CN108273480A - A kind of preparation method of degradable oil absorption material - Google Patents

A kind of preparation method of degradable oil absorption material Download PDF

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CN108273480A
CN108273480A CN201810353860.1A CN201810353860A CN108273480A CN 108273480 A CN108273480 A CN 108273480A CN 201810353860 A CN201810353860 A CN 201810353860A CN 108273480 A CN108273480 A CN 108273480A
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oil absorption
sponge
absorption material
slurry
nanofiber
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许水仙
何伟仁
张建初
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02Separation of non-miscible liquids
    • B01D17/0202Separation of non-miscible liquids by ab- or adsorption
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/041Oxides or hydroxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • B01J20/24Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • B01J20/26Synthetic macromolecular compounds
    • B01J20/262Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28004Sorbent size or size distribution, e.g. particle size
    • B01J20/28007Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like

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Abstract

The present invention relates to oil absorption material preparing technical fields, and in particular to a kind of preparation method of degradable oil absorption material.The present invention is with sepiolite, Enteromorpha is that living fossil slurry and purifying alginate fibre element is made in raw material, nanofiber is put into dispersion in living fossil slurry and obtains nanofiber sponge slurry, purifying alginate fibre element is mixed with nanofiber sponge slurry, obtain dispersed paste, by composite sponge fiber, dimethyl silicone polymer, the material mixings such as atoleine are put into fermentation cylinder for fermentation modification, obtain degradable oil absorption material, sepiolite fibre is adsorbed in organic nanofibers surface and hole, improve the oil absorption of oil absorption material, the oily matters such as dimethyl silicone polymer generate on the surface of fiber sponge has the nonpolar group of oleophylic, improve the oleophilic drainage performance of fiber sponge, fiber-like material and stone slurry recycling are relatively simple, and it is free from environmental pollution, it has a extensive future.

Description

A kind of preparation method of degradable oil absorption material
Technical field
The present invention relates to oil absorption material preparing technical fields, and in particular to a kind of preparation method of degradable oil absorption material.
Background technology
In recent years, the frequent generation of offshore oil leakage accident and a large amount of discharges of industrial oily wastewater so that grease point Become focus of people's attention again from problem.Oily wastewater source is wider, such as Oil spills, land exploitation oil ore, food Many industries such as product, weaving, mechanical processing all discharge a large amount of oily wastewater into environment, and either industrial oily wastewater is still The arbitrary discharge of life oily wastewater all causes prodigious pollution to production and living environment, and the environmental problem thereby resulted in has not been allowed Ignore.
In recent decades, the research of oil absorption material is rapid with application development, and purposes is also very extensive.Traditional oil suction material Material, such as sponge, clay porous mass are widely used, although these materials have preferable oil absorbing effect, due to material The structural property of material itself makes traditional oil absorption material have the shortcomings that oil absorption is little, oil-water selectivity is not high, usually oil suction While also absorb water, and service life is short.It is just being answered extensively using artificial synthesized high molecular polymer as new oil absorption material With, such as polyurethane, polyethylene, polypropylene, this kind of polymer oil absorption material is big with oil absorption, the good advantage of oil absorbing effect, However this kind of material is poisonous and hazardous petrochemical industry material mostly, and it is not degradable after oil suction, handle the overall cost of waste Higher, reusability is poor, the problems such as being easy to bring secondary environmental pollution.
It can effectively overcome traditional natural organic oil absorption material by the novel oil absorption material that base material is developed of natural materials Defect, and have the characteristics that the rate of adsorption is fast, oil absorbency is high, biodegradable, people are paying more and more attention to it.Generally Ground, such oil absorption material mainly using agricultural wastes as raw material and it is hydrophobically modified be prepared, such as modified bagasse, modified rice Shell etc..Mainly oil is adsorbed by the capillarity in the gap of material surface and tube chamber, wherein material composition ratio pair Its oil absorbency is affected.Compared with polypropylene, the adsorption capacity of these modified natural materials is stronger, and rice husk and bagasse As agricultural waste material, derive from a wealth of sources, it being capable of natural degradation.But due in the cellulose of biological material hydroxyl it is more, There is larger hydrophily, cause its oil absorption little, oil suction multiplying power is smaller, and oil-water selectivity is not high, often while oil suction Also it absorbs water, reduces its oil suction and oil-retaining, fine and close pore structure limits the raising of oil absorbency, in addition, these are passed System organic adsorption material has a single function, it is impossible to be used in extreme harsh environment, such as superhigh temperature, ultralow temperature and acidity environment, limit Their applications in aerospace, industry and daily life are made.
Therefore, environmentally protective, biodegradable, efficient oil absorption material are developed as raw material using the compatible substance of environment, It is had a very important significance for improving marine environment and ecological environment.
Invention content
Present invention mainly solves the technical issues of, for traditional oil absorption material at present, such as sponge, clay porous mass It is widely used, although there is these materials preferable oil absorbing effect, the structural property of material itself to make traditional oil suction Material has the shortcomings that oil absorption is little, oil-water selectivity is not high, not degradable after oil absorption material oil suction, handles the comprehensive of waste This is higher for synthesis, and reusability is poor, and the defect for the problems such as being easy to bring secondary environmental pollution provides a kind of degradable oil suction The preparation method of material.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of preparation method of degradable oil absorption material, it is characterised in that specifically preparation process is:
(1)200~250g sepiolites are taken, is placed in stone mill and grinds, sieving obtains sepiolite powder, and 400 are added into plastic tub ~500mL phosphoric acid solutions, sepiolite powder is poured into plastic tub, is dispersed with stirring, and obtains sepiolite suspension, is suspended to sepiolite Liquid is passed through ammonia, obtains living fossil slurry;
(2)5~10g Enteromorphas are taken to be placed in Soxhlet extractor, it is molten with the ethyl alcohol that 80~100mL mass fractions are 20% ethyl acetate Liquid after extracting removes extraction of lipid object, then 40~50mL sodium carbonate liquors is added into Soxhlet extractor, extracts polysaccharide, filtering Isolated Enteromorpha slag afterwards, then by Enteromorpha slag sodium chlorite solution's oxide impregnation, filtering removal filtrate obtains residue, will It after the potassium hydroxide solution impregnation of residue, then is washed to neutrality with absolute ethyl alcohol, obtains purifying alginate fibre element;
(3)40~50g beta-cyclodextrins, 12~15g sodium hydroxides and 200~300mL distilled water are added in four-hole boiling flask, to four Mouth flask water-bath heat temperature raising starts blender and is stirred, and the dimethyl sulfoxide (DMSO) of 60~75mLE-51 type epoxy resin is molten Liquid is fitted into constant pressure funnel, and the dimethyl sulfoxide (DMSO) that E-51 type epoxy resin is added dropwise to four-hole boiling flask with constant pressure funnel is molten Liquid, insulation reaction obtain reaction product;
(4)Above-mentioned reaction product is washed with absolute ethyl alcohol 3~5 times, then the reaction product after washing is placed in vacuum drying chamber It is dried to obtain nanofiber sponge, 40~50g nanofiber sponges are put into 200~220mL living fossils slurry, are dispersed with stirring 30 Nanofiber sponge slurry is obtained after~45min;
(5)Purifying alginate fibre element is mixed with nanofiber sponge slurry, high speed dispersor high speed is placed in and disperses point Slurry is dissipated, dispersed paste is placed in vacuum filtration machine and is filtered, removal filtrate obtains composite sponge fiber;
(6)It counts in parts by weight, by 40~45 parts of composite sponge fibers, 5~8 parts of dimethyl silicone polymers, 10~15 parts of liquid Paraffin, 10~12 parts of yeast powders, 4~5 parts of water are put into fermentation cylinder for fermentation, obtain oleophylic modified sponge, by oleophylic modified sponge It is washed to neutrality with absolute ethyl alcohol, is placed in oven and dried to obtain degradable oil absorption material.
Step(1)The milling time is 2~3h, and be sieved specification is 200 mesh, and the mass fraction of phosphoric acid solution is 30%, it is 40~50min to be dispersed with stirring the time, and it is 8~10L to be passed through ammonia amount.
Step(2)The mass fraction of the ethanol solution of the ethyl acetate is 20%, and temperature is 85 when extracting removes lipid ~90 DEG C, extraction times are 6~8h, and the mass fraction of sodium carbonate liquor is 20%, and temperature is 58~62 DEG C of sub- chlorine when extracting polysaccharide The mass fraction of acid sodium solution is 10%, and the oxide impregnation time is 2~3h, and the mass fraction of potassium hydroxide solution is 40%, dipping Processing time is 5~10min.
Step(3)Described is 80~90 DEG C to temperature after the heating of four-hole boiling flask heating water bath, E-51 type epoxy resin The mass fraction 40% of dimethyl sulphoxide solution, the drop rate of constant pressure funnel be 5~10mL/min insulation reactions be 6~ 8h。
Step(4)The vacuum drying chamber set temperature is 90~100 DEG C, and drying time is 3~4h.
Step(5)The purifying alginate fibre element is 1 ︰ 5, high speed dispersion with nanofiber sponge slurry mixing quality ratio Rotating speed is 3000~4500r/min, and the high speed dispersion time is 10~15min.
Step(6)The fermentation temperature is 35~40 DEG C, and fermentation time is 3~5 days, and baking oven set temperature is 80~90 DEG C, drying time is 4~5h.
The beneficial effects of the invention are as follows:
(1)Incorporation phosphoric acid solution, which mixes dispersion and is passed through ammonia, after the present invention pulverizes sepiolite obtains living fossil slurry, will Enteromorpha obtains Enteromorpha slag with the ethanol solution of ethyl acetate and sodium carbonate liquor extracting removing lipid and polysaccharide respectively, then uses successively Washing to neutrality obtains purifying alginate fibre element after sodium chlorite solution and potassium hydroxide solution are handled, by E-51 type epoxy resin Dimethyl sulphoxide solution instill beta-cyclodextrin alkaline solution in, by heating react, obtain nanofiber, nanofiber put Enter dispersion in living fossil slurry and obtain nanofiber sponge slurry, purifying alginate fibre element is mixed with nanofiber sponge slurry, By high speed dispersion, dispersed paste is obtained, suction filtration processing is carried out to dispersed paste with vacuum filtration machine, filtrate is removed, detaches To composite sponge fiber, the material mixings such as composite sponge fiber, dimethyl silicone polymer, atoleine, yeast powder, water are put into In fermentation tank, be modified through everfermentation, obtain oleophylic modified sponge, obtain degradable oil absorption material after drying, the present invention pass through by Resin is prepared to obtain organic nanofibers sponge with cyclodextrin hybrid reaction, and sepiolite fibre is adsorbed on organic nanofibers surface In hole, nanofiber sponge slurry is obtained, so that its pore surface area is increased, improves the oil absorption of oil absorption material, phosphorus used Acid is a kind of acidic activator, can be by its swollen even by the certain ingredients of sepiolite during sepiolite comes into full contact with Dissolving, when purifying alginate fibre element is added, phosphoric acid molecules, which can penetrate into, wherein dissolves cellulose, a large amount of empty to be formed Gap makes the oil absorption of oil absorption material improve;
(2)Present invention oily matters such as dimethyl silicone polymer in the modifying process that ferments open simultaneously fibre under microbial action Blind hole and the inner passage for tieing up sponge, being generated on the surface of fiber sponge has the nonpolar group of oleophylic, and makes its surface Roughening, improves the oleophilic drainage performance of fiber sponge, it is made tentatively to have good oil-water selectivity, wherein alginate fibre element Aeroge can be formed after fermented inflation, have higher biocompatibility, adaptability and good biodegradability, seaweed Cellulose aerogels pore size is moderate, porosity is high, can have good oleophilic drainage after simple hydrophobically modified Property, it is a kind of good oil absorption material, oil absorption material ingredient of the invention is mainly vegetative fiber element, stone slurry, organic nano Fiber forms oil absorption material between them by simple physical action, is convenient for degradation treatment, fiber-like material and stone slurry recycling It is relatively simple and free from environmental pollution, it has a extensive future.
Specific implementation mode
200~250g sepiolites are taken, 2~3h of grinding in stone mill is placed in, 200 mesh is crossed and sieves to obtain sepiolite powder, to plastics The phosphoric acid solution that 400~500mL mass fractions are 30% is added in basin, sepiolite powder is poured into plastic tub, it is dispersed with stirring 40~ 50min obtains sepiolite suspension, and the ammonia of 8~10L is passed through to sepiolite suspension, obtains living fossil slurry;Take 5~10g watersides Tongue is placed in Soxhlet extractor, is the ethanol solution of 20% ethyl acetate with 80~100mL mass fractions, in 85~90 DEG C of conditions 6~8h of lower extracting after removing extraction of lipid object, then the carbonic acid that 40~50mL mass fractions are 20% is added into Soxhlet extractor Sodium solution extracts polysaccharide at 58~62 DEG C, isolated Enteromorpha slag after filtering, is then 10% by Enteromorpha slag mass fraction Sodium chlorite solution 2~3h of oxide impregnation, filtering removal filtrate, obtain residue, by residue mass fraction be 40% hydrogen-oxygen It after changing potassium solution impregnation 5~10min, then is washed to neutrality with absolute ethyl alcohol, obtains purifying alginate fibre element;By 40~ 50g beta-cyclodextrins, 12~15g sodium hydroxides and 200~300mL distilled water are added in four-hole boiling flask, add to four-hole boiling flask water-bath Heat is warming up to 80~90 DEG C, starts blender, 35~40min is stirred with the rotating speed of 300~350r/min, by 60~75mL The dimethyl sulphoxide solution of the E-51 type epoxy resin of mass fraction 40% is fitted into constant pressure funnel, uses constant pressure funnel The dimethyl sulphoxide solution of E-51 type epoxy resin, insulation reaction 6 is added dropwise to four-hole boiling flask with the drop rate of 5~10mL/min ~8h, obtains reaction product;Above-mentioned reaction product is washed with absolute ethyl alcohol 3~5 times, then the reaction product after washing is placed in and is set Constant temperature degree is in 90~100 DEG C of vacuum drying chambers, and dry 3~4h obtains nanofiber sponge, by 40~50g nanofibers sea Silk floss is put into 200~220mL living fossils slurry, and nanofiber sponge slurry is obtained after being dispersed with stirring 30~45min;Seaweed will be purified Cellulose is mixed with nanofiber sponge slurry 1 ︰ 5 in mass ratio, is placed in high speed dispersor, with 3000~4500r/min's Rotating speed 10~15min of high speed dispersion, obtains dispersed paste, and dispersed paste is placed in vacuum filtration machine and is filtered, and removal filtrate obtains To composite sponge fiber;Count in parts by weight, by 40~45 parts of composite sponge fibers, 5~8 parts of dimethyl silicone polymers, 10~ 15 parts of atoleines, 10~12 parts of yeast powders, 4~5 parts of water are put into fermentation tank, are fermented 3~5 days, are obtained at 35~40 DEG C Oleophylic modified sponge washs oleophylic modified sponge to neutrality with absolute ethyl alcohol, is put into the baking that set temperature is 80~90 DEG C Dry 4~5h, obtains degradable oil absorption material in case.
Example 1
200g sepiolites are taken, is placed in stone mill and grinds 2h, 200 mesh is crossed and sieves to obtain sepiolite powder, 400mL is added into plastic tub The phosphoric acid solution that mass fraction is 30%, sepiolite powder is poured into plastic tub, 40min is dispersed with stirring, and obtains sepiolite suspension Liquid is passed through the ammonia of 8L to sepiolite suspension, obtains living fossil slurry;5g Enteromorphas are taken to be placed in Soxhlet extractor, with 80mL matter The ethanol solution that score is 20% ethyl acetate is measured, extracts 6h under the conditions of 85 DEG C, after removing extraction of lipid object, then is carried to Soxhlet The sodium carbonate liquor for being added that 40mL mass fractions are 20% in device is taken, polysaccharide is extracted at 58 DEG C, isolated Enteromorpha after filtering Slag, the sodium chlorite solution oxide impregnation 2h for being then 10% by Enteromorpha slag mass fraction, filtering removal filtrate obtain residue, It after the potassium hydroxide solution impregnation 5min for being 40% by residue mass fraction, then is washed to neutrality with absolute ethyl alcohol, is obtained Purify alginate fibre element;40g beta-cyclodextrins, 12g sodium hydroxides and 200mL distilled water are added in four-hole boiling flask, four mouthfuls are burnt Bottle heating water bath is warming up to 80 DEG C, starts blender, 35min is stirred with the rotating speed of 300r/min, by 60mL mass fractions The dimethyl sulphoxide solution of 40% E-51 type epoxy resin is fitted into constant pressure funnel, with constant pressure funnel with 5mL/min Drop rate to four-hole boiling flask be added dropwise E-51 type epoxy resin dimethyl sulphoxide solution, insulation reaction 6h, obtain reaction production Object;Above-mentioned reaction product is washed with absolute ethyl alcohol 3 times, then it is that 90 DEG C of vacuum are done that the reaction product after washing, which is placed in set temperature, In dry case, dry 3h obtains nanofiber sponge, and 40g nanofiber sponges are put into 200mL living fossils slurry, are dispersed with stirring Nanofiber sponge slurry is obtained after 30min;Purifying alginate fibre element is mixed with nanofiber sponge slurry 1 ︰ 5 in mass ratio It closes, is placed in high speed dispersor, with the rotating speed high speed dispersion 10min of 3000r/min, obtains dispersed paste, dispersed paste is set It is filtered in vacuum filtration machine, removal filtrate obtains composite sponge fiber;It counts in parts by weight, by 40 parts of composite sponge fibers, 5 Part dimethyl silicone polymer, 10 parts of atoleines, 10 parts of yeast powders, 4 parts of water are put into fermentation tank, are fermented 3 days, are obtained at 35 DEG C To oleophylic modified sponge, oleophylic modified sponge is washed with absolute ethyl alcohol to neutrality, is put into the baking oven that set temperature is 80 DEG C Middle dry 4h, obtains degradable oil absorption material.
Example 2
225g sepiolites are taken, is placed in stone mill and grinds 2.5h, 200 mesh is crossed and sieves to obtain sepiolite powder, be added into plastic tub The phosphoric acid solution that 450mL mass fractions are 30%, sepiolite powder is poured into plastic tub, 45min is dispersed with stirring, obtains sepiolite Suspension is passed through the ammonia of 9L to sepiolite suspension, obtains living fossil slurry;It takes 7g Enteromorphas to be placed in Soxhlet extractor, uses 90mL mass fractions are the ethanol solution of 20% ethyl acetate, and 7h is extracted under the conditions of 87 DEG C, after removing extraction of lipid object, then to The sodium carbonate liquor that 45mL mass fractions are 20% is added in Soxhlet extractor, polysaccharide is extracted at 60 DEG C, it is isolated after filtering Enteromorpha slag, the sodium chlorite solution oxide impregnation 2.5h for being then 10% by Enteromorpha slag mass fraction, filtering removal filtrate obtain To residue, after the potassium hydroxide solution impregnation 7min for being 40% by residue mass fraction, then washed into absolute ethyl alcohol Property, obtain purifying alginate fibre element;45g beta-cyclodextrins, 14g sodium hydroxides and 250mL distilled water are added in four-hole boiling flask, it is right Four-hole boiling flask heating water bath is warming up to 85 DEG C, starts blender, 38min is stirred with the rotating speed of 325r/min, by 68mL matter The dimethyl sulphoxide solution of E-51 type epoxy resin for measuring score 40% is fitted into constant pressure funnel, with constant pressure funnel with The dimethyl sulphoxide solution of E-51 type epoxy resin is added dropwise to four-hole boiling flask for the drop rate of 7mL/min, and insulation reaction 7h is obtained Reaction product;Above-mentioned reaction product is washed with absolute ethyl alcohol 4 times, then it is 95 DEG C that the reaction product after washing, which is placed in set temperature, In vacuum drying chamber, dry 3.5h obtains nanofiber sponge, and 45g nanofiber sponges are put into 210mL living fossils slurry, Nanofiber sponge slurry is obtained after being dispersed with stirring 38min;Purifying alginate fibre element is pressed into quality with nanofiber sponge slurry It is mixed than 1 ︰ 5, is placed in high speed dispersor, with the rotating speed high speed dispersion 13min of 3750r/min, obtains dispersed paste, will disperse Slurry is placed in vacuum filtration machine and filters, and removal filtrate obtains composite sponge fiber;It counts in parts by weight, by 43 parts of composite sponges Fiber, 7 parts of dimethyl silicone polymers, 13 parts of atoleines, 11 parts of yeast powders, 4 parts of water are put into fermentation tank, are fermented at 38 DEG C 4 days, oleophylic modified sponge is obtained, oleophylic modified sponge is washed with absolute ethyl alcohol to neutrality, it is 85 DEG C to be put into set temperature Baking oven in dry 4.5h, obtain degradable oil absorption material.
Example 3
250g sepiolites are taken, is placed in stone mill and grinds 3h, 200 mesh is crossed and sieves to obtain sepiolite powder, 500mL is added into plastic tub The phosphoric acid solution that mass fraction is 30%, sepiolite powder is poured into plastic tub, 50min is dispersed with stirring, and obtains sepiolite suspension Liquid is passed through the ammonia of 10L to sepiolite suspension, obtains living fossil slurry;It takes 10g Enteromorphas to be placed in Soxhlet extractor, uses 100mL Mass fraction is the ethanol solution of 20% ethyl acetate, extracts 8h under the conditions of 90 DEG C, after removing extraction of lipid object, then to Soxhlet The sodium carbonate liquor that 50mL mass fractions are 20% is added in extractor, polysaccharide is extracted at 62 DEG C, isolated Enteromorpha after filtering Slag, the sodium chlorite solution oxide impregnation 3h for being then 10% by Enteromorpha slag mass fraction, filtering removal filtrate obtain residue, It after the potassium hydroxide solution impregnation 10min for being 40% by residue mass fraction, then is washed to neutrality with absolute ethyl alcohol, is obtained To purifying alginate fibre element;50g beta-cyclodextrins, 15g sodium hydroxides and 300mL distilled water are added in four-hole boiling flask, to four mouthfuls Flask water-bath is heated to 90 DEG C, starts blender, 40min is stirred with the rotating speed of 350r/min, by 75mL mass point The dimethyl sulphoxide solution of the E-51 type epoxy resin of number 40% is fitted into constant pressure funnel, with constant pressure funnel with 10mL/ The dimethyl sulphoxide solution of E-51 type epoxy resin is added dropwise to four-hole boiling flask for the drop rate of min, and insulation reaction 8h is reacted Product;Above-mentioned reaction product is washed with absolute ethyl alcohol 5 times, then it is 100 DEG C true that the reaction product after washing, which is placed in set temperature, In empty drying box, dry 4h obtains nanofiber sponge, 50g nanofiber sponges is put into 220mL living fossils slurry, stirring Nanofiber sponge slurry is obtained after dispersion 45min;It will purifying alginate fibre element and nanofiber sponge slurry 1 ︰ 5 in mass ratio Mixing, is placed in high speed dispersor, with the rotating speed high speed dispersion 15min of 4500r/min, dispersed paste is obtained, by dispersed paste It is placed in vacuum filtration machine and filters, removal filtrate obtains composite sponge fiber;It counts in parts by weight, by 45 parts of composite sponge fibres Dimension, 8 parts of dimethyl silicone polymers, 15 parts of atoleines, 12 parts of yeast powders, 5 parts of water are put into fermentation tank, ferment 5 at 40 DEG C It, obtains oleophylic modified sponge, and oleophylic modified sponge is washed with absolute ethyl alcohol to neutrality, and it is 90 DEG C to be put into set temperature Dry 5h, obtains degradable oil absorption material in baking oven.
Comparative example
As a comparison case with the oil absorption material of Chengdu company production
Oil absorption material in degradable oil absorption material produced by the present invention and comparative example is detected, testing result such as 1 institute of table Show:
The test of product oil suction multiplying power and water absorbent rate:
Oil product and clear water are respectively charged into the dry glass beaker of 500mL, gathered 30 mesh equipped with oil absorption material at 25 DEG C It is put into the container that propylene net is made in the beaker for filling oil product or water, after adsorbing a hour respectively.It is taken out and is held with tweezers Device is put on stainless steel mesh after draining 5min and weighs, while doing blank test, in triplicate, is averaged.
Oil suction multiplying power, water absorbent rate calculation formula are as follows:
Q=(m3-m2-m1)/m1
In formula:Q is oil suction multiplying power or water absorbent rate(g/g);m1For the quality of dry oil absorption material(g);m2For the matter of container Amount(g);m3For the quality of oil absorption material and container after oil suction or water suction(g).
The measurement of oil holdup:
Sample is weighed after oil absorption test, is put into the 500mL beakers equipped with 300mL water, after then vibrating 10min, takes out examination After sample drains 5min, sample is removed.At this point, being rushed out the oil come in the process containing water and sample earthquake in beaker.It will burn Oil water mixture in cup pours into separatory funnel together, stratification, releases the lower water in separatory funnel, and weighing is rushed The quality of the oil gone out.
H=(m3-m2-m1-m4)/(m3-m2-m1)×100%
H is oil holdup, %;m1For the weight of dry oil absorption material(g);m2For the quality of container(g);m3For oil absorption material after oil suction With the quality of container(g);m4It is oscillated the quality for the oil gone out in water for sample(g).
1 performance measurement result of table
From the data in table 1, it can be seen that degradable oil absorption material produced by the present invention, has very strong adsorption capacity, and density to oil product Small, good mechanical property, easy to use, high recycling rate, service life is long, free from environmental pollution etc., before having good market Scape.

Claims (7)

1. a kind of preparation method of degradable oil absorption material, it is characterised in that specifically preparation process is:
(1)200~250g sepiolites are taken, is placed in stone mill and grinds, sieving obtains sepiolite powder, and 400 are added into plastic tub ~500mL phosphoric acid solutions, sepiolite powder is poured into plastic tub, is dispersed with stirring, and obtains sepiolite suspension, is suspended to sepiolite Liquid is passed through ammonia, obtains living fossil slurry;
(2)5~10g Enteromorphas are taken to be placed in Soxhlet extractor, it is molten with the ethyl alcohol that 80~100mL mass fractions are 20% ethyl acetate Liquid after extracting removes extraction of lipid object, then 40~50mL sodium carbonate liquors is added into Soxhlet extractor, extracts polysaccharide, filtering Isolated Enteromorpha slag afterwards, then by Enteromorpha slag sodium chlorite solution's oxide impregnation, filtering removal filtrate obtains residue, will It after the potassium hydroxide solution impregnation of residue, then is washed to neutrality with absolute ethyl alcohol, obtains purifying alginate fibre element;
(3)40~50g beta-cyclodextrins, 12~15g sodium hydroxides and 200~300mL distilled water are added in four-hole boiling flask, to four Mouth flask water-bath heat temperature raising starts blender and is stirred, and the dimethyl sulfoxide (DMSO) of 60~75mLE-51 type epoxy resin is molten Liquid is fitted into constant pressure funnel, and the dimethyl sulfoxide (DMSO) that E-51 type epoxy resin is added dropwise to four-hole boiling flask with constant pressure funnel is molten Liquid, insulation reaction obtain reaction product;
(4)Above-mentioned reaction product is washed with absolute ethyl alcohol 3~5 times, then the reaction product after washing is placed in vacuum drying chamber It is dried to obtain nanofiber sponge, 40~50g nanofiber sponges are put into 200~220mL living fossils slurry, are dispersed with stirring 30 Nanofiber sponge slurry is obtained after~45min;
(5)Purifying alginate fibre element is mixed with nanofiber sponge slurry, high speed dispersor high speed is placed in and disperses point Slurry is dissipated, dispersed paste is placed in vacuum filtration machine and is filtered, removal filtrate obtains composite sponge fiber;
(6)It counts in parts by weight, by 40~45 parts of composite sponge fibers, 5~8 parts of dimethyl silicone polymers, 10~15 parts of liquid Paraffin, 10~12 parts of yeast powders, 4~5 parts of water are put into fermentation cylinder for fermentation, obtain oleophylic modified sponge, by oleophylic modified sponge It is washed to neutrality with absolute ethyl alcohol, is placed in oven and dried to obtain degradable oil absorption material.
2. a kind of preparation method of degradable oil absorption material according to claim 1, it is characterised in that:Step(1)It is described Milling time be 2~3h, be sieved specification is 200 mesh, and the mass fraction of phosphoric acid solution is 30%, and it is 40 to be dispersed with stirring the time ~50min, it is 8~10L to be passed through ammonia amount.
3. a kind of preparation method of degradable oil absorption material according to claim 1, it is characterised in that:Step(2)It is described Ethyl acetate ethanol solution mass fraction be 20%, extracting removing lipid when temperature be 85~90 DEG C, extraction times 6 The mass fraction of~8h, sodium carbonate liquor are 20%, and temperature is the mass fraction of 58~62 DEG C of sodium chlorite solutions when extracting polysaccharide It is 10%, the oxide impregnation time is 2~3h, and the mass fraction of potassium hydroxide solution is 40%, and the impregnation time is 5~10min.
4. a kind of preparation method of degradable oil absorption material according to claim 1, it is characterised in that:Step(3)It is described To four-hole boiling flask heating water bath heat up after temperature be 80~90 DEG C, the quality of the dimethyl sulphoxide solution of E-51 type epoxy resin Score 40%, it is 6~8h that the drop rate of constant pressure funnel, which is 5~10mL/min insulation reactions,.
5. a kind of preparation method of degradable oil absorption material according to claim 1, it is characterised in that:Step(4)It is described Vacuum drying chamber set temperature be 90~100 DEG C, drying time be 3~4h.
6. a kind of preparation method of degradable oil absorption material according to claim 1, it is characterised in that:Step(5)It is described Purifying alginate fibre element and nanofiber sponge slurry mixing quality ratio be 1 ︰ 5, high speed dispersion rotating speed is 3000~4500r/ Min, high speed dispersion time are 10~15min.
7. a kind of preparation method of degradable oil absorption material according to claim 1, it is characterised in that:Step(6)It is described Fermentation temperature be 35~40 DEG C, fermentation time be 3~5 days, baking oven set temperature be 80~90 DEG C, drying time be 4~5h.
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CN109174030A (en) * 2018-10-10 2019-01-11 广西科学院 A kind of petroleum improvement modified montmorillonoid complex microorganism cleanser
CN109762525A (en) * 2019-01-28 2019-05-17 皮蒙 A kind of preparation method of degradable recycling fuel thickener
CN110314657A (en) * 2019-06-13 2019-10-11 安徽工程大学 A kind of biology based oil-absorption material and its application
CN112047570A (en) * 2020-09-03 2020-12-08 常德鑫芙蓉环保有限公司 Treatment method of oily industrial wastewater
CN112403527A (en) * 2020-11-27 2021-02-26 广东嘉荣环保新能源科技有限公司 Catalyst for degrading kitchen waste and preparation method and application thereof
CN116375421A (en) * 2023-03-27 2023-07-04 河源市源隆新型环保建材有限公司 Dry-mixed thin-layer masonry mortar and preparation method thereof

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CN105797431A (en) * 2016-03-28 2016-07-27 桂林理工大学 Method for preparing efficient hydrophobic oil-absorbing sponge
CN107641252A (en) * 2017-10-09 2018-01-30 常州汉唐文化传媒有限公司 A kind of polyacrylic preparation method of flame-retardant smoke inhibition

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CN103980530A (en) * 2014-05-27 2014-08-13 哈尔滨工业大学 Method for preparing seaweed cellulose aerogel oil absorption material
CN105797431A (en) * 2016-03-28 2016-07-27 桂林理工大学 Method for preparing efficient hydrophobic oil-absorbing sponge
CN107641252A (en) * 2017-10-09 2018-01-30 常州汉唐文化传媒有限公司 A kind of polyacrylic preparation method of flame-retardant smoke inhibition

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109174030A (en) * 2018-10-10 2019-01-11 广西科学院 A kind of petroleum improvement modified montmorillonoid complex microorganism cleanser
CN109762525A (en) * 2019-01-28 2019-05-17 皮蒙 A kind of preparation method of degradable recycling fuel thickener
CN110314657A (en) * 2019-06-13 2019-10-11 安徽工程大学 A kind of biology based oil-absorption material and its application
CN112047570A (en) * 2020-09-03 2020-12-08 常德鑫芙蓉环保有限公司 Treatment method of oily industrial wastewater
CN112403527A (en) * 2020-11-27 2021-02-26 广东嘉荣环保新能源科技有限公司 Catalyst for degrading kitchen waste and preparation method and application thereof
CN112403527B (en) * 2020-11-27 2023-08-01 广东嘉荣环保新能源科技有限公司 Catalyst for degrading kitchen waste and preparation method and application thereof
CN116375421A (en) * 2023-03-27 2023-07-04 河源市源隆新型环保建材有限公司 Dry-mixed thin-layer masonry mortar and preparation method thereof
CN116375421B (en) * 2023-03-27 2023-10-24 河源市源隆新型环保建材有限公司 Dry-mixed thin-layer masonry mortar and preparation method thereof

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