CN109569519A - The method for preparing active sludge carbon base formaldehyde adsorbent using municipal sludge - Google Patents
The method for preparing active sludge carbon base formaldehyde adsorbent using municipal sludge Download PDFInfo
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- CN109569519A CN109569519A CN201811231554.7A CN201811231554A CN109569519A CN 109569519 A CN109569519 A CN 109569519A CN 201811231554 A CN201811231554 A CN 201811231554A CN 109569519 A CN109569519 A CN 109569519A
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- 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
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01D2257/00—Components to be removed
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
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- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
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- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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Abstract
The invention discloses a kind of preparation methods that active sludge carbon base formaldehyde adsorbent is prepared using municipal sludge, the following steps are included: the first step, mixed raw material preparation: rice husk is cleaned, drying, crushes simultaneously charing process, sludge drying, then, rice husk after charing is mixed with sludge, obtains mixed raw material；Second step, activation process: mixed raw material and activator that the first step obtains being impregnated under ultrasound condition, are subsequently washed with water to neutrality, sludge carbon-based adsorption material after roasting is activated under inert atmosphere protection；Ammonifying process: third step sludge carbon-based adsorption material after activation that second step obtains and aminating agent is impregnated under ultrasound condition, is then washed with deionized to neutrality, active sludge carbon base formaldehyde adsorbent can be obtained after drying.The active sludge carbon base of this method preparation adsorbs adsorption capacity with higher, without secondary pollution, and preparation process is simple and easy.
Description
Technical field
The invention belongs to environment protection fields, and in particular to a kind of to prepare active sludge carbon base formaldehyde adsorbent using municipal sludge
Preparation method.
Background technique
As the newly-built and new finishing house in China is fast-developing, meanwhile, the closure of new building house and building is more next
It is better, exacerbate the pollution level of room air.Common indoor air pollutants matter includes the tool such as formaldehyde, ammonia, benzene homologues
There is volatile substance, wherein formaldehyde is primary pollutant, is also considered as a kind of carcinogenic, teratogenesis harmful substance, more next
More cause the extensive concern of people.
Currently, mainly having air exchange process, plant purification method, absorption method and chemical method to the processing method of indoor formaldehyde.
Wherein, air exchange method is the simplest, it is considered that and new decorating house can achieve safety standard after windowing ventilation six months,
But there is also certain sustained release problems for formaldehyde in finishing material, i.e., remain to detect after windowing was using 1~2 year between finishing back room
Formaldehyde.Plant purification method is mainly to be had extremely strong according to the plants such as cactus, bracketplant, aloe, kaffir lily, sago cycas, chrysanthemum
Absorption formaldehyde ability and put forward, although plant plays the role of centainly purifying air, it is not intended that plant energy
The absorption of formaldehyde in fully erased air, plant PARA FORMALDEHYDE PRILLS(91,95) can only play an auxiliary during entirely purification air
Effect.If the content of formaldehyde in air is too high, in some instances it may even be possible to cause the death of plant itself.Further, since plant is to pass through
Photosynthesis consumes the formaldehyde of surrounding, therefore, at night will be very low with rainy weather absorption efficiency.Chemical Treatment first
Aldehyde mainly falls the formaldehyde in air by consumption of chemical reaction, and carrying out formaldehyde catching using chemical method in the market is mainly one
Aspect purifies air neutralizing formaldehyde in a manner of generating innocuous substance, but can only neutralize first of partially dissociating in air
Aldehyde；On the other hand air is purified to prevent the volatilization of formaldehyde by closed methanal, but in fact formaldehyde will be slow release eventually
Out.For above-mentioned three kinds of methods, absorption method is the most commonly used, also maximally efficient, at present with all kinds of active carbons, compound work
Property porous carbon materials, modified active carbon fiber etc. as the method for solid absorbent removal formaldehyde have relevant report.
Patent CN103980759A discloses the preparation method for coating that a kind of absorption-photocatalysis combined type removes formaldehyde, will live
Property Carbon fiber Wesy concentrated nitric acid processing after, carried titanium dioxide, finally compound by titanium dioxide/activated carbon fiber of preparation on it
Powder uses after being mixed with coating.Although carried titanium dioxide can effectively solve absorption in activated carbon fibre after treatment
The saturation regeneration issues of agent, but concentrated nitric acid has been used during the preparation process, increase the insecurity factor of preparation process.
Patent CN107876015A discloses a kind of composite reactive porous carbon materials and its preparation method and application, will be porous
Carbon material is carried out while being grafted using organic polyatomic acid, ethylenediamine or propane diamine, and prepared active porous carbon material surface is deposited
In a large amount of amino and carboxyl and amide groups, the absorption of PARA FORMALDEHYDE PRILLS(91,95) has many advantages, such as that rate is fast, capacity is big, but during the preparation process
Used porous carbon materials are polyacrylonitrile-based carbon fibre, viscose base activated carbon fiber, asphalt activity carbon fiber, phenolic aldehyde base
Different types of activated carbon fiber such as activated carbon fiber etc., and the cost is relatively high for above-mentioned carbon fiber.
Patent CN108212084A discloses a kind of amination CNT/ graphene sponge preparation method of adsorbable formaldehyde, with
Sponge is skeleton, and carbon nanotube and graphene form nanoscale sponge structure in sponge skeleton, and-NH2 to graphene and
The modification of carbon nanotube exists simultaneously, and can be effectively improved the absorption property of PARA FORMALDEHYDE PRILLS(91,95) gas.However in amination CNT/ stone
In the preparation process of black alkene sponge, needs to take out product and be put into freeze drier and be dried, and cryogenic temperature is -50 DEG C
To -15 DEG C, vacuum degree is less than 10Pa, causes preparation process energy consumption higher.
Patent CN108187633A discloses a kind of formaldehyde adsorbent and its preparation method and application, with graphene, six hydroxyls
Base closes sodium antimonate, glutathione, freeze-drying dragon fruit fruit peel powder, matrine, erythorbic acid sodium and fishbone dust and is prepared as a raw material,
Have the characteristics that methanol adsorption effect is good, but involved raw material is more, and part material is not cheap and is easy to get.
Patent CN108187629A discloses a kind of formaldehyde adsorbent and preparation method thereof, with charcoal, sepiolite, tobacco leaf
18 kinds of raw materials such as powder, microcrystalline cellulose, nano-titanium dioxide prepare a kind of formaldehyde adsorbent.Obtained formaldehyde adsorbent can
Effectively, stablize formaldehyde adsorption, and can be recycled, however, the type of feed for being related to preparing formaldehyde adsorbent in the patent is more
Up to 18 kinds, and the absorption of PARA FORMALDEHYDE PRILLS(91,95) is only physical absorption, therefore adsorption capacity is extremely limited.
Summary of the invention
Object of the present invention is to for deficiency present in methyl aldehyde adsorption material preparation method, provide a kind of to utilize municipal sludge
The preparation method for preparing active sludge carbon base formaldehyde adsorbent is prepared using municipal sludge, rice husk as raw material, by activation process and
Ammonifying process prepares a kind of activated sludge carbon-based adsorption material.The formaldehyde adsorbent prepared using this method, on the one hand can be to city
City's sludge, rice husk carry out resource utilization；On the other hand, prepared active sludge carbon base adsorbs absorption with higher and holds
Amount, it is without secondary pollution, and preparation process is simple and easy.The technical solution is as follows:
The embodiment of the invention provides a kind of preparation sides that active sludge carbon base formaldehyde adsorbent is prepared using municipal sludge
Method, which comprises the following steps:
The first step, mixed raw material preparation: rice husk is cleaned, drying, crushes simultaneously charing process, and sludge drying then, will carbonize
Rice husk is mixed with sludge afterwards, obtains mixed raw material；
Second step, activation process: mixed raw material and activator that the first step obtains are impregnated under ultrasound condition, are then used
Water washing is to neutrality, sludge carbon-based adsorption material after roasting is activated under inert atmosphere protection；
Third step, ammonifying process: sludge carbon-based adsorption material and aminating agent are in ultrasonic item after the activation that second step is obtained
It impregnates, is then washed with deionized to neutrality under part, active sludge carbon base formaldehyde adsorbent can be obtained after drying.
It is preferably 100~150 DEG C of drying sludge temperature, dry in the first step in a kind of implementation of the invention
Time preferably 1~4 hour；Preferably 400~800 DEG C of charred rice husk temperature, the time preferably 1~4 hour；Rice husk and sludge after charing
It is preferred that being that 1:1~3 are mixed according to mass ratio.
In a kind of implementation of the invention, in the second step, mixed raw material and the preferred 1:1 of activator solid-liquid ratio~
3；Activator preferably uses organic acid or inorganic acid or salt.
In a kind of implementation of the invention, in the second step, preferred acetic acid when activator is using organic acid；Activation
Preferred phosphoric acid or sulfuric acid or nitric acid when agent is using inorganic acid；Preferred zinc chloride or iron chloride when activator is using salt；At ultrasound
The reason time preferably 1~4 hour, inert gas preferably use nitrogen or argon gas, and preferably 500~800 DEG C of maturing temperature, calcining time
It is preferred that 0.5~4 hour.
In a kind of implementation of the invention, in the third step, aminating agent uses inorganic and organic mixing ammonia
Agent, inorganic aminating agent preferably use ammonium hydroxide, and organic amino agent preferably uses ethylenediamine or propane diamine.
In a kind of implementation of the invention, in the third step, inorganic and organic aminating agent in aminating agent are mixed
Preferred 1:1~3 of mass ratio；Preferred 1:1~3 of the solid-liquid ratio of sludge carbon-based adsorption material and aminating agent after activation；Ultrasonic treatment
Time preferably 1~4 hour；Preferably 100~150 DEG C of drying temperature, drying time preferably 1~4 hour.
Technical solution provided in an embodiment of the present invention has the benefit that
In a kind of preparation for preparing active sludge carbon base formaldehyde adsorbent using municipal sludge provided in an embodiment of the present invention
Method, raw material are that municipal sludge and rice husk are carried out resource utilization, and it is attached to provide the height with " clean manufacturing " thinking
The approaches and methods of value added resource utilization；Involved raw material are easy in activated sludge carbon-based adsorption material preparation method
, cost is relatively low, and preparation process is simple and easy, and energy consumption is lower, and industrialized production is easy；The carbon-based absorption of prepared activated sludge
Material specific surface area is larger, and alcoholic extract hydroxyl group, phenolic hydroxyl group, the carboxylic group of adsorbent surface are improved by activation process, passes through ammonia
Change process improves the amino and amide group of adsorbent surface, carries out physics so as to PARA FORMALDEHYDE PRILLS(91,95) and the dual suction-operated of chemistry mentions
The adsorption capacity of high formaldehyde.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, embodiment of the present invention will be made into one below
Step ground detailed description.
The present invention provides a kind of preparation method that active sludge carbon base formaldehyde adsorbent is prepared using municipal sludge, specific real
Under applying for example.
Embodiment 1:
The present embodiment provides a kind of preparation methods of the activated sludge carbon-based adsorption material of adsorbable formaldehyde, including following step
It is rapid:
Step 1: city dehydrated sludge 110 DEG C of dry 2h in an oven, it is spare；Rice husk is cleaned, 110 DEG C of dryings in baking oven
2h is smashed, is placed in Muffle furnace and carbonizes 1h at 400 DEG C, spare；
Step 2: dewatered sludge being uniformly mixed with rice husk after charing according to mass ratio 1:1, adsorbent mixed raw material is made；
Step 3: using 50wt% concentration ZnCl2Solution is as activator, according to adsorbent mixed raw material: activator is by material
Liquor ratio is uniformly mixed for 1:2, is washed with deionized after impregnating 2h under ultrasound condition to neutrality, the material after washing is put into horse
600 DEG C of roasting 1h are not warming up to the heating rate of 5 DEG C/min in furnace, the sludge carbon-based adsorption material after being activated, and will
Sample obtained is ground up, sieved 140 mesh, spare；
Step 4: concentration is used as mixed after being mixed for the ethylenediamine of 1mol/L ammonium hydroxide and 0.5mol/L according to 1:2 mass ratio
Aminating agent is closed, according to the sludge carbon-based adsorption material after activation: mixing aminating agent solid-liquid ratio is uniformly mixed for 1:2, ultrasound condition
It is washed with deionized after lower dipping 2h to neutrality, sample after washing is dried to 2h at 110 DEG C to get the suction of active sludge carbon base
Enclosure material.
According to the institutional framework such as table 1 of the activated sludge carbon-based adsorption material of the adsorbable formaldehyde of above-mentioned preparation method preparation
It is shown.
Embodiment 2:
The present embodiment provides a kind of preparation methods of the activated sludge carbon-based adsorption material of adsorbable formaldehyde, including following step
It is rapid:
Step 1: city dehydrated sludge 110 DEG C of dry 2h in an oven, it is spare；Rice husk is cleaned, 110 DEG C of dryings in baking oven
2h is smashed, is placed in Muffle furnace and carbonizes 1h at 400 DEG C, spare；
Step 2: dewatered sludge being uniformly mixed with rice husk after charing according to mass ratio 1:2, adsorbent mixed raw material is made；
Step 3: using 50wt% concentration ZnCl2Solution is as activator, according to adsorbent mixed raw material: activator is by material
Liquor ratio is uniformly mixed for 1:2, is washed with deionized after impregnating 2h under ultrasound condition to neutrality, the material after washing is put into horse
600 DEG C of roasting 1h are not warming up to the heating rate of 5 DEG C/min in furnace, the sludge carbon-based adsorption material after being activated, and will
Sample obtained is ground up, sieved 140 mesh, spare；
Step 4: concentration is used as mixed after being mixed for the ethylenediamine of 1mol/L ammonium hydroxide and 0.5mol/L according to 1:2 mass ratio
Aminating agent is closed, according to the sludge carbon-based adsorption material after activation: mixing aminating agent solid-liquid ratio is uniformly mixed for 1:2, ultrasound condition
It is washed with deionized after lower dipping 2h to neutrality, sample after washing is dried to 2h at 110 DEG C to get the suction of active sludge carbon base
Enclosure material.
According to the institutional framework such as table 1 of the activated sludge carbon-based adsorption material of the adsorbable formaldehyde of above-mentioned preparation method preparation
It is shown.
Embodiment 3:
The present embodiment provides a kind of preparation methods of the activated sludge carbon-based adsorption material of adsorbable formaldehyde, including following step
It is rapid:
Step 1: city dehydrated sludge 110 DEG C of dry 2h in an oven, it is spare；Rice husk is cleaned, 110 DEG C of dryings in baking oven
2h is smashed, is placed in Muffle furnace and carbonizes 1h at 400 DEG C, spare；
Step 2: dewatered sludge being uniformly mixed with rice husk after charing according to mass ratio 1:3, adsorbent material is made；
Step 3: using 50wt% concentration ZnCl2Solution is as activator, according to activator: adsorbent material presses solid-liquid ratio
It is uniformly mixed for 1:2,2h is impregnated under ultrasound condition, then deionized water washs 30min；Mixture after dipping is put into horse
Not in furnace, 600 DEG C of roasting 2h are warming up to the heating rate of 5 DEG C/min, sample obtained is ground up, sieved 140 mesh, is lived
Sludge carbon-based adsorption material after change；
Step 4: concentration is used as mixed after being mixed for the ethylenediamine of 1mol/L ammonium hydroxide and 0.5mol/L according to 1:2 mass ratio
Aminating agent is closed, according to the sludge carbon-based adsorption material after activation: mixing aminating agent solid-liquid ratio is uniformly mixed for 1:2, in ultrasonic item
2h is impregnated under part, and deionized water is then gone to wash 30min, the dry 2h at 110 DEG C.
According to the institutional framework such as table 1 of the activated sludge carbon-based adsorption material of the adsorbable formaldehyde of above-mentioned preparation method preparation
It is shown.
Embodiment 4:
The present embodiment provides a kind of preparation methods of the activated sludge carbon-based adsorption material of adsorbable formaldehyde, including following step
It is rapid:
Step 1: 110 DEG C in an oven of city dehydrated sludge, time are 2 hours, are dried for standby；Rice husk is cleaned, is placed in
110 DEG C of drying in baking oven, crush, carbonize 1 hour under the conditions of 400 DEG C in Muffle furnace；
Step 2: dewatered sludge being uniformly mixed with rice husk after charing according to mass ratio 1:2, adsorbent material is made；
Step 3: using 30wt% concentration ZnCl2Solutions Solution is as activator, according to activator: adsorbent material is by material
Liquor ratio is uniformly mixed for 1:3, and 2h is impregnated under ultrasound condition, and then deionized water washs 30min；Mixture after dipping is put
Enter in Muffle furnace, 600 DEG C of roasting 2h are warming up to the heating rate of 5 DEG C/min, sample obtained is ground up, sieved 140 mesh, is obtained
Sludge carbon-based adsorption material after to activation；
Step 4: concentration is used as mixed after being mixed for the ethylenediamine of 1mol/L ammonium hydroxide and 0.5mol/L according to 1:2 mass ratio
Aminating agent is closed, according to the sludge carbon-based adsorption material after activation: mixing aminating agent solid-liquid ratio is uniformly mixed for 1:2, in ultrasonic item
2h is impregnated under part, and deionized water is then gone to wash 30min, the dry 2h at 110 DEG C.
According to the institutional framework such as table 1 of the activated sludge carbon-based adsorption material of the adsorbable formaldehyde of above-mentioned preparation method preparation
It is shown.
Embodiment 5:
The present embodiment provides a kind of preparation methods of the activated sludge carbon-based adsorption material of adsorbable formaldehyde, including following step
It is rapid:
Step 1: 110 DEG C in an oven of city dehydrated sludge, time are 2 hours, are dried for standby；Rice husk is cleaned, is placed in
110 DEG C of drying in baking oven, crush, carbonize 1 hour under the conditions of 400 DEG C in Muffle furnace；
Step 2: dewatered sludge being uniformly mixed with rice husk after charing according to mass ratio 1:2, adsorbent material is made；
Step 3: using 5wt% concentration FeCl2Solution is as activator, according to activator: adsorbent material presses solid-liquid ratio
It is uniformly mixed for 1:1,2h is impregnated under ultrasound condition, then deionized water washs 30min；Mixture after dipping is put into horse
Not in furnace, 600 DEG C of roasting 1h are warming up to the heating rate of 5 DEG C/min, sample obtained is ground up, sieved 140 mesh, is lived
Sludge carbon-based adsorption material after change；
Step 4: concentration is used as mixed after being mixed for the ethylenediamine of 1mol/L ammonium hydroxide and 0.5mol/L according to 1:2 mass ratio
Aminating agent is closed, according to the sludge carbon-based adsorption material after activation: mixing aminating agent solid-liquid ratio is uniformly mixed for 1:2, in ultrasonic item
2h is impregnated under part, and deionized water is then gone to wash 30min, the dry 2h at 110 DEG C.
According to the institutional framework such as table 1 of the activated sludge carbon-based adsorption material of the adsorbable formaldehyde of above-mentioned preparation method preparation
It is shown.
Embodiment 6:
The present embodiment provides a kind of preparation methods of the activated sludge carbon-based adsorption material of adsorbable formaldehyde, including following step
It is rapid:
Step 1: 110 DEG C in an oven of city dehydrated sludge, time are 2 hours, are dried for standby；Rice husk is cleaned, is placed in
110 DEG C of drying in baking oven, crush, carbonize 1 hour under the conditions of 400 DEG C in Muffle furnace；
Step 2: dewatered sludge being uniformly mixed with rice husk after charing according to mass ratio 1:2, adsorbent material is made；
Step 3: using 10wt%HNO3Solution is as activator, according to activator: adsorbent material is 1:2 by solid-liquid ratio
It is uniformly mixed, 2h is impregnated under ultrasound condition, then deionized water washs 30min；Mixture after dipping is put into Muffle furnace
In, 600 DEG C of roasting 1h are warming up to the heating rate of 5 DEG C/min, sample obtained are ground up, sieved 140 mesh, after obtaining activation
Sludge carbon-based adsorption material；
Step 4: concentration is used as mixed after being mixed for the ethylenediamine of 1mol/L ammonium hydroxide and 0.5mol/L according to 1:2 mass ratio
Aminating agent is closed, according to the sludge carbon-based adsorption material after activation: mixing aminating agent solid-liquid ratio is uniformly mixed for 1:2, in ultrasonic item
2h is impregnated under part, and deionized water is then gone to wash 30min, the dry 2h at 110 DEG C.
According to the institutional framework such as table 1 of the activated sludge carbon-based adsorption material of the adsorbable formaldehyde of above-mentioned preparation method preparation
It is shown.
Embodiment 7:
The present embodiment provides a kind of preparation methods of the activated sludge carbon-based adsorption material of adsorbable formaldehyde, including following step
It is rapid:
Step 1: 110 DEG C in an oven of city dehydrated sludge, time are 2 hours, are dried for standby；Rice husk is cleaned, is placed in
110 DEG C of drying in baking oven, crush, carbonize 1 hour under the conditions of 400 DEG C in Muffle furnace；
Step 2: dewatered sludge being uniformly mixed with rice husk after charing according to mass ratio 1:2, adsorbent material is made；
Step 3: using 10wt%H3PO4Solution is as activator, according to activator: adsorbent material is 1:2 by solid-liquid ratio
It is uniformly mixed, 2h is impregnated under ultrasound condition, then deionized water washs 30min；Mixture after dipping is put into Muffle furnace
In, 600 DEG C of roasting 1h are warming up to the heating rate of 5 DEG C/min, sample obtained are ground up, sieved 140 mesh, after obtaining activation
Sludge carbon-based adsorption material；
Step 4: concentration is used as mixed after being mixed for the ethylenediamine of 1mol/L ammonium hydroxide and 0.5mol/L according to 1:2 mass ratio
Aminating agent is closed, according to the sludge carbon-based adsorption material after activation: mixing aminating agent solid-liquid ratio is uniformly mixed for 1:2, in ultrasonic item
2h is impregnated under part, and deionized water is then gone to wash 30min, the dry 2h at 110 DEG C.
According to the institutional framework such as table 1 of the activated sludge carbon-based adsorption material of the adsorbable formaldehyde of above-mentioned preparation method preparation
It is shown.
Embodiment 8:
The present embodiment provides a kind of preparation methods of the activated sludge carbon-based adsorption material of adsorbable formaldehyde, including following step
It is rapid:
Step 1: 110 DEG C in an oven of city dehydrated sludge, time are 2 hours, are dried for standby；Rice husk is cleaned, is placed in
110 DEG C of drying in baking oven, crush, carbonize 1 hour under the conditions of 400 DEG C in Muffle furnace；
Step 2: dewatered sludge being uniformly mixed with rice husk after charing according to mass ratio 1:2, adsorbent material is made；
Step 3: using 50wt% concentration ZnCl2Solution is as activator, according to adsorbent mixed raw material: activator is by material
Liquor ratio is uniformly mixed for 1:2, is washed with deionized after impregnating 2h under ultrasound condition to neutrality, the material after washing is put into horse
600 DEG C of roasting 1h are not warming up to the heating rate of 5 DEG C/min in furnace, the sludge carbon-based adsorption material after being activated, and will
Sample obtained is ground up, sieved 140 mesh, spare；
Step 4: concentration is used as mixing after being mixed for the ethylenediamine of 1mol/L ammonium hydroxide and 1mol/L according to 1:3 mass ratio
Aminating agent, according to aminating agent: adsorbent material is uniformly mixed by solid-liquid ratio for 1:2 after activation, 2h is impregnated under ultrasound condition, then
Deionized water is gone to wash 30min, the dry 2h at 110 DEG C.
According to the institutional framework such as table 1 of the activated sludge carbon-based adsorption material of the adsorbable formaldehyde of above-mentioned preparation method preparation
It is shown.
Embodiment 9:
The present embodiment provides a kind of preparation methods of the activated sludge carbon-based adsorption material of adsorbable formaldehyde, including following step
It is rapid:
Step 1: 110 DEG C in an oven of city dehydrated sludge, time are 2 hours, are dried for standby；Rice husk is cleaned, is placed in
110 DEG C of drying in baking oven, crush, carbonize 1 hour under the conditions of 400 DEG C in Muffle furnace；
Step 2: dewatered sludge being uniformly mixed with rice husk after charing according to mass ratio 1:2, adsorbent material is made；
Step 3: using 50wt% concentration ZnCl2Solution is as activator, according to adsorbent mixed raw material: activator is by material
Liquor ratio is uniformly mixed for 1:2, is washed with deionized after impregnating 2h under ultrasound condition to neutrality, the material after washing is put into horse
600 DEG C of roasting 1h are not warming up to the heating rate of 5 DEG C/min in furnace, the sludge carbon-based adsorption material after being activated, and will
Sample obtained is ground up, sieved 140 mesh, spare；
Step 4: concentration is used as mixed after being mixed for the propane diamine of 1mol/L ammonium hydroxide and 0.5mol/L according to 1:2 mass ratio
Aminating agent is closed, according to aminating agent: adsorbent material is uniformly mixed by solid-liquid ratio for 1:2 after activation, and 2h is impregnated under ultrasound condition, and
After go deionized water to wash 30min, the dry 2h at 110 DEG C.
According to the institutional framework such as table 1 of the activated sludge carbon-based adsorption material of the adsorbable formaldehyde of above-mentioned preparation method preparation
It is shown.
Experimental example
Formaldehyde absorption experiment is carried out in the closed gas chamber of a built-in fans, is discharged in closed gas test case
Formaldehyde gas, concentration of formaldehyde is 5.0mg/m in closed gas chamber after keeping stable3, place 0.40m2/m3Formaldehyde absorbing
Agent carries out adsorption test, and when adsorption saturation, the purifying rate data and adsorption capacity of formaldehyde are as shown in table 2.
1 activated sludge carbon-based adsorption material institutional framework of table
The purifying formaldehyde rate of 2 activated sludge carbon-based adsorption material of table
| Adsorbent | Formaldehyde absorbing capacity mg/m2 | Purifying rate % |
| Embodiment 1 | 9.40 | 75.2 |
| Embodiment 2 | 9.78 | 78.3 |
| Embodiment 3 | 8.76 | 70.1 |
| Embodiment 4 | 9.06 | 72.5 |
| Embodiment 5 | 8.15 | 65.2 |
| Embodiment 6 | 10.04 | 80.3 |
| Embodiment 7 | 10.32 | 82.6 |
| Embodiment 8 | 10.13 | 81.0 |
| Embodiment 9 | 9.85 | 78.8 |
| Commercial active carbon | 7.02 | 56.2 |
By the absorption property of above-described embodiment and commercial active carbon PARA FORMALDEHYDE PRILLS(91,95) it is found that active sludge carbon base prepared by the present invention
There is a large amount of oxygen-containing alcoholic extract hydroxyl group, phenolic hydroxyl group, carboxyl, amino and amide group in adsorbent surface.It is utilized using resourcebility
Municipal sludge and rice husk are raw material, and the alcoholic extract hydroxyl group, phenolic hydroxyl group, carboxylic group of adsorbent surface are improved by activating, passes through ammonia
Change to improve the amino and amide group of adsorbent surface, has absorption property good.Preparation method provided by the invention is simply easy
Row, it is easy to industrialized production.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (13)
1. a kind of preparation method for preparing active sludge carbon base formaldehyde adsorbent using municipal sludge, which is characterized in that including with
Lower step:
The first step, mixed raw material preparation: rice husk is cleaned, drying, crushes simultaneously charing process, sludge drying, then, by rice after charing
Shell is mixed with sludge, obtains mixed raw material；
Activation process: second step mixed raw material and activator that the first step obtains is impregnated under ultrasound condition, are then washed with water
It washs to neutrality, sludge carbon-based adsorption material after roasting is activated under inert atmosphere protection；
Third step, ammonifying process: sludge carbon-based adsorption material and aminating agent are under ultrasound condition after the activation that second step is obtained
Dipping, is then washed with deionized to neutrality, active sludge carbon base formaldehyde adsorbent can be obtained after drying.
2. the preparation method according to claim 1 that active sludge carbon base formaldehyde adsorbent is prepared using municipal sludge,
Be characterized in that: in the first step, drying sludge temperature is 100~150 DEG C, and drying time is 1~4 hour.
3. the preparation method according to claim 1 that active sludge carbon base formaldehyde adsorbent is prepared using municipal sludge,
Be characterized in that: in the first step, charred rice husk temperature is 400~800 DEG C, and carbonization time is 1~4 hour.
4. the preparation method according to claim 1 that active sludge carbon base formaldehyde adsorbent is prepared using municipal sludge,
Be characterized in that: in the first step, the mass ratio of rice husk and sludge is 1:1~3 after charing.
5. the preparation method according to claim 1 that active sludge carbon base formaldehyde adsorbent is prepared using municipal sludge,
Be characterized in that: in the second step, mixed raw material and activator solid-liquid ratio are 1:1~3.
6. the preparation method according to claim 1 that active sludge carbon base formaldehyde adsorbent is prepared using municipal sludge,
Be characterized in that: in the second step, activator is using organic acid or inorganic acid or salt.
7. the preparation method according to claim 6 that active sludge carbon base formaldehyde adsorbent is prepared using municipal sludge,
Be characterized in that: the organic acid is acetic acid；Inorganic acid is phosphoric acid or sulfuric acid or nitric acid；Salt is zinc chloride or iron chloride.
8. the preparation method according to claim 1 that active sludge carbon base formaldehyde adsorbent is prepared using municipal sludge,
Be characterized in that: in the second step, sonication treatment time is 1~4 hour, and inert atmosphere uses nitrogen or argon gas, maturing temperature
It is 500~800 DEG C, calcining time is 0.5~4 hour.
9. the preparation method according to claim 1 that active sludge carbon base formaldehyde adsorbent is prepared using municipal sludge,
Be characterized in that: in the third step, aminating agent uses inorganic and organic mixing aminating agent.
10. the preparation method according to claim 9 that active sludge carbon base formaldehyde adsorbent is prepared using municipal sludge,
Be characterized in that: the inorganic aminating agent uses ammonium hydroxide, and organic amino agent uses ethylenediamine or propane diamine；It mixes inorganic in aminating agent
The mass ratio of class and organic aminating agent is 1:1~3.
11. the preparation method according to claim 1 that active sludge carbon base formaldehyde adsorbent is prepared using municipal sludge,
Be characterized in that: in the third step, the solid-liquid ratio of sludge carbon-based adsorption material and aminating agent is 1:1~3 after activation.
12. the preparation method according to claim 1 that active sludge carbon base formaldehyde adsorbent is prepared using municipal sludge,
Be characterized in that: in the third step, sonication treatment time is 1~4 hour.
13. the preparation method according to claim 1 that active sludge carbon base formaldehyde adsorbent is prepared using municipal sludge,
Be characterized in that: in the third step, drying temperature is 100~150 DEG C, and drying time is 1~4 hour.
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