CN105949519A - Preparation method of nano-zinc oxide cellulose sponge material - Google Patents
Preparation method of nano-zinc oxide cellulose sponge material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/05—Derivatives containing elements other than carbon, hydrogen, oxygen, halogens or sulfur
- C08B15/06—Derivatives containing elements other than carbon, hydrogen, oxygen, halogens or sulfur containing nitrogen, e.g. carbamates
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/08—Cellulose derivatives
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- C09K3/00—Materials not provided for elsewhere
- C09K3/32—Materials not provided for elsewhere for absorbing liquids to remove pollution, e.g. oil, gasoline, fat
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
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- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
Abstract
Belonging to the field of nano-material synthesis, the invention discloses a preparation method of a nano-zinc oxide cellulose sponge material. The method includes: adopting hemp stem fiber as the raw material, using a NaOH solution to swell the fiber, then using saturated steam pressurization to split cellulose into smaller fibers, then reacting N, N'-carbonyldiimidazole with cellulose to generate high activity cellulose, adding a KH-550 silane coupling agent to graft nano-zinc oxide to a high activity cellulose surface, then using absorbent cotton as the reinforcing fiber, taking sodium sulfate as the pore-forming agent, and using a NaOH/thiourea solution as the solvent, and carrying out die molding to prepare a nano-zinc oxide cellulose sponge material under low temperature and dry conditions. The obtained nano-zinc oxide cellulose sponge material has a sponge porous structure, the cellulose composing the sponge structure is easily degradable and does not cause secondary pollution, also the complex nano-zinc oxide bulge structure on the surface can realize reversible conversion of surface super-hydrophobicity and super-hydrophilicity, thus realizing adsorption and removal of oil.
Description
Technical field
The invention discloses the preparation method of a kind of nano zinc oxide fiber element sponge material, belong to nano material synthesis field.
Background technology
In recent years, along with petroleum industry and the fast development of oil transportation at sea, the Crude oil from CNOOC leakage that blowout, shipwreck etc. cause be relatively common in environmental pollution be also pollution problem difficult to deal with.Oil absorption material is a kind of very effective marine oil spill processing method, has the advantages such as efficient, economy and oil product easily recovery, is widely used in marine oil spill contamination accident emergency processing.
Oil absorption material currently mainly has following several: natural inorganic oil absorption material, natural organic oil absorption material and chemosynthesis class oil absorption material, the common active charcoal of natural inorganic oil absorption material, zeolite, perlite, clay and graphite etc., this kind of material is typically in granular form or loose porous structure, low price, material is easy to get, but the shortcomings such as it is poor that major part material exists oil-water selectivity, and saturated oil absorption is low, regeneration difficulty；Natural organic oil absorption material includes Caulis et Folium Oryzae, straw, bark and peat bog etc., and this kind of material has the advantages such as cheap and easy to get and biodegradable, but it is poor to there is oil-water selectivity, the shortcoming that the low suspension of saturated oil absorption is poor.And chemical classes synthetic material lipophilic-hydrophobic property is good, oil absorption highlights, but biological degradability is poor.
Summary of the invention
nullThe technical problem that present invention mainly solves: in use occur for current oil absorption material，Regeneration difficulty，Ability capable of circulation and biological degradability are poor，Apply the requirement being extremely difficult to quick Environment control in excessive trip incident processing procedure，The problem being simultaneously likely to result in secondary pollution，Provide the preparation method of a kind of nano zinc oxide fiber element sponge material，The present invention uses boony fibre to be raw material，First processing by NaOH solution makes fiber swelling，Increase fiber surface roughness，Recycling saturated vapor pressurization makes cellulose be further split into less fiber，Recycling N,N '-carbonyl dimidazoles and fibrin reaction，Generate the high activity cellulose with imidazole ring，Add KH-550 silane coupler，The nano zine oxide making reaction generate grafts on high activity cellulose surface，Recycling absorbent cotton is as reinforcing fiber，Sodium sulfate is pore former，NaOH/ thiourea solution is solvent，After after mould molding，Nano zinc oxide fiber element sponge material is prepared under the conditions of cold drying.Gained nano zinc oxide fiber element sponge material possesses the loose structure of sponge, the cellulose constituting sponge structure is degradable, secondary pollution will not be produced, and the nano zine oxide bulge-structure of its surface complexity can realize surface super hydrophobic and super hydrophilic reversible transformation under illumination and dark condition, thus realize absorption and the removing of oil product.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is:
(1) weighing 80～100g boony fibres, being placed in 180～200mL mass concentrations is in 10～15%NaOH solution, after soaking 1～3h, it is washed with deionized 3～5 times, being proceeded to reactor again, start agitator, setting speed is 600～800r/min, it is passed through saturated vapor to reactor, until reacting kettle inner pressure reaches 1.5～1.8MPa, after pressurize 20～30min, material in reactor is proceeded in 105～110 DEG C of baking ovens, dry to constant weight, obtain alkali cellulose siccative；
(2) weigh 30～50g above-mentioned alkali cellulose siccatives and 20～40gN, N '-carbonyl dimidazoles respectively, join and fill 30～36mL toluene, in the there-necked flask of the belt stirrer of 20～24mL dimethyl fumarates, it is placed on again in 55～75 DEG C of thermostat water baths, starts agitator, with 500～700r/min constant temperature stirrings 3～5h, sucking filtration, it is washed with deionized filter cake 3～5 times, filter cake is proceeded in 90～105 DEG C of baking ovens, be dried 3～5h, obtain activated cellulose, standby；
(3) measuring 90～100mL concentration is 0.4～0.8mol/LNaOH solution, pass through Dropping funnel, dropwise drop to fill in the there-necked flask that 60～80mL concentration are 0.3～0.5mol/L solution of zinc sulfate, under 60～80 DEG C of waters bath with thermostatic control and 600～800r/min stirrings, control rate of addition so that it is in 1.5～3h, dropping is complete；
(4) after waiting to drip, add 2～4mLKH-550 silane couplers, continue constant temperature stirring reaction 3～5h, again step (2) standby activated cellulose is added in there-necked flask, continue constant temperature stirring reaction 3～5h, sucking filtration, it is washed with deionized filter cake 3～5 times, again filter cake is proceeded in 100～105 DEG C of baking ovens, be dried 2～4h, obtain nano zinc oxide fiber element siccative；
(5) 30～50g above-mentioned nano zinc oxide fiber element siccatives, 10～20g a length of 5～10mm are weighed successively
Absorbent cotton particle and 3～5gNa2SO4Powder, adding fills in the beaker that 150～200mL mass concentrations are 8～12%NaOH/ thiourea solutions, it is placed on again in sonic oscillation instrument, after vibration 10～20min, obtain uniform sizing material, then measure 60～80mL above-mentioned uniform sizing materials, pour in mould, proceeded to-35～-45 DEG C of vacuum freezing drying ovens in, be dried 16～24h, obtain nano zinc oxide fiber element sponge material.
The operation principle of gained nano zinc oxide fiber element sponge material of the present invention:
The nano zine oxide bulge-structure of gained nano zinc oxide fiber element sponge material surface of the present invention complexity is after ultraviolet irradiates, produce metal ion defects, formation Surface Oxygen hole is reacted with free oxygen, oxygen molecule and hydrone competitive Adsorption are at hole, under illumination condition, hydrone is easier to be adsorbed at Surface Oxygen hole, causes water to instead of in the space that air enters coarse structure, add the contact area of water droplet and sponge surface, substantially increase the hydrophilic of sponge；Under dark condition, oxygen molecule is easier to be adsorbed at oxygen vacancies, thus inhibit the absorption of hydrone, increase the hydrophobicity on surface, thus realize surface super hydrophobic and super hydrophilic reversible transformation by the transformation of illumination Yu dark condition, resulting materials can absorb own wt 6～the oil product of 14 times or organic solvent, and material still can keep the absorbance of 80～90% after the absorption/release cycle of 100～200 times.
Beneficial effects of the present invention:
(1) present invention uses the cellulose of wide material sources to be raw material, and raw material is cheap and easy to get, and gained sponge material is degradable after using, and will not produce secondary environmental pollution；
(2) resulting materials oleophylic of the present invention and hydrophilic can realize reversible transformation under illumination and dark condition, easily regenerate.
Detailed description of the invention
Weighing 80～100g boony fibres, being placed in 180～200mL mass concentrations is in 10～15%NaOH solution, after soaking 1～3h, it is washed with deionized 3～5 times, being proceeded to reactor again, start agitator, setting speed is 600～800r/min, it is passed through saturated vapor to reactor, until reacting kettle inner pressure reaches 1.5～1.8MPa, after pressurize 20～30min, material in reactor is proceeded in 105～110 DEG C of baking ovens, dry to constant weight, obtain alkali cellulose siccative；Weigh 30～50g above-mentioned alkali cellulose siccatives and 20～40gN, N '-carbonyl dimidazoles respectively, join and fill 30～36mL toluene, in the there-necked flask of the belt stirrer of 20～24mL dimethyl fumarates, it is placed on again in 55～75 DEG C of thermostat water baths, starts agitator, with 500～700r/min constant temperature stirrings 3～5h, sucking filtration, it is washed with deionized filter cake 3～5 times, filter cake is proceeded in 90～105 DEG C of baking ovens, be dried 3～5h, obtain activated cellulose, standby；Measuring 90～100mL concentration is 0.4～0.8mol/LNaOH solution, pass through Dropping funnel, dropwise drop to fill in the there-necked flask that 60～80mL concentration are 0.3～0.5mol/L solution of zinc sulfate, under 60～80 DEG C of waters bath with thermostatic control and 600～800r/min stirrings, control rate of addition so that it is in 1.5～3h, dropping is complete；After waiting to drip, add 2～4mLKH-550 silane couplers, continue constant temperature stirring reaction 3～5h, again standby activated cellulose is added in there-necked flask, continue constant temperature stirring reaction 3～5h, sucking filtration, it is washed with deionized filter cake 3～5 times, again filter cake is proceeded in 100～105 DEG C of baking ovens, be dried 2～4h, obtain nano zinc oxide fiber element siccative；Weigh 30～50g above-mentioned nano zinc oxide fiber element siccatives, 10～20g a length of 5～10mm successively
Absorbent cotton particle and 3～5gNa2SO4Powder, adding fills in the beaker that 150～200mL mass concentrations are 8～12%NaOH/ thiourea solutions, it is placed on again in sonic oscillation instrument, after vibration 10～20min, obtain uniform sizing material, then measure 60～80mL above-mentioned uniform sizing materials, pour in mould, proceeded to-35～-45 DEG C of vacuum freezing drying ovens in, be dried 16～24h, obtain nano zinc oxide fiber element sponge material.
Example 1
Weighing 80g boony fibre, being placed in 180mL mass concentration is in 10%NaOH solution, after soaking 1h, it is washed with deionized 3 times, being proceeded to reactor again, start agitator, setting speed is 600r/min, it is passed through saturated vapor to reactor, until reacting kettle inner pressure reaches 1.5MPa, after pressurize 20min, material in reactor is proceeded in 105 DEG C of baking ovens, dry to constant weight, obtain alkali cellulose siccative；Weigh 30g above-mentioned alkali cellulose siccative and 20gN, N '-carbonyl dimidazoles respectively, join and fill 30mL toluene, in the there-necked flask of the belt stirrer of 20mL dimethyl fumarate, it is placed on again in 55 DEG C of thermostat water baths, starts agitator, stir 3h with 500r/min constant temperature, sucking filtration, it is washed with deionized filter cake 3 times, filter cake is proceeded in 90 DEG C of baking ovens, be dried 3h, obtain activated cellulose, standby；Measuring 90mL concentration is 0.4mol/LNaOH solution, by Dropping funnel, dropwise drop to fill in the there-necked flask that 60mL concentration is 0.3mol/L solution of zinc sulfate, under 60 DEG C of waters bath with thermostatic control and 600r/min stirring, control rate of addition so that it is in 1.5h, dropping is complete；After waiting to drip, add 2mLKH-550 silane coupler, continue constant temperature stirring reaction 3h, again standby activated cellulose is added in there-necked flask, continue constant temperature stirring reaction 3h, sucking filtration, it is washed with deionized filter cake 3 times, again filter cake is proceeded in 100 DEG C of baking ovens, be dried 2h, obtain nano zinc oxide fiber element siccative；Weigh 30g above-mentioned nano zinc oxide fiber element siccative, a length of 5mm of 10g successively
Absorbent cotton particle and 3gNa2SO4Powder, adding fills in the beaker that 150mL mass concentration is 8%NaOH/ thiourea solution, it is placed on again in sonic oscillation instrument, after vibration 10min, obtain uniform sizing material, then measure the above-mentioned uniform sizing material of 60mL, pour in mould, proceeded in-35 DEG C of vacuum freezing drying ovens, be dried 16h, obtain nano zinc oxide fiber element sponge material.
The nano zine oxide bulge-structure of gained nano zinc oxide fiber element sponge material surface of the present invention complexity is after ultraviolet irradiates, produce metal ion defects, formation Surface Oxygen hole is reacted with free oxygen, oxygen molecule and hydrone competitive Adsorption are at hole, under illumination condition, hydrone is easier to be adsorbed at Surface Oxygen hole, causes water to instead of in the space that air enters coarse structure, add the contact area of water droplet and sponge surface, substantially increase the hydrophilic of sponge；Under dark condition, oxygen molecule is easier to be adsorbed at oxygen vacancies, thus inhibit the absorption of hydrone, increase the hydrophobicity on surface, thus realize surface super hydrophobic and super hydrophilic reversible transformation by the transformation of illumination Yu dark condition, resulting materials can absorb oil product or the organic solvent of own wt 6 times, and material still can keep the absorbance of 80% after the absorption/release cycle of 100 times.
Example 2
Weighing 90g boony fibre, being placed in 190mL mass concentration is in 12%NaOH solution, after soaking 2h, it is washed with deionized 4 times, being proceeded to reactor again, start agitator, setting speed is 700r/min, it is passed through saturated vapor to reactor, until reacting kettle inner pressure reaches 1.6MPa, after pressurize 25min, material in reactor is proceeded in 108 DEG C of baking ovens, dry to constant weight, obtain alkali cellulose siccative；Weigh 40g above-mentioned alkali cellulose siccative and 30gN, N '-carbonyl dimidazoles respectively, join and fill 34mL toluene, in the there-necked flask of the belt stirrer of 22mL dimethyl fumarate, it is placed on again in 65 DEG C of thermostat water baths, starts agitator, stir 4h with 600r/min constant temperature, sucking filtration, it is washed with deionized filter cake 4 times, filter cake is proceeded in 100 DEG C of baking ovens, be dried 4h, obtain activated cellulose, standby；Measuring 95mL concentration is 0.6mol/LNaOH solution, by Dropping funnel, dropwise drop to fill in the there-necked flask that 70mL concentration is 0.4mol/L solution of zinc sulfate, under 70 DEG C of waters bath with thermostatic control and 700r/min stirring, control rate of addition so that it is in 2h, dropping is complete；After waiting to drip, add 3mLKH-550 silane coupler, continue constant temperature stirring reaction 4h, again standby activated cellulose is added in there-necked flask, continue constant temperature stirring reaction 4h, sucking filtration, it is washed with deionized filter cake 4 times, again filter cake is proceeded in 102 DEG C of baking ovens, be dried 3h, obtain nano zinc oxide fiber element siccative；Weigh 40g above-mentioned nano zinc oxide fiber element siccative, 15g a length of 7mm absorbent cotton particle and 4gNa successively2SO4Powder, adding fills in the beaker that 180mL mass concentration is 10%NaOH/ thiourea solution, it is placed on again in sonic oscillation instrument, after vibration 15min, obtain uniform sizing material, then measure the above-mentioned uniform sizing material of 70mL, pour in mould, proceeded in-40 DEG C of vacuum freezing drying ovens, be dried 20h, obtain nano zinc oxide fiber element sponge material.
The nano zine oxide bulge-structure of gained nano zinc oxide fiber element sponge material surface of the present invention complexity is after ultraviolet irradiates, produce metal ion defects, formation Surface Oxygen hole is reacted with free oxygen, oxygen molecule and hydrone competitive Adsorption are at hole, under illumination condition, hydrone is easier to be adsorbed at Surface Oxygen hole, causes water to instead of in the space that air enters coarse structure, add the contact area of water droplet and sponge surface, substantially increase the hydrophilic of sponge；Under dark condition, oxygen molecule is easier to be adsorbed at oxygen vacancies, thus inhibit the absorption of hydrone, increase the hydrophobicity on surface, thus realize surface super hydrophobic and super hydrophilic reversible transformation by the transformation of illumination Yu dark condition, resulting materials can absorb oil product or the organic solvent of own wt 10 times, and material still can keep the absorbance of 85% after the absorption/release cycle of 150 times.
Example 3
Weighing 100g boony fibre, being placed in 200mL mass concentration is in 15%NaOH solution, after soaking 3h, it is washed with deionized 5 times, being proceeded to reactor again, start agitator, setting speed is 800r/min, it is passed through saturated vapor to reactor, until reacting kettle inner pressure reaches 1.8MPa, after pressurize 30min, material in reactor is proceeded in 110 DEG C of baking ovens, dry to constant weight, obtain alkali cellulose siccative；Weigh 50g above-mentioned alkali cellulose siccative and 40gN, N '-carbonyl dimidazoles respectively, join and fill 36mL toluene, in the there-necked flask of the belt stirrer of 24mL dimethyl fumarate, it is placed on again in 75 DEG C of thermostat water baths, starts agitator, stir 5h with 700r/min constant temperature, sucking filtration, it is washed with deionized filter cake 5 times, filter cake is proceeded in 105 DEG C of baking ovens, be dried 5h, obtain activated cellulose, standby；Measure 100mL concentration 0.8mol/LNaOH solution, by Dropping funnel, dropwise drop to fill in the there-necked flask that 80mL concentration is 0.5mol/L solution of zinc sulfate, under 80 DEG C of waters bath with thermostatic control and 800r/min stirring, control rate of addition so that it is in 3h, dropping is complete；After waiting to drip, add 4mLKH-550 silane coupler, continue constant temperature stirring reaction 5h, again standby activated cellulose is added in there-necked flask, continue constant temperature stirring reaction 5h, sucking filtration, it is washed with deionized filter cake 5 times, again filter cake is proceeded in 105 DEG C of baking ovens, be dried 4h, obtain nano zinc oxide fiber element siccative；Weigh 50g above-mentioned nano zinc oxide fiber element siccative, 20g a length of 10mm absorbent cotton particle and 5gNa successively2SO4Powder, adding fills in the beaker that 200mL mass concentration is 12%NaOH/ thiourea solution, it is placed on again in sonic oscillation instrument, after vibration 20min, obtain uniform sizing material, then measure the above-mentioned uniform sizing material of 80mL, pour in mould, proceeded in-45 DEG C of vacuum freezing drying ovens, be dried 24h, obtain nano zinc oxide fiber element sponge material.
The nano zine oxide bulge-structure of gained nano zinc oxide fiber element sponge material surface of the present invention complexity is after ultraviolet irradiates, produce metal ion defects, formation Surface Oxygen hole is reacted with free oxygen, oxygen molecule and hydrone competitive Adsorption are at hole, under illumination condition, hydrone is easier to be adsorbed at Surface Oxygen hole, causes water to instead of in the space that air enters coarse structure, add the contact area of water droplet and sponge surface, substantially increase the hydrophilic of sponge；Under dark condition, oxygen molecule is easier to be adsorbed at oxygen vacancies, thus inhibit the absorption of hydrone, increase the hydrophobicity on surface, thus realize surface super hydrophobic and super hydrophilic reversible transformation by the transformation of illumination Yu dark condition, resulting materials can absorb oil product or the organic solvent of own wt 14 times, and material still can keep the absorbance of 90% after the absorption/release cycle of 200 times.
Claims (1)
1. the preparation method of a nano zinc oxide fiber element sponge material, it is characterised in that concrete preparation process is:
(1) weighing 80～100g boony fibres, being placed in 180～200mL mass concentrations is in 10～15%NaOH solution, after soaking 1～3h, it is washed with deionized 3～5 times, being proceeded to reactor again, start agitator, setting speed is 600～800r/min, it is passed through saturated vapor to reactor, until reacting kettle inner pressure reaches 1.5～1.8MPa, after pressurize 20～30min, material in reactor is proceeded in 105～110 DEG C of baking ovens, dry to constant weight, obtain alkali cellulose siccative；
(2) weigh 30～50g above-mentioned alkali cellulose siccatives and 20～40gN, N '-carbonyl dimidazoles respectively, join and fill 30～36mL toluene, in the there-necked flask of the belt stirrer of 20～24mL dimethyl fumarates, it is placed on again in 55～75 DEG C of thermostat water baths, starts agitator, with 500～700r/min constant temperature stirrings 3～5h, sucking filtration, it is washed with deionized filter cake 3～5 times, filter cake is proceeded in 90～105 DEG C of baking ovens, be dried 3～5h, obtain activated cellulose, standby；
(3) measuring 90～100mL concentration is 0.4～0.8mol/LNaOH solution, pass through Dropping funnel, dropwise drop to fill in the there-necked flask that 60～80mL concentration are 0.3～0.5mol/L solution of zinc sulfate, under 60～80 DEG C of waters bath with thermostatic control and 600～800r/min stirrings, control rate of addition so that it is in 1.5～3h, dropping is complete；
(4) after waiting to drip, add 2～4mLKH-550 silane couplers, continue constant temperature stirring reaction 3～5h, again step (2) standby activated cellulose is added in there-necked flask, continue constant temperature stirring reaction 3～5h, sucking filtration, it is washed with deionized filter cake 3～5 times, again filter cake is proceeded in 100～105 DEG C of baking ovens, be dried 2～4h, obtain nano zinc oxide fiber element siccative；
(5) 30～50g above-mentioned nano zinc oxide fiber element siccatives, 10～20g a length of 5～10mm are weighed successively
Absorbent cotton particle and 3～5gNa2SO4Powder, adding fills in the beaker that 150～200mL mass concentrations are 8～12%NaOH/ thiourea solutions, it is placed on again in sonic oscillation instrument, after vibration 10～20min, obtain uniform sizing material, then measure 60～80mL above-mentioned uniform sizing materials, pour in mould, proceeded to-35～-45 DEG C of vacuum freezing drying ovens in, be dried 16～24h, obtain nano zinc oxide fiber element sponge material.
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| CN106674586A (en) * | 2016-12-14 | 2017-05-17 | 浙江理工大学 | Method for preparing cellulose nanocrystalline sponge material |
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