CN105797694A - Recyclable water purifying agent preparation method - Google Patents

Recyclable water purifying agent preparation method Download PDF

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CN105797694A
CN105797694A CN201610367496.5A CN201610367496A CN105797694A CN 105797694 A CN105797694 A CN 105797694A CN 201610367496 A CN201610367496 A CN 201610367496A CN 105797694 A CN105797694 A CN 105797694A
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sol
mixed
recyclable water
water quality
cleansing agent
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CN105797694B (en
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不公告发明人
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Nanjing Lanting Green Building Technology Co ltd
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/288Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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    • C02F1/48Treatment of water, waste water, or sewage with magnetic or electric fields
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/50Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
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Abstract

The invention provides a recyclable water purifying agent preparation method. The method includes: step 1, mixing polyether polyol, isocyanate, sodium dodecyl benzene sulfonate, carboxymethyl cellulose, dibutyltin dilaurate, aluminium hydroxide and ferroferric oxide magnetic powder to obtain a foam material; step 2, mixing butyl titanate, sepiolite powder, halloysite nanotubes, nanocrystalline cellulose, polyvinylpyrrolidone, ferroferric oxide magnetic powder and absolute ethyl alcohol to obtain a mixed liquid A; mixing a hydrochloric acid solution, absolute ethyl alcohol and water to obtain a mixed liquid B; dropwise adding the mixed liquid B into the mixed liquid A, and reacting to obtain sol; subjecting the sol to silver loading treatment; step 3, mixing the foam material, the silver-loaded sol and phenoxy resin to obtain a mixed foam material; ageing and cleaning to obtain wet sponge; step 4, drying and grinding the wet sponge to obtain a recyclable water purifying agent. The recyclable water purifying agent prepared according to the method is effective in adsorption, high in adsorption capacity, high in efficiency and recyclability.

Description

A kind of preparation method of recyclable water quality cleansing agent
Technical field
The present invention relates to technical field of water purification, especially, the preparation method relating to a kind of recyclable water quality cleansing agent.
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, it is common to there is the situation that the sewage after will not pass through purification directly discharges.The environmental disruption of many decades, causes the most of rivers,lakes and seas water quality serious deterioration of current China, containing substantial amounts of graininess impurity, oil system pollutant, heavy metal and Eutrophication materials etc. in the water body of these natural stream networks.
At present, for the improvement of natural water source, generally there are the methods such as artificial salvaging, ecological management, cleanser purification in China.Artificial salvaging is wasted time and energy, and the ecological management cycle is long, and effect is notable not, and cleanser adsorbs, flocculating effect is poor, is not easily recycled.The Chinese patent that such as Authorization Notice No. is CN101928069B discloses a kind of purifying agent for polluted water, it is made up of PHA, kieselguhr, humic acid, bioactivator, inorganic metal salt and other materials, 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 completely biodegradable material is slowly degraded and release bioactive agent, it is achieved the long-term high-efficient purification function of bioactivator.And in conjunction with the aquatic plant combined effect purified treatment to realizing sewage phosphorus, nitrogen, polycyclic aromatic hydrocarbon, heavy metal.
Except above-mentioned purifying agent for polluted water, also having the purifying agent for polluted water being main material with activated carbon in a large number in the market, its principle is that water body is purified by the adsorptivity utilizing activated carbon.
But above-mentioned water purification agent is limited to the clean-up effect of sewage, and the adsorption effect of impurity is poor, adsorption capacity is low, and the clarification time is long, inefficiency;And be not easily recycled.
Summary of the invention
Present invention aim at the preparation method providing a kind of recyclable water quality cleansing agent, poor to solve purifying agent for polluted water adsorption effect in prior art, 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 recyclable water quality cleansing agent, comprise the following steps:
Step 1: by polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, dibutyl tin laurate, aluminium hydroxide and ferroferric oxide magnetic powder 0.8-1.2:1.2-1.6:0.01-0.03:0.04-0.06:0.01-0.03:0.1-0.3:0. 01-0.03 mix homogeneously in mass ratio, at 30-40 DEG C, it is stirred foaming, prepares the foam material of non-ripening.
Step 2: butyl titanate, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinylpyrrolidone, ferroferric oxide magnetic powder and dehydrated alcohol 1:0.04-0.06:0.04-0.06:0.01-0.03:0.03-0.05:30-50:0.01-0.0 3 in mass ratio are mixed, obtains mixed liquor A;The hydrochloric acid solution of 3mol/L, dehydrated alcohol are mixed with water 3-5:5-15:5 by volume, obtains mixed liquid B;Under agitation mixed liquid B is added drop-wise in isopyknic mixed liquor A;Then at 50-60 DEG C, react 8-16h, obtain colloidal sol;Sol impregnation and is stirred in the silver nitrate solution that concentration is 0.25mol/L of 10-15 times of volume, lucifuge heating 2-3h at 50-60 DEG C, take out colloidal sol, by sol impregnation in the citric acid three sodium solution of 10-15 times of 0.5mol/L, at 80-90 DEG C, react 3-4h;After finally colloidal sol being taken out and washed, obtain load silver sol.
Step 3: by foam material, load silver sol, focus ratio 3-5:1:0.2-0.3 in mass ratio mixing, and stir at 130-150 DEG C, obtain mix-froth material;After mix-froth material ageing 12-24h, after washing, obtain wet sponge.
Step 4: adopt supercritical fluid that wet sponge is dried, after being ground into granule, obtain recyclable water quality cleansing agent.
In the inventive solutions, not using traditional flocculant or activated carbon as main component, change into and adopt the water quality cleansing agent being main base with polyurethane material and titania aerogel.Compared with activated carbon, this water quality cleansing agent has better adsorption capacity and the duct of sizes rank, pore size in polyurethane foamed material is bigger, the impurity of particulate species can be carried out active adsorption, pore size in titania aerogel is less, it is possible to the material such as heavy metal, pigment adsorbs.Therefore higher for the adsorptivity of the polluter of different size, kind in water.In the preparation process of foam material, dodecylbenzene sodium sulfonate plays foaming effect, carboxymethyl cellulose can increase the degree of cross linking, dibutyl tin laurate plays catalytic action, aluminium hydroxide can thermally decompose more than 130 DEG C, producing Alpha-alumina and steam, steam plays pore effect after escaping.Ferroferric oxide magnetic powder is coated in material so that by the natural waters such as water quality cleansing agent input and rivers,lakes and seas, after the purification of certain time, it is possible to reclaimed by magnetic field.
Titanium dioxide has stronger photo-catalysis capability under light illumination, after being loaded with silver, it is possible to work in coordination, and the harmful microorganism in water body, Organic substance can be degraded.After adsorbed mass degradation, release a large amount of internal capacity of water quality cleansing agent, indirectly improve adsorption capacity.
And in traditional aeroge preparation process, prepare in the process of aeroge at gel through super-dry, owing to the intensity of its internal three-dimensional net structure is not high, original structure is easily caved in, cause that porosity and specific surface area reduce, and material fragility is higher after molding, mechanical strength, toughness, poor water resistance, have a strong impact on practical application.The titania aerogel material of the present invention, with titanium dioxide-meerschaum-nanometer galapectite pipe-cellulosic composite of nano-crystal for matrix, wherein meerschaum has the hole of nano-scale, and the material such as pigment, heavy metal ion is had very strong absorbability;Nanometer galapectite pipe is the chopped fiber tubulose with hollow structure, there is the duct of nano-scale, the intensity of material can be greatly improved after preparing titania aerogel, and the toughness of titania aerogel material can also be improved simultaneously, existence due to meerschaum, nanometer galapectite pipe, can play a supporting role in titania aerogel material dry run, three-dimensional net structure in titania aerogel not easily caves in, thus pore structure when keeping collosol state and specific surface area.Further, owing to meerschaum, nanometer galapectite pipe self also have nano pore, it may have strong adsorptivity, therefore, it is possible to make up by meerschaum, nanometer hole that the space that galapectite pipe occupies is lost.Nano-crystal cellulose not only self can the heavy metal ion such as Adsorption of Lead, chromium, and the combination of each material can be assisted when preparing colloidal sol;Polyvinylpyrrolidone is as porogen, it is possible to make the duct of micron level, the pore size of abundant recyclable water quality cleansing agent such that it is able to each pollutant is adsorbed.
Wherein in process foam material, colloidal sol mixed, being added with focus ratio, focus ratio not only has adhesive effect, and it can improve the resistance to water of composite, mechanical strength and resistance to contractility.Enable to recyclable water quality cleansing agent for a long time at underwater work.
Further, the preparation method of polyether polyol described in step 1 is as follows: mixed homogeneously with phenol 1-2:15-25 in mass ratio by lignin, stirring reaction 40-60min at 170-180 DEG C, the sodium hydroxide solution of the 10wt% that quality is phenol 1.5 times is at the uniform velocity dripped during reaction, after reaction, reacting liquid pH value is adjusted to neutrality, and it is cooled to 50-60 DEG C, quality is added to be the formaldehyde of phenol 2-3 times, quality is the polyhydric alcohol of phenol 0.25-0.35 times in reactant liquor, last stirring reaction 40-80min under heat-retaining condition, prepares polyether polyol.
Further, described polyhydric alcohol is at least one in glycerol, xylitol, sorbitol.
Further, the rate of addition of mixed liquid B described in step 2 is 15-20mL/min.
Further, described sepiolite powder and nanometer galapectite pipe are through activation processing: sepiolite powder and nanometer galapectite pipe are soaked 4-6h respectively in the 4wt% hydrochloric acid solution of its 400-600 times of quality, obtains nanometer galapectite pipe and the sepiolite powder of activation.
A nanometer galapectite pipe is carried out acid activation process, it is possible to increase the adsorption efficiency of himself, it is possible to increase the adsorption efficiency of recyclable water quality cleansing agent.
Further, step 4 condition is: adopt carbon dioxide as dry medium, temperature 40-50 DEG C, pressure 5-15MPa, time 6-24h.
The method have the advantages that
Recyclable water quality cleansing agent prepared by the inventive method, has multistage pore canal, and to the dirt advantages of good adsorption effect in water body, adsorption capacity is big, the feature that adsorption efficiency is high.Additionally, it is additionally favorable for reclaiming, it is possible to prevent water quality to be secondary polluted.
Except purpose described above, feature and advantage, the present invention also has other purpose, feature and advantage.The present invention is further detailed explanation below.
Detailed description of the invention
Hereinafter embodiments of the invention are described in detail, but the multitude of different ways that the present invention can limit according to claim and cover is implemented.
Embodiment 1
The preparation method of a kind of recyclable water quality cleansing agent, comprises the following steps:
Step 1: lignin is mixed homogeneously with phenol 1.5:20 in mass ratio, stirring reaction 50min at 175 DEG C, the sodium hydroxide solution of the 10wt% that quality is phenol 1.5 times is at the uniform velocity dripped during reaction, after reaction, reacting liquid pH value is adjusted to neutrality, and it is cooled to 55 DEG C, in reactant liquor, add quality to be the formaldehyde of phenol 2.5 times, quality be the glycerol of phenol 0.3 times, finally stirring reaction 60min under heat-retaining condition, prepare polyether polyol.
By polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, dibutyl tin laurate, aluminium hydroxide and ferroferric oxide magnetic powder 1:1.4:0.02:0.05:0.02:0.2:0.02 mix homogeneously in mass ratio, at 35 DEG C, it is stirred foaming, prepares the foam material of non-ripening.
Step 2: butyl titanate, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinylpyrrolidone, ferroferric oxide magnetic powder and dehydrated alcohol 1:0.05:0.05:0.02:0.04:40:0.02 in mass ratio are mixed, obtains mixed liquor A;The hydrochloric acid solution of 3mol/L, dehydrated alcohol are mixed with water 4:10:5 by volume, obtains mixed liquid B;Under agitation mixed liquid B is added drop-wise in isopyknic mixed liquor A with the rate of addition of 18mL/min;Then at 55 DEG C, react 12h, obtain colloidal sol;And being stirred in the silver nitrate solution that concentration is 0.25mol/L of 12 times of volumes by sol impregnation, at 55 DEG C, lucifuge heating 2.5h, takes out colloidal sol, by sol impregnation in the citric acid three sodium solution of 12.5 times of 0.5mol/L, reacts 3.5h at 85 DEG C;After finally colloidal sol being taken out and washed, obtain load silver sol.
Wherein said sepiolite powder and nanometer galapectite pipe are through activation processing: sepiolite powder and nanometer galapectite pipe are soaked 5h respectively in the 4wt% hydrochloric acid solution of its 500 times of quality, obtains nanometer galapectite pipe and the sepiolite powder of activation.
Step 3: by foam material, load silver sol, focus ratio 4:1:0.25 in mass ratio mixing, and stir at 140 DEG C, obtain mix-froth material;After mix-froth material ageing 18h, after washing, obtain wet sponge.
Step 4: adopt supercritical fluid that wet sponge is dried, after being ground into granule, obtain recyclable water quality cleansing agent.Wherein drying condition is: adopt carbon dioxide as dry medium, temperature 45 C, pressure 10MPa, time 15h.
The pore capacities of the recyclable water quality cleansing agent that the present embodiment prepares is 3.31cm3/ g, porosity is 81%.
Embodiment 2
The preparation method of a kind of recyclable water quality cleansing agent, comprises the following steps:
Step 1: lignin is mixed homogeneously with phenol 1:15 in mass ratio, stirring reaction 60min at 170 DEG C, the sodium hydroxide solution of the 10wt% that quality is phenol 1.5 times is at the uniform velocity dripped during reaction, after reaction, reacting liquid pH value is adjusted to neutrality, and it is cooled to 50 DEG C, add quality in reactant liquor to be the formaldehyde of phenol 2 times, quality be the glycerol of phenol 0.15 times, quality is the sorbitol of phenol 0.1 times, finally stirring reaction 40min under heat-retaining condition, prepares polyether polyol.
By polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, dibutyl tin laurate, aluminium hydroxide and ferroferric oxide magnetic powder 0.8:1.2:0.01:0.04:0.01:0.1:0.01 mix homogeneously in mass ratio, at 30 DEG C, it is stirred foaming, prepares the foam material of non-ripening.
Step 2: butyl titanate, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinylpyrrolidone, ferroferric oxide magnetic powder and dehydrated alcohol 1:0.04:0.04:0.01:0.03:30:0.01 in mass ratio are mixed, obtains mixed liquor A;The hydrochloric acid solution of 3mol/L, dehydrated alcohol are mixed with water 3:5:5 by volume, obtains mixed liquid B;Under agitation mixed liquid B is added drop-wise in isopyknic mixed liquor A with the rate of addition of 15mL/min;Then at 50 DEG C, react 8h, obtain colloidal sol;And being stirred in the silver nitrate solution that concentration is 0.25mol/L of 10 times of volumes by sol impregnation, at 50 DEG C, lucifuge heating 3h, takes out colloidal sol, by sol impregnation in the citric acid three sodium solution of 10 times of 0.5mol/L, reacts 4h at 80 DEG C;After finally colloidal sol being taken out and washed, obtain load silver sol.
Wherein said sepiolite powder and nanometer galapectite pipe are through activation processing: sepiolite powder and nanometer galapectite pipe are soaked 6h respectively in the 4wt% hydrochloric acid solution of its 400 times of quality, obtains nanometer galapectite pipe and the sepiolite powder of activation.
Step 3: by foam material, load silver sol, focus ratio 3:1:0.2 in mass ratio mixing, and stir at 13 DEG C, obtain mix-froth material;After mix-froth material ageing 24h, after washing, obtain wet sponge.
Step 4: adopt supercritical fluid that wet sponge is dried, after being ground into granule, obtain recyclable water quality cleansing agent.Wherein drying condition is: adopt carbon dioxide as dry medium, temperature 40 DEG C, pressure 5MPa, time 24h.
The pore capacities of the recyclable water quality cleansing agent that the present embodiment prepares is 3.13cm3/ g, porosity is 79%.
Embodiment 3
The preparation method of a kind of recyclable water quality cleansing agent, comprises the following steps:
Step 1: lignin is mixed homogeneously with phenol 2:25 in mass ratio, stirring reaction 40min at 180 DEG C, the sodium hydroxide solution of the 10wt% that quality is phenol 1.5 times is at the uniform velocity dripped during reaction, after reaction, reacting liquid pH value is adjusted to neutrality, and it is cooled to 60 DEG C, in reactant liquor, add quality to be the formaldehyde of phenol 3 times, quality be the sorbitol of phenol 0.35 times, finally stirring reaction 80min under heat-retaining condition, prepare polyether polyol.
By polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, dibutyl tin laurate, aluminium hydroxide and ferroferric oxide magnetic powder 1.2:1.6:0.03:0.06:0.03:0.3:0.03 mix homogeneously in mass ratio, at 40 DEG C, it is stirred foaming, prepares the foam material of non-ripening.
Step 2: butyl titanate, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinylpyrrolidone, ferroferric oxide magnetic powder and dehydrated alcohol 1:0.06:0.06:0.03:0.05:50:0.03 in mass ratio are mixed, obtains mixed liquor A;The hydrochloric acid solution of 3mol/L, dehydrated alcohol are mixed with water 5:15:5 by volume, obtains mixed liquid B;Under agitation mixed liquid B is added drop-wise in isopyknic mixed liquor A with the rate of addition of 20mL/min;Then at 60 DEG C, react 8h, obtain colloidal sol;And being stirred in the silver nitrate solution that concentration is 0.25mol/L of 15 times of volumes by sol impregnation, at 60 DEG C, lucifuge heating 2h, takes out colloidal sol, by sol impregnation in the citric acid three sodium solution of 15 times of 0.5mol/L, reacts 3h at 90 DEG C;After finally colloidal sol being taken out and washed, obtain load silver sol.
Wherein said sepiolite powder and nanometer galapectite pipe are through activation processing: sepiolite powder and nanometer galapectite pipe are soaked 4h respectively in the 4wt% hydrochloric acid solution of its 600 times of quality, obtains nanometer galapectite pipe and the sepiolite powder of activation.
Step 3: by foam material, load silver sol, focus ratio 5:1:0.3 in mass ratio mixing, and stir at 150 DEG C, obtain mix-froth material;After mix-froth material ageing 12h, after washing, obtain wet sponge.
Step 4: adopt supercritical fluid that wet sponge is dried, after being ground into granule, obtain recyclable water quality cleansing agent.Wherein drying condition is: adopt carbon dioxide as dry medium, temperature 50 C, pressure 15MPa, time 6h.
The pore capacities of the recyclable water quality cleansing agent that the present embodiment prepares is 3.06cm3/ g, porosity is 80%.
Embodiment 4
The present embodiment and embodiment 1 are different in that:
In step 1, polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, dibutyl tin laurate, aluminium hydroxide and ferroferric oxide magnetic powder 0.9:1.3:0.015:0.045:0.015:0.15:0.015 in mass ratio is mixed.
In step 2, butyl titanate, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinylpyrrolidone, ferroferric oxide magnetic powder and dehydrated alcohol 1:0.045:0.045:0.015:0.035:35:0.015 in mass ratio are mixed.
In step 3, by foam material, load silver sol, focus ratio 3.5:1:0.225 in mass ratio mixing.
The pore capacities of the recyclable water quality cleansing agent that the present embodiment prepares is 3.01cm3/ g, porosity is 79%.
Embodiment 5
The present embodiment and embodiment 1 are different in that:
In step 1, polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, dibutyl tin laurate, aluminium hydroxide and ferroferric oxide magnetic powder 1.1:1.5:0.025:0.055:0.025:0.25:0.025 in mass ratio is mixed.
In step 2, butyl titanate, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinylpyrrolidone, ferroferric oxide magnetic powder and dehydrated alcohol 1:0.055:0.055:0.025:0.045:45:0.025 in mass ratio are mixed.
In step 3, by foam material, load silver sol, focus ratio 4.5:1:0.275 in mass ratio mixing.
The pore capacities of the recyclable water quality cleansing agent that the present embodiment prepares is 2.97cm3/ g, porosity is 79%.
Embodiment 6
The present embodiment and embodiment 1 are different in that:
In step 1, polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, dibutyl tin laurate, aluminium hydroxide and ferroferric oxide magnetic powder 0.9:1.5:0.01:0.06:0.02:0.2:0.02 in mass ratio is mixed.
In step 2, butyl titanate, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinylpyrrolidone, ferroferric oxide magnetic powder and dehydrated alcohol 1:0.04:0.06:0.01:0.05:35:0.02 in mass ratio are mixed.
In step 3, by foam material, load silver sol, focus ratio 3:1:0.3 in mass ratio mixing.
The pore capacities of the recyclable water quality cleansing agent that the present embodiment prepares is 3.03cm3/ g, porosity is 79%.
Comparative example 1
The present embodiment and embodiment 1 are different in that:
In step 1, polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, dibutyl tin laurate, aluminium hydroxide and ferroferric oxide magnetic powder 0.7:1.1:0.01:0.03:0.01:0.1:0.01 in mass ratio is mixed.
In step 2, butyl titanate, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinylpyrrolidone, ferroferric oxide magnetic powder and dehydrated alcohol 1:0.03:0.03:0.01:0.02:25:0.01 in mass ratio are mixed.
In step 3, by foam material, load silver sol, focus ratio 2.5:1:0.15 in mass ratio mixing.
The pore capacities of the recyclable water quality cleansing agent that the present embodiment prepares is 2.65cm3/ g, porosity is 76%.
Comparative example 2
The present embodiment and embodiment 1 are different in that:
In step 1, polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, dibutyl tin laurate, aluminium hydroxide and ferroferric oxide magnetic powder 1.3:1.7:0.04:0.07:0.04:0.35:0.04 in mass ratio is mixed.
In step 2, butyl titanate, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinylpyrrolidone, ferroferric oxide magnetic powder and dehydrated alcohol 1:0.07:0.07:0.04:0.06:55:0.04 in mass ratio are mixed.
In step 3, by foam material, load silver sol, focus ratio 5.51:.35 in mass ratio mixing.
The pore capacities of the recyclable water quality cleansing agent that the present embodiment prepares is 249cm3/ g, porosity is 75%.
Comparative example 3
The present embodiment and embodiment 1 are different in that:
In step 1, polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, dibutyl tin laurate, aluminium hydroxide and ferroferric oxide magnetic powder 0.7:1.7:0.01:0.07:0.01:0.4:0.01 in mass ratio is mixed.
In step 2, butyl titanate, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinylpyrrolidone, ferroferric oxide magnetic powder and dehydrated alcohol 1:0.03:0.07:0.01:0.06:25:0.04 in mass ratio are mixed.
In step 3, by foam material, load silver sol, focus ratio 2.5:1:0.4 in mass ratio mixing.
The pore capacities of the recyclable water quality cleansing agent that the present embodiment prepares is 2.36cm3/ g, porosity is 74%.
From the Data Comparison of embodiment 1-6 and comparative example 1-3 it can be seen that the performance parameter of recyclable water quality cleansing agent for preparing of embodiment 1-6 is more excellent.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.

Claims (6)

1. the preparation method of a recyclable water quality cleansing agent, it is characterised in that comprise the following steps:
Step 1: by polyether polyol, isocyanates, dodecylbenzene sodium sulfonate, carboxymethyl cellulose, dibutyl tin laurate, aluminium hydroxide and ferroferric oxide magnetic powder 0.8-1.2:1.2-1.6:0.01-0.03:0.04-0.06:0.01-0.03:0.1-0.3:0. 01-0.03 mix homogeneously in mass ratio, at 30-40 DEG C, it is stirred foaming, prepares the foam material of non-ripening;
Step 2: butyl titanate, sepiolite powder, nanometer galapectite pipe, nano-crystal cellulose, polyvinylpyrrolidone, ferroferric oxide magnetic powder and dehydrated alcohol 1:0.04-0.06:0.04-0.06:0.01-0.03:0.03-0.05:30-50:0.01-0.0 3 in mass ratio are mixed, obtains mixed liquor A;The hydrochloric acid solution of 3mol/L, dehydrated alcohol are mixed with water 3-5:5-15:5 by volume, obtains mixed liquid B;Under agitation mixed liquid B is added drop-wise in isopyknic mixed liquor A;Then at 50-60 DEG C, react 8-16h, obtain colloidal sol;Sol impregnation and is stirred in the silver nitrate solution that concentration is 0.25mol/L of 10-15 times of volume, lucifuge heating 2-3h at 50-60 DEG C, take out colloidal sol, by sol impregnation in the citric acid three sodium solution of 10-15 times of 0.5mol/L, at 80-90 DEG C, react 3-4h;After finally colloidal sol being taken out and washed, obtain load silver sol;
Step 3: by foam material, load silver sol, focus ratio 3-5:1:0.2-0.3 in mass ratio mixing, and stir at 130-150 DEG C, obtain mix-froth material;After mix-froth material ageing 12-24h, after washing, obtain wet sponge;
Step 4: adopt supercritical fluid that wet sponge is dried, after being ground into granule, obtain recyclable water quality cleansing agent.
2. the preparation method of a kind of recyclable water quality cleansing agent according to claim 1, it is characterized in that, the preparation method of polyether polyol described in step 1 is as follows: mixed homogeneously with phenol 1-2:15-25 in mass ratio by lignin, stirring reaction 40-60min at 170-180 DEG C, the sodium hydroxide solution of the 10wt% that quality is phenol 1.5 times is at the uniform velocity dripped during reaction, after reaction, reacting liquid pH value is adjusted to neutrality, and it is cooled to 50-60 DEG C, the formaldehyde that quality is phenol 2-3 times is added in reactant liquor, quality is the polyhydric alcohol of phenol 0.25-0.35 times, last stirring reaction 40-80min under heat-retaining condition, prepare polyether polyol.
3. the preparation method of a kind of recyclable water quality cleansing agent according to claim 2, it is characterised in that described polyhydric alcohol is at least one in glycerol, xylitol, sorbitol.
4. the preparation method of a kind of recyclable water quality cleansing agent as claimed in claim 1, it is characterised in that the rate of addition of mixed liquid B described in step 2 is 15-20mL/min.
5. the preparation method of a kind of recyclable water quality cleansing agent according to claim 1, it is characterized in that, described sepiolite powder and nanometer galapectite pipe are through activation processing: sepiolite powder and nanometer galapectite pipe are soaked 4-6h respectively in the 4wt% hydrochloric acid solution of its 400-600 times of quality, obtains nanometer galapectite pipe and the sepiolite powder of activation.
6. the preparation method of a kind of recyclable water quality cleansing agent according to claim 1, it is characterised in that step 4 condition is: adopt carbon dioxide as dry medium, temperature 40-50 DEG C, pressure 5-15MPa, time 6-24h.
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