preparation method thereof
CN109569519A (en) The method for preparing active sludge carbon base formaldehyde adsorbent using municipal sludge
CN106824088A (en) A kind of fluffy base optic catalytic cellular activated carbon of Chinese chestnut fruit and its off-gas cleaning equipment
CN109894007A (en) A kind of environment-friendly type air scavenging material and its preparation process
CN109647342A (en) Moisture-proof renewable active carbon of one kind and preparation method thereof
CN107617313B (en) A kind of filtering glued membrane and preparation method thereof for the middle organic pollution that purifies the air of a room
CN108298519A (en) A kind of preparation method using the enhanced charcoal-aero gel of Ludox
CN107213868A (en) One kind has formaldehyde absorbing degradation function safe green composite and preparation method
Duan et al. Performance and characterization of bamboo-based activated carbon prepared by boric acid activation
CN110203930A (en) A kind of active carbon and preparation method thereof
CN104772133B (en) A kind of indoor cleaning photoactivation agent and preparation method thereof
CN109046272A (en) A kind of preparation method of high absorbent-type formaldehyde adsorbent
CN106040186B (en) A kind of method of Chinese medicine dreg synthesis porous adsorbing material

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

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

TA01 Transfer of patent application right
GR01 Patent grant
GR01 Patent grant