CN105968790B - A kind of preparation method of sewage water filtration composite sponge - Google Patents

A kind of preparation method of sewage water filtration composite sponge Download PDF

Info

Publication number
CN105968790B
CN105968790B CN201610332926.XA CN201610332926A CN105968790B CN 105968790 B CN105968790 B CN 105968790B CN 201610332926 A CN201610332926 A CN 201610332926A CN 105968790 B CN105968790 B CN 105968790B
Authority
CN
China
Prior art keywords
water filtration
sewage water
composite sponge
filtration composite
preparation
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.)
Expired - Fee Related
Application number
CN201610332926.XA
Other languages
Chinese (zh)
Other versions
CN105968790A (en
Inventor
不公告发明人
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.)
Guoke Technology Innovation Center Jiujiang Co ltd
Original Assignee
Jiangxi Province O Tai Green Garden Sponge Co Ltd
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 Jiangxi Province O Tai Green Garden Sponge Co Ltd filed Critical Jiangxi Province O Tai Green Garden Sponge Co Ltd
Priority to CN201610332926.XA priority Critical patent/CN105968790B/en
Publication of CN105968790A publication Critical patent/CN105968790A/en
Application granted granted Critical
Publication of CN105968790B publication Critical patent/CN105968790B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L75/00Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
    • C08L75/04Polyurethanes
    • C08L75/08Polyurethanes from polyethers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/48Polyethers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/34Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
    • C08G65/38Macromolecular 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/14Applications used for foams
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Abstract

The present invention provides a kind of preparation methods of sewage water filtration composite sponge.Including:Step 1:Polyether polyol, isocyanates, neopelex, carboxymethyl cellulose, dibutyl tin laurate and aluminium hydroxide are uniformly mixed, uncooked foam material is made in stirring foaming;Step 2:Furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinylpyrrolidone and water are mixed, mixed liquor A is obtained, ammonium hydroxide is added drop-wise in mixed liquor A;Colloidal sol is obtained by the reaction;Step 3:Foam material, colloidal sol, focus ratio are mixed, obtain mix-froth material;After mix-froth material is aged, it is eluted with water, obtains wet sponge;Step 4:Wet sponge is dried, obtains sewage water filtration composite sponge.Sewage water filtration composite sponge advantages of good adsorption effect prepared by the method for the present invention, adsorption capacity is high, and the clarification time is short, efficient.

Description

A kind of preparation method of sewage water filtration composite sponge
Technical field
The present invention relates to technical field of water purification, particularly, are related to a kind of preparation method 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 in China does not focus on environmental protection, Generally existing will not pass through the situation that purified sewage directly discharges.This year, with the continuous deterioration of environment, China's environment Protection part has also carried out strict supervision to the discharge of sewage.All factories of enterprise, after sewage has to pass through purification, water quality symbol After closing discharging standards, it could be discharged.
At present, the purification method of trade effluent is by including standing sedimentation, flocculation sediment and etc..Such as Authorization Notice No. Chinese patent for 101928069 B of CN discloses a kind of purifying agent for polluted water, by polyhydroxyalkanoates, diatomite, humic acid, Bioactivator, inorganic metal salt and other material compositions, the invention also discloses net using the sewage of the purifying agent for polluted water Change method.The present invention, should due to the use of the slow-release material that completely biodegradable material polyhydroxyalkanoates is bioactivator Completely biodegradable material is slowly degraded and release bioactive agent, realizes the long-term high-efficient purification function of bioactivator. And combine water plant synergy to realize sewage phosphorus, nitrogen, polycyclic aromatic hydrocarbon, heavy metal purified treatment.
In addition to above-mentioned purifying agent for polluted water, also have currently on the market largely using activated carbon as the purifying agent for polluted water of main material, Its principle is that water body is purified using the adsorptivity of activated carbon.
But above-mentioned water purification agent is limited to the clean-up effect of sewage, and it is poor to the adsorption effect of impurity, adsorption capacity is low, only The change time is long, inefficiency.
The content of the invention
Present invention aims at a kind of preparation method of sewage water filtration composite sponge is provided, to solve sewage in the prior art The technical issues of cleanser adsorption effect is poor, and adsorption capacity is low, and the clarification time is long, inefficiency.
To achieve the above object, a kind of preparation method of sewage water filtration composite sponge, comprises the following steps:
Step 1:By polyether polyol, isocyanates, neopelex, carboxymethyl cellulose, tin dilaurate two Butyl tin and aluminium hydroxide 0.8-1.2 in mass ratio:1.2-1.6:0.01-0.03:0.04-0.06:0.01-0.03:0.1-0.3 It is uniformly mixed, foaming is stirred at 30-40 DEG C, uncooked foam material is made.
Step 2:By furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyethylene pyrrole Pyrrolidone and water 3-5 in mass ratio:1:0.3-0.5:0.1-0.3:0.5-1.5:0.4-0.6:100 mixing, after stirring evenly To mixed liquor A, the ammonium hydroxide that concentration is 1mol/L is added drop-wise in mixed liquor A under agitation until the pH value of mixed liquor A is 7-8;Then 16-48h is reacted at 55-65 DEG C, obtains colloidal sol.
Step 3:By foam material, colloidal sol, focus ratio 3-5 in mass ratio:1:0.2-0.3 is mixed, and at 130-150 DEG C Under stir evenly, obtain mix-froth material;After mix-froth material is aged 12-24h, after being eluted with water, wet sponge is obtained.
Step 4:Wet sponge is dried using supercritical fluid, obtains sewage water filtration composite sponge.
In the inventive solutions, it is not changed to use using traditional flocculant or activated carbon as main component Using polyurethane material and charcoal-aero gel as the composite foam sponge material of main base.Compared with activated carbon, composite foam sea Continuous material possesses the duct of better adsorption capacity and sizes rank, the pore size in polyurethane foam sponge compared with Greatly, the impurity of particulate species can effectively be adsorbed, the pore size in charcoal-aero gel is smaller, can be to heavy metal, pigment Substances is waited to be adsorbed.Therefore it is stronger for the adsorptivity of the polluter of different size in water, species.In the preparation of foam material In the process, neopelex plays foaming effect, and carboxymethyl cellulose can increase the degree of cross linking, di lauric dibutyl Tin plays catalytic action, and aluminium hydroxide can be thermally decomposed at 130 DEG C or more, generates Alpha-alumina and vapor, vapor After escape, play the role of pore.
And in traditional aeroge preparation process, during gel prepares aeroge by drying, by the inner The intensity of the three-dimensional net structure in portion is not high, and original structure is easily caved in, and porosity and specific surface area is caused to reduce, and is molded Material fragility is higher afterwards, and mechanical strength, toughness, poor water resistance have seriously affected practical application.The charcoal-aero gel material of the present invention Material, using the composite material of charcoal-sepiolite-nanometer galapectite pipe-nano-crystal cellulose as matrix, wherein sepiolite has nano-scale Hole, to the substances such as pigment, heavy metal ion have very strong adsorption capacity;Nanometer galapectite pipe is with hollow structure Staple fiber tubulose has the duct of nano-scale, can greatly improve the intensity of material after charcoal-aero gel is made, and go back simultaneously The toughness of carbon aerogel material can be improved, due to the presence of sepiolite, nanometer galapectite pipe, can be done in carbon aerogel material It plays a supporting role during dry, the three-dimensional net structure in charcoal-aero gel is not easy to cave in, hole during so as to keep collosol state Gap structure and specific surface area.Also, since sepiolite, nanometer galapectite pipe itself also possess nano pore, it may have strong to inhale Attached property, therefore the hole lost by the space that sepiolite, nanometer galapectite pipe occupy can be made up.Nano-crystal cellulose not only from Body can the heavy metal ion such as Adsorption of Lead, chromium, and the combination of each substance can be aided in when preparing colloidal sol;Polyvinylpyrrolidine The duct of micron level can be made as pore-foaming agent in ketone, the pore size of sewage water filtration composite sponge is enriched, so as to right Each pollutant is adsorbed.
Wherein during foam material, colloidal sol are mixed, added with focus ratio, focus ratio not only has viscous Cooperation is used, and it can improve the water resistance of composite material, mechanical strength and resistance to shrinkage.Enable to sewage water filtration compound Sponge operation in water for a long time.
Further, the preparation method of polyether polyol described in step 1 is as follows:By lignin and phenol 1- in mass ratio 2:15-25 is uniformly mixed, and 40-60min is stirred to react at 170-180 DEG C, and quality is at the uniform velocity added dropwise during reaction as 1.5 times of phenol 10wt% sodium hydroxide solution, reacting liquid pH value is adjusted to neutrality after reaction, and be cooled to 50-60 DEG C, into reaction solution Addition quality is the formaldehyde of 2-3 times of phenol, the polyalcohol that quality is 0.25-0.35 times of phenol, is finally stirred under heat-retaining condition 40-80min is reacted, polyether polyol is made.
Further, the polyalcohol is at least one of glycerine, xylitol, sorbierite.
Further, the solid content of the water soluble phenol resin is 40-50%, and free phenol content is less than or equal to 10%.
Further, the rate of addition of ammonium hydroxide described in step 2 is 20-30mL/min.
Further, the sepiolite powder and nanometer galapectite pipe pass through activation process:By sepiolite powder and nanometer angstrom Lip river Madreporic canal impregnates 4-6h in the 4wt% hydrochloric acid solutions of its 400-600 times of quality respectively, the nanometer galapectite pipe activated and sea Afrodite powder.
Acid activation processing is carried out to nanometer galapectite pipe, the adsorption efficiency of its own can be improved, sewage mistake can be improved Filter the adsorption efficiency of composite sponge.
Further, step 4 condition is:Using carbon dioxide as dried medium, 40-50 DEG C of temperature, pressure 5- 15MPa, time 6-24h.
The invention has the advantages that:
Sewage water filtration composite sponge prepared by the method for the present invention has multistage pore canal, to the dirt adsorption effect in water body Well, the characteristics of adsorption capacity is big, and adsorption efficiency is high.
In addition to objects, features and advantages described above, the present invention also has other objects, features and advantages. The present invention is further detailed explanation below.
Specific embodiment
The embodiment of the present invention is described in detail below, but the present invention can be limited and covered according to claim Multitude of different ways implement.
Embodiment 1
A kind of preparation method of sewage water filtration composite sponge, comprises the following steps:
Step 1:By lignin and phenol in mass ratio 1.5:20 are uniformly mixed, and 50min are stirred to react at 175 DEG C, instead Period sodium hydroxide solution of the quality for the 10wt% of 1.5 times of phenol should at the uniform velocity be added dropwise, during reacting liquid pH value is adjusted to after reaction Property, and be cooled to 55 DEG C, added into reaction solution quality be the formaldehyde of 2.5 times of phenol, the glycerine that quality is 0.3 times of phenol, most 60min is stirred to react under heat-retaining condition afterwards, polyether polyol is made.
By polyether polyol, isocyanates, neopelex, carboxymethyl cellulose, dibutyl tin laurate With aluminium hydroxide in mass ratio 1:1.3:0.02:0.05:0.02:0.2 is uniformly mixed, and foaming is stirred at 35 DEG C, is made Uncooked foam material.
Step 2:By furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyethylene pyrrole Pyrrolidone and water in mass ratio 4:1:0.4:0.2:1:0.5:100 mixing, obtain mixed liquor A, in stirring condition after stirring evenly The lower rate of addition by the ammonium hydroxide that concentration is 1mol/L using 25mL/min be added drop-wise in mixed liquor A until mixed liquor A pH value as 7-8;Then 16-48h is reacted at 60 DEG C, obtains colloidal sol.
The solid content of the water soluble phenol resin is 45%, and free phenol content is less than or equal to 10%.The sepiolite powder Pass through activation process with nanometer galapectite pipe:By sepiolite powder and nanometer galapectite pipe respectively in the 4wt% salt of its 500 times of quality 5h is impregnated in acid solution, the nanometer galapectite pipe and sepiolite powder activated.
Step 3:By foam material, colloidal sol, focus ratio in mass ratio 4:1:0.25 mixing, and stirred at 140 DEG C It is even, obtain mix-froth material;After mix-froth material is aged 18h, after being eluted with water, wet sponge is obtained.
Step 4:Wet sponge is dried using supercritical fluid, obtains sewage water filtration composite sponge.Wherein dried strip Part is:Using carbon dioxide as dried medium, temperature 45 C, pressure 10MPa, time 15h.
The pore capacities of sewage water filtration composite sponge made from the present embodiment are 3.54cm3/ g, porosity 81%.
Embodiment 2
A kind of preparation method of sewage water filtration composite sponge, comprises the following steps:
Step 1:By lignin and phenol in mass ratio 1:15 are uniformly mixed, and 60min is stirred to react at 170 DEG C, react The sodium hydroxide solution for the 10wt% that quality is 1.5 times of phenol is at the uniform velocity added dropwise in period, and reacting liquid pH value is adjusted to neutrality after reaction, And 50 DEG C are cooled to, into reaction solution, addition quality is the formaldehyde of 2 times of phenol, quality is the xylitol of 0.15 times of phenol, quality For 0.05 times of sorbierite of phenol, 40min finally is stirred to react under heat-retaining condition, polyether polyol is made.
By polyether polyol, isocyanates, neopelex, carboxymethyl cellulose, dibutyl tin laurate With aluminium hydroxide in mass ratio 0.8:1.2:0.01:0.04:0.01:0.1 is uniformly mixed, and foaming is stirred at 30 DEG C, makes Obtain uncooked foam material.
Step 2:By furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyethylene pyrrole Pyrrolidone and water in mass ratio 3:1:0.3:0.1:0.5:0.4:100 mixing, obtain mixed liquor A, in stirring bar after stirring evenly The ammonium hydroxide that concentration is 1mol/L is added drop-wise in mixed liquor A the pH value until mixed liquor A with the rate of addition of 20mL/min under part For 7-8;Then 8h is reacted at 55 DEG C, obtains colloidal sol.
The solid content of the water soluble phenol resin is 40%, and free phenol content is less than or equal to 10%.The sepiolite powder Pass through activation process with nanometer galapectite pipe:By sepiolite powder and nanometer galapectite pipe respectively in the 4wt% salt of its 400 times of quality 4h is impregnated in acid solution, the nanometer galapectite pipe and sepiolite powder activated.
Step 3:By foam material, colloidal sol, focus ratio in mass ratio 3:1:0.2 mixing, and stirred at 130 DEG C It is even, obtain mix-froth material;After the ageing for 24 hours of mix-froth material, after being eluted with water, wet sponge is obtained.
Step 4:Wet sponge is dried using supercritical fluid, obtains sewage water filtration composite sponge.Wherein dried strip Part is:Using carbon dioxide as dried medium, 40 DEG C of temperature, pressure 5MPa, the time is for 24 hours.
The pore capacities of sewage water filtration composite sponge made from the present embodiment are 3.32cm3/ g, porosity 80%.
Embodiment 3
A kind of preparation method of sewage water filtration composite sponge, comprises the following steps:
Step 1:By lignin and phenol in mass ratio 2:25 are uniformly mixed, and 40min is stirred to react at 180 DEG C, react The sodium hydroxide solution for the 10wt% that quality is 1.5 times of phenol is at the uniform velocity added dropwise in period, and reacting liquid pH value is adjusted to neutrality after reaction, And be cooled to 60 DEG C, into reaction solution add quality be the formaldehyde of 3 times of phenol, the sorbierite that quality is 0.35 times of phenol, finally 80min is stirred to react under heat-retaining condition, polyether polyol is made.
By polyether polyol, isocyanates, neopelex, carboxymethyl cellulose, dibutyl tin laurate With aluminium hydroxide in mass ratio 1.2:1.6:0.03:-0.06:0.03:0.3 is uniformly mixed, and foaming is stirred at 40 DEG C, makes Obtain uncooked foam material.
Step 2:By furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyethylene pyrrole Pyrrolidone and water in mass ratio 5:1:0.5:0.3:1.5:0.6:100 mixing, obtain mixed liquor A, in stirring bar after stirring evenly The ammonium hydroxide that concentration is 1mol/L is added drop-wise in mixed liquor A the pH value until mixed liquor A with the rate of addition of 30mL/min under part For 7-8;Then 16h is reacted at 65 DEG C, obtains colloidal sol.
The solid content of the water soluble phenol resin is 50%, and free phenol content is less than or equal to 10%.The sepiolite powder Pass through activation process with nanometer galapectite pipe:By sepiolite powder and nanometer galapectite pipe respectively in the 4wt% salt of its 600 times of quality 6h is impregnated in acid solution, the nanometer galapectite pipe and sepiolite powder activated.
Step 3:By foam material, colloidal sol, focus ratio in mass ratio 5:1:0.3 mixing, and stirred at 150 DEG C It is even, obtain mix-froth material;After mix-froth material is aged 12h, after being eluted with water, wet sponge is obtained.
Step 4:Wet sponge is dried using supercritical fluid, obtains sewage water filtration composite sponge.Wherein dried strip Part is:Using carbon dioxide as dried medium, temperature 50 C, pressure 15MPa, time 6h.
The pore capacities of sewage water filtration composite sponge made from the present embodiment are 3.28cm3/G, porosity 80%.
Embodiment 4
The present embodiment and embodiment 1 the difference is that:
In step 1, by polyether polyol, isocyanates, neopelex, carboxymethyl cellulose, tin dilaurate Dibutyl tin and aluminium hydroxide in mass ratio 0.9:1.3:0.015:0.045:0.015:0.15 mixing.
In step 2, by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyethylene Pyrrolidones and water in mass ratio 3.5:1:0.35:0.15:0.75:0.45:100 mixing.
In step 3, by foam material, colloidal sol, focus ratio in mass ratio 3.5:1:0.225 mixing.
The pore capacities of sewage water filtration composite sponge made from the present embodiment are 3.41cm3/ g, porosity 81%.
Embodiment 5
The present embodiment and embodiment 1 the difference is that:
In step 1, by polyether polyol, isocyanates, neopelex, carboxymethyl cellulose, tin dilaurate Dibutyl tin and aluminium hydroxide in mass ratio 1.1:1.5:0.025:0.05:0.025:0.25 mixing.
In step 2, by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyethylene Pyrrolidones and water in mass ratio 4.5:1:0.45:0.25:1.25:0.55:100 mixing.
In step 3, by foam material, colloidal sol, focus ratio in mass ratio 4.5:1:0.275 mixing.
The pore capacities of sewage water filtration composite sponge made from the present embodiment are 3.11cm3/ g, porosity 80%.
Embodiment 6
The present embodiment and embodiment 1 the difference is that:
In step 1, by polyether polyol, isocyanates, neopelex, carboxymethyl cellulose, tin dilaurate Dibutyl tin and aluminium hydroxide in mass ratio 0.9:1.5:0.01:0.06:0.01:0.3 mixing.
In step 2, by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyethylene Pyrrolidones and water in mass ratio 4:1:0.5:0.3:1:0.5:100 mixing.
In step 3, by foam material, colloidal sol, focus ratio in mass ratio 3:1:0.3 mixing.
The pore capacities of sewage water filtration composite sponge made from the present embodiment are 3.48cm3/ g, porosity 80%.
Comparative example 1
The present embodiment and embodiment 1 the difference is that:
In step 1, by polyether polyol, isocyanates, neopelex, carboxymethyl cellulose, tin dilaurate Dibutyl tin and aluminium hydroxide in mass ratio 0.7:1.1:0.01:0.03:0.01:0.1 mixing.
In step 2, by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyethylene Pyrrolidones and water in mass ratio 6:1:0.6:0.4:1.75:0.7:100 mixing.The rate of addition of ammonium hydroxide is 15mL/min.
In step 3, by foam material, colloidal sol, focus ratio in mass ratio 2.5:1:0.15 mixing.
The pore capacities of sewage water filtration composite sponge made from the present embodiment are 2.88cm3/ g, porosity 78%.
Comparative example 2
The present embodiment and embodiment 1 the difference is that:
In step 1, by polyether polyol, isocyanates, neopelex, carboxymethyl cellulose, tin dilaurate Dibutyl tin and aluminium hydroxide in mass ratio 1.3:1.1:0.03:0.05:0.01:0.3 mixing.
In step 2, by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyethylene Pyrrolidones and water in mass ratio 2:1:0.2:0.05:0.25:0.3:100 mixing.The rate of addition of ammonium hydroxide is 35mL/min.
In step 3, by foam material, colloidal sol, focus ratio in mass ratio 5.5:1:0.35 mixing.
The pore capacities of sewage water filtration composite sponge made from the present embodiment are 2.71cm3/ g, porosity 77%.
Comparative example 3
The present embodiment and embodiment 1 the difference is that:
In step 1, by polyether polyol, isocyanates, neopelex, carboxymethyl cellulose, tin dilaurate Dibutyl tin and aluminium hydroxide in mass ratio 1.3:1.7:0.04:0.07:0.04:0.35 mixing.
In step 2, by furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyethylene Pyrrolidones and water in mass ratio 6:1:0.2:0.4:1.75:0.3:100 mixing.The rate of addition of ammonium hydroxide is 15mL/min.
In step 3, by foam material, colloidal sol, focus ratio in mass ratio 5.5:1:0.15 mixing.
The pore capacities of sewage water filtration composite sponge made from the present embodiment are 2.66cm3/ g, porosity 76%.
It was found from the data comparison of embodiment 1-6 and comparative example 1-3, sewage water filtration made from embodiment 1-6 is compound The performance parameter of sponge is more excellent.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the invention, for the skill of this field For art personnel, the invention may be variously modified and varied.Within the spirit and principles of the invention, that is made any repaiies Change, equivalent substitution, improvement etc., should all be included in the protection scope of the present invention.

Claims (6)

1. a kind of preparation method of sewage water filtration composite sponge, it is characterised in that comprise the following steps:
Step 1:By polyether polyol, isocyanates, neopelex, carboxymethyl cellulose, di lauric dibutyl Tin and aluminium hydroxide 0.8-1.2 in mass ratio:1.2-1.6:0.01-0.03:0.04-0.06:0.01-0.03:0.1-0.3 is mixed Uniformly, foaming is stirred at 30-40 DEG C, uncooked foam material is made;
Step 2:By furfural, water soluble phenol resin, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinylpyrrolidine Ketone and water 3-5 in mass ratio:1:0.3-0.5:0.1-0.3:0.5-1.5:0.4-0.6:100 mixing, are mixed after stirring evenly Liquid A is closed, the ammonium hydroxide that concentration is 1mol/L is added drop-wise in mixed liquor A under agitation until the pH value of mixed liquor A is 7-8; Then 16-48h is reacted at 55-65 DEG C, obtains colloidal sol;
Step 3:By foam material, colloidal sol, focus ratio 3-5 in mass ratio:1:0.2-0.3 is mixed, and is stirred at 130-150 DEG C It mixes uniformly, obtains mix-froth material;After mix-froth material is aged 12-24h, after being eluted with water, wet sponge is obtained;
Step 4:Wet sponge is dried using supercritical fluid, obtains sewage water filtration composite sponge;
Wherein, the preparation method of polyether polyol described in step 1 is as follows:By lignin and phenol 1-2 in mass ratio:15-25 It is uniformly mixed, 40-60min is stirred to react at 170-180 DEG C, quality is at the uniform velocity added dropwise during reaction as 1.5 times of phenol Reacting liquid pH value is adjusted to neutrality after reaction, and is cooled to 50-60 DEG C by the sodium hydroxide solution of 10wt%, is added into reaction solution Add the polyalcohol that quality is the formaldehyde of 2-3 times of phenol, quality is 0.25-0.35 times of phenol, finally stirred under heat-retaining condition anti- 40-80min is answered, polyether polyol is made.
A kind of 2. preparation method of sewage water filtration composite sponge according to claim 1, which is characterized in that the polyalcohol For at least one of glycerine, xylitol, sorbierite.
A kind of 3. preparation method of sewage water filtration composite sponge according to claim 1, which is characterized in that the water solubility The solid content of phenolic resin is 40-50%, and free phenol content is less than or equal to 10%.
A kind of 4. preparation method of sewage water filtration composite sponge according to claim 1, which is characterized in that institute in step 2 The rate of addition for stating ammonium hydroxide is 20-30mL/min.
A kind of 5. preparation method of sewage water filtration composite sponge according to claim 1, which is characterized in that the sepiolite Powder and nanometer galapectite pipe pass through activation process:By sepiolite powder and nanometer galapectite pipe respectively in its 400-600 times of quality 4-6h is impregnated in 4wt% hydrochloric acid solutions, the nanometer galapectite pipe and sepiolite powder activated.
A kind of 6. preparation method of sewage water filtration composite sponge according to claim 1, which is characterized in that step 4 condition For:Using carbon dioxide as dried medium, 40-50 DEG C of temperature, pressure 5-15MPa, time 6-24h.
CN201610332926.XA 2016-05-18 2016-05-18 A kind of preparation method of sewage water filtration composite sponge Expired - Fee Related CN105968790B (en)

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

Applications Claiming Priority (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

Publications (2)

Publication Number Publication Date
CN105968790A CN105968790A (en) 2016-09-28
CN105968790B true CN105968790B (en) 2018-06-01

Family

ID=56955282

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610332926.XA Expired - Fee Related CN105968790B (en) 2016-05-18 2016-05-18 A kind of preparation method of sewage water filtration composite sponge

Country Status (1)

Country Link
CN (1) CN105968790B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN111040125B (en) * 2019-12-27 2022-01-28 陕西科技大学 Composite fulvic acid antibacterial sponge matrix and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4445352B2 (en) * 2004-09-01 2010-04-07 秀樹 原田 Purification zone manufacturing method, purification zone, and purification zone assembly
CN103599734A (en) * 2013-11-22 2014-02-26 中国工程物理研究院核物理与化学研究所 Aerogel material and preparation method thereof
CN103641991A (en) * 2013-11-13 2014-03-19 安徽金马海绵有限公司 High elasticity sponge and production method
CN104174358A (en) * 2014-08-11 2014-12-03 南京信息工程大学 Reticular nitrogenous carbon adsorbent material as well as preparation method and application thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4445352B2 (en) * 2004-09-01 2010-04-07 秀樹 原田 Purification zone manufacturing method, purification zone, and purification zone assembly
CN103641991A (en) * 2013-11-13 2014-03-19 安徽金马海绵有限公司 High elasticity sponge and production method
CN103599734A (en) * 2013-11-22 2014-02-26 中国工程物理研究院核物理与化学研究所 Aerogel material and preparation method thereof
CN104174358A (en) * 2014-08-11 2014-12-03 南京信息工程大学 Reticular nitrogenous carbon adsorbent material as well as preparation method and application thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Facile synthesis of sponge reinforced monolithic silica aerogels with improved mechanical property and excellent absorptivity;He Song等;《materials letters》;20150901;第154卷;第107-111页 *
聚氨酯纳米复合泡沫的制备及表征研究;孙德文;《中国博士学位论文全文数据库工程科技I辑》;20120115(第01期);B020-48 *

Also Published As

Publication number Publication date
CN105968790A (en) 2016-09-28

Similar Documents

Publication Publication Date Title
Ngah et al. Adsorption of dyes and heavy metal ions by chitosan composites: A review
CN105800724B (en) A kind of preparation method of aerogel type purifying agent for polluted water
CN105797694B (en) A kind of preparation method of recyclable water quality cleansing agent
CN105968790B (en) A kind of preparation method of sewage water filtration composite sponge
CN101077795A (en) Composite biological adsorption and preparing method thereof
CN105413629A (en) Alga-calcium-mineral air purification medium and preparation method and application thereof
CN112958090B (en) Efficient and stable iron-copper montmorillonite heterogeneous Fenton catalyst and preparation method and application thereof
US6129846A (en) Activated carbon composite with crystalline tin silicate
US20210002817A1 (en) Ceramic coated antibacterial fabric, and method for manufacturing the same
CN111437778A (en) Amino modified microcrystalline cellulose/graphene oxide aerogel and preparation method and application thereof
CN113861772A (en) Anti-formaldehyde coating and preparation method thereof
CN114015326A (en) Formaldehyde-removing environment-friendly new material and preparation method thereof
CN110256735A (en) A kind of amidoxim-azanol oxime cellulose/nanometer silver/chitosan composite aerogel preparation method
CN112604670A (en) Cellulose-based composite aerogel for sewage treatment
CN115090319B (en) Ozone catalyst and preparation method and application thereof
CN114700065B (en) Waste resin carbon sphere composite ozone catalyst and preparation method and application thereof
CN106276895A (en) A kind of preparation method of amberlite aliphatic radical material with carbon element
CN106000078A (en) Air purifying wallpaper
CN105921122A (en) Preparation method of granular sewage purifying agent
CN114702723A (en) Method for preparing cellulose composite aerogel by using reed as raw material
CN108772050B (en) Adsorbent, preparation method and application thereof
CN115055174B (en) Ca-based ozone catalytic oxidation catalyst for advanced treatment of salt-containing organic wastewater and preparation method thereof
CN110639542B (en) In-situ hybridization room-temperature formaldehyde removal catalyst, composite gel, and preparation method and application thereof
CN105778670A (en) Environment-friendly polyvinyl acetate emulsion paint and preparation method thereof
CN112158853A (en) Tubular free radical oxidant and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
TA01 Transfer of patent application right

Effective date of registration: 20180504

Address after: 331100 No. 2 Torch Road, Fengcheng high tech Industrial Park, Yichun, Jiangxi

Applicant after: Jiangxi Province Ao Tailv gardens sponge Co.,Ltd.

Address before: 410015 No. 102, Bront District, Hester moonlight estate, 118 Zheng Xing Road, Lei Feng Town, Changsha high tech Development Zone, Changsha, Hunan, China.

Applicant before: HUNAN XIXIN INFORMATION TECHNOLOGY Co.,Ltd.

TA01 Transfer of patent application right
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right

Effective date of registration: 20211201

Address after: 332005 No. 798, Lianxi Avenue, Lianxi District, Jiujiang City, Jiangxi Province

Patentee after: Guoke Technology Innovation Center (Jiujiang) Co.,Ltd.

Address before: 331100 No. 2 Torch Road, Fengcheng high tech Industrial Park, Yichun, Jiangxi

Patentee before: Jiangxi Province Ao Tailv gardens sponge Co.,Ltd.

TR01 Transfer of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20180601

CF01 Termination of patent right due to non-payment of annual fee