CN105968790A - Preparation method of composite sponge for sewage filtration - Google Patents
Preparation method of composite sponge for sewage filtration Download PDFInfo
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- CN105968790A CN105968790A CN201610332926.XA CN201610332926A CN105968790A CN 105968790 A CN105968790 A CN 105968790A CN 201610332926 A CN201610332926 A CN 201610332926A CN 105968790 A CN105968790 A CN 105968790A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/08—Polyurethanes from polyethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
- C08G65/38—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention provides a preparation method of composite sponge for sewage filtration. The preparation method comprises the following steps: 1: uniformly mixing polyether polyol, isocyanate, sodium dodecyl benzene sulfonate, carboxymethylcellulose, dibutyltin dilaurate and aluminium hydroxide and stirring and foaming the materials, thus preparing a non-cured foam material; 2: mixing furfural, water-soluble phenolic resin, sepiolite powder, halloysite nanotubes, nanocrystalline cellulose, polyvinylpyrrolidone and water, obtaining mixed liquor A and dropwise adding ammonia water to the mixed liquor A; reacting to obtain sol; 3: mixing the foam material, sol and phenoxy resin to obtain a mixed foam material; aging the mixed foam material and then washing the mixed foam material with water, thus obtaining a wet sponge; 4: drying the wet sponge, thus obtaining the composite sponge for sewage filtration. The composite sponge for sewage filtration, which is prepared by the method, has good adsorbing effects, high adsorption capacity, short purification time and high efficiency.
Description
Technical field
The present invention relates to technical field of water purification, especially, relate to the preparation method of a kind of sewage water filtration composite sponge.
Background technology
In recent decades, China's industrial development is rapid.But in the past, the factory and enterprise of China does not focus on environmental conservation, generally
There is the situation that the sewage after will not pass through purification directly discharges.This year, along with the continuous deterioration of environment, China environmental protection
The most also the discharge to sewage has carried out strict supervision.Factory of all of enterprise, after sewage has to pass through purification, water quality meets state
After family's discharge standard, just can discharge.
At present, the purification method of trade effluent is by including the steps such as standing sedimentation, flocculation sediment.If Authorization Notice No. is CN
The Chinese patent of 101928069 B discloses a kind of purifying agent for polluted water, PHA, kieselguhr, humic acid, biology live
Property agent, inorganic metal salt and other materials composition, the invention also discloses the effluent purification method utilizing this purifying agent for polluted water.
Due to the fact that use completely biodegradable material PHA is the slow-release material of bioactivator, this can be completely biological
Degradable material is slowly degraded and release bioactive agent, it is achieved the long-term high-efficient purification function of bioactivator.And combine aquatic planting
The thing synergy purified treatment to realizing sewage phosphorus, nitrogen, polycyclic aromatic hydrocarbon, heavy metal.
In addition to above-mentioned purifying agent for polluted water, also have a large amount of purifying agent for polluted water with activated carbon as main material, its principle in the market
For utilizing the adsorptivity of activated carbon that water body is purified.
But above-mentioned water purification agent is limited to the clean-up effect of sewage and poor to the adsorption effect of impurity, adsorption capacity is low, during purification
Between long, inefficiency.
Summary of the invention
Present invention aim at providing the preparation method of a kind of sewage water filtration composite sponge, to solve purifying agent for polluted water in prior art
Adsorption effect is poor, and adsorption capacity is low, and the clarification time is long, the technical problem of inefficiency.
For achieving the above object, the preparation method of a kind of sewage water filtration composite sponge, comprise the following steps:
Step 1: by polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, di lauric dibutyl
Stannum and the aluminium hydroxide mix homogeneously of 0.8-1.2:1.2-1.6:0.01-0.03:0.04-0.06:0.01-0.03:0.1-0.3 in mass ratio, at 30-40
It is stirred foaming at DEG C, prepares uncooked foam material.
Step 2: by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinyl pyrrole
Alkanone and water 3-5:1:0.3-0.5:0.1-0.3:0.5-1.5:0.4-0.6:100 in mass ratio mixes, and obtains mixed liquor A after stirring,
The ammonia that concentration is 1mol/L is added drop-wise in mixed liquor A until the pH value of mixed liquor A is 7-8 under stirring condition；Then exist
React 16-48h at 55-65 DEG C, obtain colloidal sol.
Step 3: foam material, colloidal sol, focus ratio 3-5:1:0.2-0.3 in mass ratio is mixed, and stirs at 130-150 DEG C
Mix uniformly, obtain mix-froth material；After mix-froth material ageing 12-24h, after washing, obtain wet sponge.
Step 4: use supercritical fluid that wet sponge is dried, obtain sewage water filtration composite sponge.
In the inventive solutions, not using traditional flocculant or activated carbon as main component, change into using with poly-ammonia
Ester material and the composite foam sponge material that charcoal-aero gel is main base.Compared with activated carbon, this composite foam sponge material is gathered around
Having more preferable adsorption capacity and the duct of sizes rank, the pore size in polyurethane foam sponge is bigger, it is possible to
The impurity of grain class carries out active adsorption, and the pore size in charcoal-aero gel is less, it is possible to the material such as heavy metal, pigment is inhaled
Attached.Therefore higher for the adsorptivity of the polluter of different size, kind in water.In the preparation process of foam material, 12
Sodium alkyl benzene sulfonate plays foaming effect, and carboxymethyl cellulose can increase the degree of cross linking, and dibutyl tin laurate plays catalysis and makees
With, aluminium hydroxide can thermally decompose more than 130 DEG C, produces Alpha-alumina and steam, after steam is escaped, plays
Pore effect.
And in traditional aeroge preparation process, during gel process is dried and prepares aeroge, due to the three of its inside
The intensity of dimension network structure is the highest, and original structure is easily caved in, and causes porosity and specific surface area to reduce, and material after molding
Fragility is higher, mechanical strength, toughness, poor water resistance, has had a strong impact on actual application.The carbon aerogel material of the present invention, with
The composite of charcoal-meerschaum-nanometer galapectite pipe-nano-crystal cellulose is matrix, and wherein meerschaum has the hole of nano-scale,
The material such as pigment, heavy metal ion had the strongest absorbability；Nanometer galapectite pipe is the chopped fiber pipe with hollow structure
Shape, has the duct of nano-scale, the intensity of material can be greatly improved, and can also improve simultaneously after preparing charcoal-aero gel
The toughness of carbon aerogel material, due to meerschaum, the existence of nanometer galapectite pipe, it is possible in carbon aerogel material dry run
Playing a supporting role, the three-dimensional net structure in charcoal-aero gel is difficult to cave in, thus pore structure when keeping collosol state and
Specific surface area.Further, self nano pore is also had due to meerschaum, nanometer galapectite pipe, it may have strong adsorptivity, therefore
The hole that the space occupied by meerschaum, nanometer galapectite pipe is lost can be made up.Nano-crystal cellulose not only self can adsorb
The heavy metal ion such as lead, chromium, and the combination of each material can be assisted when preparing colloidal sol；Polyvinylpyrrolidone is as pore
Agent, it is possible to make the duct of micron level, the pore size of abundant sewage water filtration composite sponge such that it is able to each pollutant
Adsorb.
Wherein during by foam material, colloidal sol mixing, being added with focus ratio, focus ratio not only has bonding and makees
With, and it can improve the resistance to water of composite, mechanical strength and resistance to contractility.Enable to sewage water filtration composite sponge
Long-time at underwater work.
Further, the preparation method of polyether polyol described in step 1 is as follows: by lignin and phenol 1-2:15-25 in mass ratio
Mix homogeneously, at 170-180 DEG C, stirring reaction 40-60min, at the uniform velocity drips the 10wt% that quality is phenol 1.5 times during reaction
Sodium hydroxide solution, after reaction, reacting liquid pH value is adjusted to neutrality, and is cooled to 50-60 DEG C, in reactant liquor add quality
For the polyhydric alcohol that the formaldehyde of phenol 2-3 times, quality are phenol 0.25-0.35 times, finally stirring reaction 40-80min under heat-retaining condition,
Prepare polyether polyol.
Further, at least one during described polyhydric alcohol is glycerol, xylitol, sorbitol.
Further, the solid content of described water soluble phenol resin is 40-50%, and free phenol content is less than or equal to 10%.
Further, the rate of addition of ammonia described in step 2 is 20-30mL/min.
Further, described sepiolite powder and nanometer galapectite pipe are through activation processing: sepiolite powder and nanometer galapectite pipe are divided
In the 4wt% hydrochloric acid solution of its 400-600 times of quality, do not soak 4-6h, obtain nanometer galapectite pipe and the sepiolite powder of activation.
Nanometer galapectite pipe is carried out acid activation process, it is possible to increase the adsorption efficiency of himself, it is possible to increase sewage water filtration is combined
The adsorption efficiency of sponge.
Further, step 4 condition is: use carbon dioxide as dry medium, temperature 40-50 DEG C, pressure 5-15MPa,
Time 6-24h.
The method have the advantages that
Sewage water filtration composite sponge prepared by the inventive method, has multistage pore canal, to the dirt advantages of good adsorption effect in water body, inhales
Attached capacity is big, the feature that adsorption efficiency is high.
In addition to objects, features and advantages described above, the present invention also has other objects, features and advantages.Below
The present invention is further detailed explanation.
Detailed description of the invention
Hereinafter embodiments of the invention are described in detail, but the present invention can according to claim limit and cover multiple
Different modes is implemented.
Embodiment 1
The preparation method of a kind of sewage water filtration composite sponge, comprises the following steps:
Step 1: mixed homogeneously with phenol 1.5:20 in mass ratio by lignin, at 175 DEG C, stirring reaction 50min, reacts the phase
Between at the uniform velocity drip the sodium hydroxide solution of the 10wt% that quality is phenol 1.5 times, after reaction, reacting liquid pH value is adjusted to neutrality, and
Be cooled to 55 DEG C, add in reactant liquor quality be the formaldehyde of phenol 2.5 times, quality be the glycerol of phenol 0.3 times, finally protecting
Under the conditions of temperature, stirring reaction 60min, prepares polyether polyol.
By polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, dibutyl tin laurate and hydrogen
The aluminium oxide mix homogeneously of 1:1.3:0.02:0.05:0.02:0.2 in mass ratio, is stirred foaming at 35 DEG C, prepares uncooked bubble
Foam material.
Step 2: by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinyl pyrrole
Alkanone and water 4:1:0.4:0.2:1:0.5:100 in mass ratio mixes, and obtains mixed liquor A, under agitation by concentration after stirring
Ammonia for 1mol/L is added drop-wise in mixed liquor A until the pH value of mixed liquor A is as 7-8 with the rate of addition of 25mL/min；So
After at 60 DEG C react 16-48h, obtain colloidal sol.
The solid content of described water soluble phenol resin is 45%, and free phenol content is less than or equal to 10%.Described sepiolite powder and nanometer
Galapectite pipe is through activation processing: by sepiolite powder and nanometer galapectite pipe respectively in the 4wt% hydrochloric acid solution of its 500 times of quality
Soak 5h, obtain nanometer galapectite pipe and the sepiolite powder of activation.
Step 3: foam material, colloidal sol, focus ratio 4:1:0.25 in mass ratio is mixed, and stirs at 140 DEG C,
Obtain mix-froth material；After mix-froth material ageing 18h, after washing, obtain wet sponge.
Step 4: use supercritical fluid that wet sponge is dried, obtain sewage water filtration composite sponge.Wherein drying condition is:
Use carbon dioxide as dry medium, temperature 45 C, pressure 10MPa, time 15h.
The pore capacities of the sewage water filtration composite sponge that the present embodiment prepares is 3.54cm3/ g, porosity is 81%.
Embodiment 2
The preparation method of a kind of sewage water filtration composite sponge, comprises the following steps:
Step 1: mixed homogeneously with phenol 1:15 in mass ratio by lignin, stirring reaction 60min at 170 DEG C, during reaction
At the uniform velocity drip the sodium hydroxide solution of the 10wt% that quality is phenol 1.5 times, after reaction, reacting liquid pH value is adjusted to neutrality, and drops
Temperature to 50 DEG C, add in reactant liquor quality be the formaldehyde of phenol 2 times, quality be the xylitol of phenol 0.15 times, quality be benzene
The sorbitol that phenol is 0.05 times, finally stirring reaction 40min under heat-retaining condition, prepares polyether polyol.
By polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, dibutyl tin laurate and hydrogen
The aluminium oxide mix homogeneously of 0.8:1.2:0.01:0.04:0.01:0.1 in mass ratio, is stirred foaming at 30 DEG C, prepares uncooked
Foam material.
Step 2: by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinyl pyrrole
Alkanone and water 3:1:0.3:0.1:0.5:0.4:100 in mass ratio mixes, and obtains mixed liquor A, under agitation by dense after stirring
The ammonia that degree is 1mol/L is added drop-wise in mixed liquor A until the pH value of mixed liquor A is as 7-8 with the rate of addition of 20mL/min；
Then at 55 DEG C, react 8h, obtain colloidal sol.
The solid content of described water soluble phenol resin is 40%, and free phenol content is less than or equal to 10%.Described sepiolite powder and nanometer
Galapectite pipe is through activation processing: by sepiolite powder and nanometer galapectite pipe respectively in the 4wt% hydrochloric acid solution of its 400 times of quality
Soak 4h, obtain nanometer galapectite pipe and the sepiolite powder of activation.
Step 3: foam material, colloidal sol, focus ratio 3:1:0.2 in mass ratio is mixed, and stirs at 130 DEG C,
To mix-froth material；After mix-froth material ageing 24h, after washing, obtain wet sponge.
Step 4: use supercritical fluid that wet sponge is dried, obtain sewage water filtration composite sponge.Wherein drying condition is:
Use carbon dioxide as dry medium, temperature 40 DEG C, pressure 5MPa, time 24h.
The pore capacities of the sewage water filtration composite sponge that the present embodiment prepares is 3.32cm3/ g, porosity is 80%.
Embodiment 3
The preparation method of a kind of sewage water filtration composite sponge, comprises the following steps:
Step 1: mixed homogeneously with phenol 2:25 in mass ratio by lignin, stirring reaction 40min at 180 DEG C, during reaction
At the uniform velocity drip the sodium hydroxide solution of the 10wt% that quality is phenol 1.5 times, after reaction, reacting liquid pH value is adjusted to neutrality, and drops
Temperature to 60 DEG C, add in reactant liquor quality be the formaldehyde of phenol 3 times, quality be the sorbitol of phenol 0.35 times, finally protecting
Under the conditions of temperature, stirring reaction 80min, prepares polyether polyol.
By polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, dibutyl tin laurate and hydrogen
The aluminium oxide mix homogeneously of 1.2:1.6:0.03:-0.06:0.03:0.3 in mass ratio, is stirred foaming at 40 DEG C, prepares uncooked
Foam material.
Step 2: by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinyl pyrrole
Alkanone and water 5:1:0.5:0.3:1.5:0.6:100 in mass ratio mixes, and obtains mixed liquor A, under agitation will after stirring
Concentration is that the ammonia of 1mol/L is added drop-wise in mixed liquor A until the pH value of mixed liquor A is as 7-8 with the rate of addition of 30mL/min；
Then at 65 DEG C, react 16h, obtain colloidal sol.
The solid content of described water soluble phenol resin is 50%, and free phenol content is less than or equal to 10%.Described sepiolite powder and nanometer
Galapectite pipe is through activation processing: by sepiolite powder and nanometer galapectite pipe respectively in the 4wt% hydrochloric acid solution of its 600 times of quality
Soak 6h, obtain nanometer galapectite pipe and the sepiolite powder of activation.
Step 3: foam material, colloidal sol, focus ratio 5:1:0.3 in mass ratio is mixed, and stirs at 150 DEG C,
Obtain mix-froth material；After mix-froth material ageing 12h, after washing, obtain wet sponge.
Step 4: use supercritical fluid that wet sponge is dried, obtain sewage water filtration composite sponge.Wherein drying condition is:
Use carbon dioxide as dry medium, temperature 50 C, pressure 15MPa, time 6h.
The pore capacities of the sewage water filtration composite sponge that the present embodiment prepares is 3.28cm3/G, porosity is 80%.
Embodiment 4
The present embodiment is with the difference of embodiment 1:
In step 1, by polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, tin dilaurate two
Butyl tin and aluminium hydroxide 0.9:1.3:0.015:0.045:0.015:0.15 in mass ratio mixes.
In step 2, by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyethylene
Ketopyrrolidine and water 3.5:1:0.35:0.15:0.75:0.45:100 in mass ratio mixes.
In step 3, foam material, colloidal sol, focus ratio 3.5:1:0.225 in mass ratio is mixed.
The pore capacities of the sewage water filtration composite sponge that the present embodiment prepares is 3.41cm3/ g, porosity is 81%.
Embodiment 5
The present embodiment is with the difference of embodiment 1:
In step 1, by polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, tin dilaurate two
Butyl tin and aluminium hydroxide 1.1:1.5:0.025:0.05:0.025:0.25 in mass ratio mixes.
In step 2, by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyethylene
Ketopyrrolidine and water 4.5:1:0.45:0.25:1.25:0.55:100 in mass ratio mixes.
In step 3, foam material, colloidal sol, focus ratio 4.5:1:0.275 in mass ratio is mixed.
The pore capacities of the sewage water filtration composite sponge that the present embodiment prepares is 3.11cm3/ g, porosity is 80%.
Embodiment 6
The present embodiment is with the difference of embodiment 1:
In step 1, by polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, tin dilaurate two
Butyl tin and aluminium hydroxide 0.9:1.5:0.01:0.06:0.01:0.3 in mass ratio mixes.
In step 2, by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyethylene
Ketopyrrolidine and water 4:1:0.5:0.3:1:0.5:100 in mass ratio mixes.
In step 3, foam material, colloidal sol, focus ratio 3:1:0.3 in mass ratio is mixed.
The pore capacities of the sewage water filtration composite sponge that the present embodiment prepares is 3.48cm3/ g, porosity is 80%.
Comparative example 1
The present embodiment is with the difference of embodiment 1:
In step 1, by polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, tin dilaurate two
Butyl tin and aluminium hydroxide 0.7:1.1:0.01:0.03:0.01:0.1 in mass ratio mixes.
In step 2, by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyethylene
Ketopyrrolidine and water 6:1:0.6:0.4:1.75:0.7:100 in mass ratio mixes.The rate of addition of ammonia is 15mL/min.
In step 3, foam material, colloidal sol, focus ratio 2.5:1:0.15 in mass ratio is mixed.
The pore capacities of the sewage water filtration composite sponge that the present embodiment prepares is 2.88cm3/ g, porosity is 78%.
Comparative example 2
The present embodiment is with the difference of embodiment 1:
In step 1, by polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, tin dilaurate two
Butyl tin and aluminium hydroxide 1.3:1.1:0.03:0.05:0.01:0.3 in mass ratio mixes.
In step 2, by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyethylene
Ketopyrrolidine and water 2:1:0.2:0.05:0.25:0.3:100 in mass ratio mixes.The rate of addition of ammonia is 35mL/min.
In step 3, foam material, colloidal sol, focus ratio 5.5:1:0.35 in mass ratio is mixed.
The pore capacities of the sewage water filtration composite sponge that the present embodiment prepares is 2.71cm3/ g, porosity is 77%.
Comparative example 3
The present embodiment is with the difference of embodiment 1:
In step 1, by polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, tin dilaurate two
Butyl tin and aluminium hydroxide 1.3:1.7:0.04:0.07:0.04:0.35 in mass ratio mixes.
In step 2, by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyethylene
Ketopyrrolidine and water 6:1:0.2:0.4:1.75:0.3:100 in mass ratio mixes.The rate of addition of ammonia is 15mL/min.
In step 3, foam material, colloidal sol, focus ratio 5.5:1:0.15 in mass ratio is mixed.
The pore capacities of the sewage water filtration composite sponge that the present embodiment prepares is 2.66cm3/ g, porosity is 76%.
Knowable to the embodiment 1-6 Data Comparison with comparative example 1-3, the sewage water filtration composite sponge that embodiment 1-6 prepares
Performance parameter is more excellent.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for those skilled in the art
For, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, any amendment of being made, etc.
With replacement, improvement etc., should be included within the scope of the present invention.
Claims (7)
1. the preparation method of a sewage water filtration composite sponge, it is characterised in that comprise the following steps:
Step 1: by polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, di lauric dibutyl
Stannum and the aluminium hydroxide mix homogeneously of 0.8-1.2:1.2-1.6:0.01-0.03:0.04-0.06:0.01-0.03:0.1-0.3 in mass ratio, at 30-40
It is stirred foaming at DEG C, prepares uncooked foam material；
Step 2: by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinyl pyrrole
Alkanone and water 3-5:1:0.3-0.5:0.1-0.3:0.5-1.5:0.4-0.6:100 in mass ratio mixes, and obtains mixed liquor A after stirring,
The ammonia that concentration is 1mol/L is added drop-wise in mixed liquor A until the pH value of mixed liquor A is 7-8 under stirring condition；Then exist
React 16-48h at 55-65 DEG C, obtain colloidal sol；
Step 3: foam material, colloidal sol, focus ratio 3-5:1:0.2-0.3 in mass ratio is mixed, and stirs at 130-150 DEG C
Mix uniformly, obtain mix-froth material；After mix-froth material ageing 12-24h, after washing, obtain wet sponge；
Step 4: use supercritical fluid that wet sponge is dried, obtain sewage water filtration composite sponge.
The preparation method of a kind of sewage water filtration composite sponge the most according to claim 1, it is characterised in that institute in step 1
The preparation method stating polyether polyol is as follows: mixed homogeneously with phenol 1-2:15-25 in mass ratio by lignin, at 170-180 DEG C
Lower stirring reaction 40-60min, at the uniform velocity drips the sodium hydroxide solution of the 10wt% that quality is phenol 1.5 times, reaction during reaction
After reacting liquid pH value is adjusted to neutrality, and be cooled to 50-60 DEG C, add in reactant liquor formaldehyde that quality is phenol 2-3 times,
Quality is the polyhydric alcohol of phenol 0.25-0.35 times, and finally stirring reaction 40-80min under heat-retaining condition, prepares polyether polyol.
The preparation method of a kind of sewage water filtration composite sponge the most according to claim 2, it is characterised in that described polyhydric alcohol
For at least one in glycerol, xylitol, sorbitol.
The preparation method of a kind of sewage water filtration composite sponge the most according to claim 1, it is characterised in that described water solublity
The solid content of phenolic resin is 40-50%, and free phenol content is less than or equal to 10%.
The preparation method of a kind of sewage water filtration composite sponge the most according to claim 1, it is characterised in that institute in step 2
The rate of addition stating ammonia is 20-30mL/min.
The preparation method of a kind of sewage water filtration composite sponge the most according to claim 1, it is characterised in that described meerschaum
Powder and nanometer galapectite pipe are through activation processing: by sepiolite powder and nanometer galapectite pipe respectively in its 400-600 times of quality
4wt% hydrochloric acid solution soaks 4-6h, obtains nanometer galapectite pipe and the sepiolite powder of activation.
The preparation method of a kind of sewage water filtration composite sponge the most according to claim 1, it is characterised in that step 4 condition
For: use carbon dioxide as dry medium, temperature 40-50 DEG C, pressure 5-15MPa, time 6-24h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610332926.XA CN105968790B (en) | 2016-05-18 | 2016-05-18 | A kind of preparation method of sewage water filtration composite sponge |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610332926.XA CN105968790B (en) | 2016-05-18 | 2016-05-18 | A kind of preparation method of sewage water filtration composite sponge |
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| Publication Number | Publication Date |
|---|---|
| CN105968790A true CN105968790A (en) | 2016-09-28 |
| CN105968790B CN105968790B (en) | 2018-06-01 |
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| IT201700122757A1 (en) * | 2017-10-27 | 2019-04-27 | Univ Degli Studi Di Palermo | A composition comprising a cellulose nanofiber and halloysite nanotube, a film, and a composite comprising the same |
| CN111040125A (en) * | 2019-12-27 | 2020-04-21 | 陕西科技大学 | Composite fulvic acid antibacterial sponge matrix and preparation method and application thereof |
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| CN105968790B (en) | 2018-06-01 |
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