CN109011709A - A kind of compound oil absorption material - Google Patents
A kind of compound oil absorption material Download PDFInfo
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- CN109011709A CN109011709A CN201811104035.4A CN201811104035A CN109011709A CN 109011709 A CN109011709 A CN 109011709A CN 201811104035 A CN201811104035 A CN 201811104035A CN 109011709 A CN109011709 A CN 109011709A
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Abstract
The invention discloses a kind of compound oil absorption materials.Belong to oil absorption material preparation field.The present invention is using cotton fiber as raw material, N, N- methylene-bisacrylamide is crosslinking agent, the cellulose aerogels with three-dimensional connected porous structure are prepared with freeze drying technology, the chemical crosslinking and hydrogen bond action that surface hydroxyl occurs in silanol and internal fiber element accumulation process, so that the contact angle of this material and water significantly increases, it can express good oil absorbing effect；The nanometer Fe that the present invention adds3O4Presence the stability of system can be improved, it is anticorrosive, cooperate the TiO with photocatalytic activity2The hydrophobic oil absorbing effect of this system can be improved well, further construct hydrophobic oleophilic oil composite system.The present invention solves the problems, such as to commonly use oil absorption material at present and holds that rate is low, oil absorbing effect is bad.
Description
Technical field
The invention belongs to oil absorption material preparation fields, and in particular to a kind of compound oil absorption material.
Background technique
With the increase of petroleum and oil product dosage, destruction caused by marine oil overflow is big with the extent of injury, involves model
The features such as wide, removing is difficult is enclosed, to be solved these problems, urgent need develops efficient, durable, clean oil absorption material.
Good oil absorption material should have hydrophobicity is strong, oil suction is fast, oil absorption is big, do not settle after oil suction, it is recyclable again
Utilize, environmentally friendly feature.Absorption method is mostly used at present, absorption method embodies the advantages such as efficient, economic.The absorption of use
Agent mainly has chemical synthesis, natural inorganic, natural organic three categories.Wherein, chemical synthesis oil absorption material mainly has polypropylene fine
Dimension, polyurethane foam and alkyl vinyl polymer are also current using most wide oil absorption material, shared in the market sales volume
Share it is maximum.It is that good lipophilic-hydrophobic property, speed of oil absorption are fast that chemical synthesis oil absorption material, which has, and oil suction multiplying power is higher, disadvantage
It is that be pressurized still can oil leak, it is difficult to biodegradable and expensive；Inorganic oil absorption material is from a wealth of sources, and oil suction multiplying power is high, preparation side
Method is easy, easy to operate, but there are problems that cyclic utilization rate is low, oil-water selectivity is poor, floatability is poor, is difficult to dispose.It is organic
Oil absorption material can be divided into natural or natural modified organic oil absorption material and artificial synthesized two class of organic oil absorption material.It is organic
Oil absorption material is fast compared to swelling rate for inorganic oil absorption material, and cyclic utilization rate is good, but synthesis is complex, can't
The universal cleaning for being individually used for oil spilling, generally handles oil spill accident together with other methods or inorganic oil absorption material for it.
For the oil absorption material being commonly used, although the problem of largely solving crude oil leakage pollution,
But degradation efficiency is low after materials'use is difficult to handle, and oil absorbing effect is bad.Therefore a kind of compound suction that oil suction effect is strong need to be developed
Light wood material.
Summary of the invention
The technical problems to be solved by the invention: hold that rate is low, oil absorbing effect is bad for current common oil absorption material
Problem provides a kind of compound oil absorption material.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of compound oil absorption material, including following component, 10 ~ 15 parts of acetic anhydrides, 8 ~ 14 parts of acetone, 12 ~ 20 parts of konjac glucomannan processing
Object, 2 ~ 5 parts of auxiliary agents, 30 ~ 50 parts of water, further includes: 25 ~ 50 parts of composite hydrophobic fiber aeroges, 12 ~ 25 parts of hydrophobic effect material.
The preparation method of the composite hydrophobic fiber aeroge, includes the following steps:
(1) taking cotton fiber is dry, and nanometer Fe is added in 3:0.1 ~ 0.3:15 in mass ratio ~ 253O4, reagent A be mixed, centrifugation,
Removal centrifugation object, obtains cellulose solution, in 35 ~ 50 DEG C, takes cellulose solution that the N of cellulose solution quality 1 ~ 4%, N- di-2-ethylhexylphosphine oxide is added
Acrylamide is mixed, and is stored at room temperature, and obtains hydrogel, water intaking gel washing, and freeze-drying obtains cross filament hydrogel；
(2) it takes cross filament hydrogel in closed drier, one is placed in the drier and contains 1 ~ 3mL methyl trichlorine silicon
The open cuvette of alkane, room temperature close drying device progress Silanization reaction 20 ~ for 24 hours, silanization aeroge is obtained, silanization aeroge is taken
The pre-treating fly ash of 5 ~ 8:0.3:1 in mass ratio, reagent B are coated, and are dried in vacuo to get composite hydrophobic fiber airsetting
Glue.
Reagent A in the step (1): in mass ratio 3:10 ~ 16 take NaOH solution, urea liquid mixing, refrigeration to get
Reagent A.
Pre-treating fly ash in the step (2): take flyash 1:12 in mass ratio ~ 18 that sodium carbonate liquor mixing is added
Stirring, filtering take filter residue 7 ~ 14:2 in mass ratio that polyvinylpyrrolidone mixing is added to get pre-treating fly ash.
Reagent B in the step (2): 1:1 ~ 3 take ethyl acetate, castor oil mixing to get reagent B in mass ratio.
The preparation of the hydrophobic effect material: in 25 ~ 35 DEG C, water intaking talcum 1:8 ~ 15:0.3 in mass ratio addition formamide,
Intercalator mixing, is stirred with shaking table, and the MnO of hydrotalcite quality 4 ~ 8% is added2Mixing, shaking table stirring, addition hydrotalcite quality 25 ~
40 times of acetone mixing, is stored at room temperature, is centrifuged, and takes centrifugation object washes of absolute alcohol, dry, obtains dried object, take dried object by
Additive mixing is added to get hydrophobic effect material in 8 ~ 12:1 of mass ratio.
The intercalator: 5:1 ~ 3 take cetyl trimethylammonium bromide, neopelex mixing in mass ratio,
Up to intercalator.
The additive: 1:4 ~ 8 take lecithin, n-butanol mixing to get additive in mass ratio.
The konjac glucomannan processed material: taking wheat bran to pulverize and sieve, and takes sieving particle 1:10 ~ 16:3 in mass ratio that NaOH is added molten
Liquid, konjaku flour are mixed, and are stored at room temperature, and filter, take filter cake to be freeze-dried to get konjac glucomannan processed material.
The auxiliary agent: 1:4 ~ 6 take bacteria cellulose, microcrystalline wax mixing to get auxiliary agent in mass ratio.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention is using cotton fiber as raw material, N, and N- methylene-bisacrylamide is crosslinking agent, and being prepared with freeze drying technology has
The cellulose aerogels of three-dimensional connected porous structure carry out silylating reagent to it with chemical vapour deposition technique, improve inside it
Contact angle, the chemical crosslinking and hydrogen bond that surface hydroxyl occurs in the silanol and internal fiber element accumulation process that siliceous ingredient generates
Effect constitutes chemical crosslinking network, improves the connection of this material internal, and the nonpolar polysiloxane molecule of fiber surface package
It can provide repulsive interaction again between middle methyl, reduce the physical crosslinking degree between tissue to a certain extent, play definitely swollen
Swollen effect, can be improved this system to the volume of holding of oil, and the introducing of non-polar group during the preparation process so that this material with
The contact angle of water significantly increases, and can express good oil absorbing effect；
(2) nanometer Fe that the present invention adds3O4Presence the stability of system can be improved, it is anticorrosive, and assign this material magnetic
Power, facilitates recycling, and the SiO of the preprocessed activation of flyash2、TiO2It can play the role of filling system and hydrophobically modified,
Intercalation is carried out to hydrotalcite with intercalator, increase interlamellar spacing and builds the hydrophobic space of interlayer, by hydrophobic effect by MnO2It sets
In interlayer, the catalyst with the open hydrophobic space of two dimension is constructed, the TiO with photocatalytic activity is cooperated2It can improve well
The hydrophobic oil absorbing effect of this system further constructs hydrophobic oleophilic oil composite system.
Specific embodiment
Reagent A: it is 12% urea liquid that 3:10 ~ 16, which take NaOH solution, mass fraction that mass fraction is 10%, in mass ratio
Mixing, in -10 DEG C of DEG C of refrigerator cold-storages to get reagent A.
Reagent B: 1:1 ~ 3 take ethyl acetate, castor oil mixing to get reagent B in mass ratio.
Pre-treating fly ash: taking flyash 1:12 in mass ratio ~ 18 that the sodium carbonate liquor that mass fraction is 8% is added and mix,
30 ~ 55min is stirred with 400 ~ 600r/min, filtering takes filter residue 7 ~ 14:2 in mass ratio that polyvinylpyrrolidone mixing is added, i.e.,
Obtain pre-treating fly ash.
Intercalator: in mass ratio 5:1 ~ 3 take cetyl trimethylammonium bromide, neopelex mixing to get
Intercalator.
Additive: 1:4 ~ 8 take lecithin, n-butanol mixing to get additive in mass ratio.
Konjac glucomannan processed material: taking wheat bran to crushed 200 meshes in pulverizer, takes sieving particle 1:10 ~ 16:3 in mass ratio
The NaOH solution that mass fraction is 8%, konjaku flour mixing is added, with 400 ~ 700r/min, 30 ~ 55min of magnetic agitation, is stored at room temperature
2 ~ 4h, filtering take filter cake in the dry 12 ~ 16h of -40 DEG C of freeze driers to get konjac glucomannan processed material.
Auxiliary agent: 1:4 ~ 6 take bacteria cellulose, microcrystalline wax mixing to get auxiliary agent in mass ratio.
The preparation method of composite hydrophobic fiber aeroge, includes the following steps:
(1) for taking cotton fiber after the dry 8 ~ 12h of 60 ~ 80 DEG C of vacuum ovens, nanometer is added in 3:0.1 ~ 0.3:15 in mass ratio ~ 25
Fe3O4, reagent A mixing centrifuge is transferred to 3000 ~ 4000r/min centrifugation with 500 ~ 800r/min, 35 ~ 60min of magnetic agitation
Handle 10 ~ 15min, removal centrifugation object, obtain cellulose solution, in 35 ~ 50 DEG C of water-bath, take cellulose solution be added cellulose solution quality 1 ~
The mixing of 4% N, N- methylene-bisacrylamide, with 400 ~ 700r/min, 30 ~ 55min of magnetic agitation, is stored at room temperature 4 ~ 6h, obtains water
Gel, water intaking gel obtain cross filament water with the dry 4 ~ 6h of -40 DEG C of freeze driers after deionized water water washing 2 ~ 4 times, are moved to
Gel；
(2) cross filament hydrogel is taken, in closed drier, and one is placed in the drier and contains 1 ~ 3mL methyl
The closed progress Silanization reaction 20 of drier room temperature ~ for 24 hours is obtained silanization aeroge, takes silane by the open cuvette of trichlorosilane
After change aeroge 5 ~ 8:0.3:1 in mass ratio pre-treating fly ash, reagent B are coated, 50 ~ 70 DEG C of vacuum ovens are moved to
Dry 6 ~ 10h is to get composite hydrophobic fiber aeroge.
The preparation of hydrophobic effect material: in 25 ~ 35 DEG C, formamide, intercalation is added in water intaking talcum 1:8 ~ 15:0.3 in mass ratio
The MnO of hydrotalcite quality 4 ~ 8% was added with 220 ~ 300r/min shaking table stirring 2 ~ 4 days in agent mixing2Mixing, with 250 ~ 320r/
Min shaking table stir 10 ~ 14h, be added 25 ~ 40 times of hydrotalcite quality acetone mixing, be stored at room temperature 1 ~ 3h, move to centrifuge with
3000 ~ 4000r/min, 10 ~ 16min of centrifugal treating, it is dry in 65 ~ 80 DEG C of vacuum after taking centrifugation object washes of absolute alcohol 2 ~ 4 times
Dry 8 ~ 12h, obtains dried object, takes dried object 8 ~ 12:1 in mass ratio that additive mixing is added to get hydrophobic effect material.
A kind of compound oil absorption material, according to the mass fraction, including following component, 10 ~ 15 parts of acetic anhydrides, 8 ~ 14 parts of acetone,
12 ~ 20 parts of konjac glucomannan processed materials, 2 ~ 5 parts of auxiliary agents, 30 ~ 50 parts of water, 25 ~ 50 parts of composite hydrophobic fiber aeroges, 12 ~ 25 parts it is hydrophobic
Make materials.
A kind of preparation method of compound oil absorption material, includes the following steps:
(1) according to the mass fraction, take 10 ~ 15 parts of acetic anhydrides, 8 ~ 14 parts of acetone, 12 ~ 20 parts of konjac glucomannan processed materials, 2 ~ 5 parts of auxiliary agents,
30 ~ 50 parts of water, 25 ~ 50 parts of composite hydrophobic fiber aeroges, 12 ~ 25 parts of hydrophobic effect material；
(2) prior to 40 ~ 55 DEG C, take acetic anhydride, acetone, konjac glucomannan processed material, water, composite hydrophobic fiber aeroge mixed in reaction kettle
It closes, with 450 ~ 700r/min, 40 ~ 60min of magnetic agitation, is warming up to 70 ~ 90 DEG C, hydrophobic effect material, auxiliary agent mixing is added, with 700
~ 1000r/min 1 ~ 3h of magnetic agitation, is cooled to room temperature, and isogel material takes gel material after -5 DEG C of 7 ~ 10h of refrigerator cold-storage, moves to
Freeze drier in -40 DEG C dry 20 ~ for 24 hours, obtain composite aerogel, composite aerogel taken under protection of argon gas, in 900 ~ 1050
DEG C 4 ~ 6h of thermal cracking is to get compound oil absorption material.
Reagent A: it is that 12% urea liquid is mixed that 3:10 in mass ratio, which takes the NaOH solution that mass fraction is 10%, mass fraction,
It closes, in -10 DEG C of DEG C of refrigerator cold-storages to get reagent A.
Reagent B: 1:1 in mass ratio takes ethyl acetate, castor oil mixing to get reagent B.
Pre-treating fly ash: taking flyash 1:12 in mass ratio that the sodium carbonate liquor that mass fraction is 8% is added and mix, with
400r/min stirs 30min, and filtering takes filter residue 7:2 in mass ratio that polyvinylpyrrolidone mixing is added to get pretreatment fine coal
Ash.
Intercalator: 5:1 in mass ratio takes cetyl trimethylammonium bromide, neopelex mixing to get slotting
Layer agent.
Additive: 1:4 in mass ratio takes lecithin, n-butanol mixing to get additive.
Konjac glucomannan processed material: taking wheat bran to crushed 200 meshes in pulverizer, and sieving particle 1:10:3 in mass ratio is taken to be added
Mass fraction be 8% NaOH solution, konjaku flour mixing, with 400r/min 30 ~ 55min of magnetic agitation, be stored at room temperature 2h, filter,
Take filter cake in the dry 12h of -40 DEG C of freeze driers to get konjac glucomannan processed material.
Auxiliary agent: 1:4 in mass ratio takes bacteria cellulose, microcrystalline wax mixing to get auxiliary agent.
The preparation method of composite hydrophobic fiber aeroge, includes the following steps:
(1) for taking cotton fiber after the dry 8h of 60 DEG C of vacuum ovens, nanometer Fe is added in 3:0.1:15 in mass ratio3O4, reagent A it is mixed
It closes, with 500r/min magnetic agitation 35min, is transferred to centrifuge with 3000r/min centrifugal treating 10min, removal centrifugation object obtains fine
Plain liquid to be tieed up, in 35 DEG C of water-bath, takes cellulose solution that the N of cellulose solution quality 1% is added, N- methylene-bisacrylamide mixes, with
400r/min magnetic agitation 30min, is stored at room temperature 4h, obtains hydrogel, water intaking gel with after deionized water water washing 2 times, move to-
The dry 4h of 40 DEG C of freeze driers, obtains cross filament hydrogel；
(2) cross filament hydrogel is taken, in closed drier, and one is placed in the drier and contains 1mL methyl three
The closed progress Silanization reaction 20h of drier room temperature is obtained silanization aeroge, takes silanization gas by the open cuvette of chlorosilane
After gel 5:0.3:1 in mass ratio pre-treating fly ash, reagent B are coated, the dry 6h of 50 DEG C of vacuum ovens is moved to, i.e.,
Obtain composite hydrophobic fiber aeroge.
The preparation of hydrophobic effect material: in 25 DEG C, formamide, intercalator mixing is added in water intaking talcum 1:8:0.3 in mass ratio,
With 220r/min shaking table stirring 2 days, the MnO of hydrotalcite quality 4% is added2Mixing stirs 10h with 250r/min shaking table, water is added
The acetone mixing that 25 times of talcum quality, is stored at room temperature 1h, moves to centrifuge with 3000r/min centrifugal treating 10min, take centrifugation object
After washes of absolute alcohol 2 times, in 65 DEG C of vacuum drying 8h, dried object is obtained, takes dried object 8:1 in mass ratio that additive is added mixed
It closes to get hydrophobic effect material.
A kind of compound oil absorption material, according to the mass fraction, including following component, 10 parts of acetic anhydrides, 8 parts of acetone, 12 parts of evil spirits
Taro glue processed material, 2 parts of auxiliary agents, 30 parts of water, 25 parts of composite hydrophobic fiber aeroges, 12 parts of hydrophobic effect material.
A kind of preparation method of compound oil absorption material, includes the following steps:
(1) according to the mass fraction, 10 parts of acetic anhydrides, 8 parts of acetone, 12 parts of konjac glucomannan processed materials, 2 parts of auxiliary agents, 30 parts of water, 25 parts are taken
Composite hydrophobic fiber aeroge, 12 parts of hydrophobic effect material；
(2) prior to 40 DEG C, acetic anhydride, acetone, konjac glucomannan processed material, water, composite hydrophobic fiber aeroge is taken to mix in reaction kettle,
With 450r/min magnetic agitation 40min, 70 DEG C are warming up to, hydrophobic effect material, auxiliary agent mixing is added, with 700r/min magnetic agitation
1h is cooled to room temperature, and isogel material takes gel material after -5 DEG C of refrigerator cold-storage 7h, moves to freeze drier in -40 DEG C of dryings
20h obtains composite aerogel, takes composite aerogel under protection of argon gas, in 900 DEG C of thermal cracking 4h to get compound oil absorption material.
Reagent A: it is that 12% urea liquid is mixed that 3:13 in mass ratio, which takes the NaOH solution that mass fraction is 10%, mass fraction,
It closes, in -10 DEG C of DEG C of refrigerator cold-storages to get reagent A.
Reagent B: 1:2 in mass ratio takes ethyl acetate, castor oil mixing to get reagent B.
Pre-treating fly ash: taking flyash 1:16 in mass ratio that the sodium carbonate liquor that mass fraction is 8% is added and mix, with
500r/min stirs 45min, and filtering takes filter residue 12:2 in mass ratio that polyvinylpyrrolidone mixing is added to get pretreatment powder
Coal ash.
Intercalator: 5:2 in mass ratio takes cetyl trimethylammonium bromide, neopelex mixing to get slotting
Layer agent.
Additive: 1:6 in mass ratio takes lecithin, n-butanol mixing to get additive.
Konjac glucomannan processed material: taking wheat bran to crushed 200 meshes in pulverizer, and sieving particle 1:13:3 in mass ratio is taken to be added
Mass fraction be 8% NaOH solution, konjaku flour mixing, with 500r/min magnetic agitation 45min, be stored at room temperature 3h, filter, take
Filter cake is in the dry 13h of -40 DEG C of freeze driers to get konjac glucomannan processed material.
Auxiliary agent: 1:5 in mass ratio takes bacteria cellulose, microcrystalline wax mixing to get auxiliary agent.
The preparation method of composite hydrophobic fiber aeroge, includes the following steps:
(1) for taking cotton fiber after the dry 10h of 70 DEG C of vacuum ovens, nanometer Fe is added in 3:0.2:20 in mass ratio3O4, reagent A
Mixing is transferred to centrifuge with 700r/min magnetic agitation 50min with 3500r/min centrifugal treating 13min, removal centrifugation object obtains
Cellulose solution takes cellulose solution that the N of cellulose solution quality 3% is added in 40 DEG C of water-bath, and N- methylene-bisacrylamide mixes, with
500r/min magnetic agitation 45min, is stored at room temperature 5h, obtains hydrogel, water intaking gel with after deionized water water washing 3 times, move to-
The dry 5h of 40 DEG C of freeze driers, obtains cross filament hydrogel；
(2) cross filament hydrogel is taken, in closed drier, and one is placed in the drier and contains 2mL methyl three
The closed progress Silanization reaction 22h of drier room temperature is obtained silanization aeroge, takes silanization gas by the open cuvette of chlorosilane
After gel 6:0.3:1 in mass ratio pre-treating fly ash, reagent B are coated, the dry 8h of 60 DEG C of vacuum ovens is moved to, i.e.,
Obtain composite hydrophobic fiber aeroge.
The preparation of hydrophobic effect material: in 30 DEG C, it is mixed that formamide, intercalator is added in water intaking talcum 1:13:0.3 in mass ratio
It closes, with 280r/min shaking table stirring 3 days, the MnO of hydrotalcite quality 6% is added2Mixing is stirred 12h with 300r/min shaking table, is added
Enter 30 times of hydrotalcite quality acetone mixing, be stored at room temperature 2h, move to centrifuge with 3500r/min centrifugal treating 14min, take from
Heart object, in 70 DEG C of vacuum drying 10h, obtains dried object with after washes of absolute alcohol 3 times, and dried object 10:1 in mass ratio addition is taken to add
Agent is added to mix to get hydrophobic effect material.
A kind of compound oil absorption material, according to the mass fraction, including following component, 13 parts of acetic anhydrides, 12 parts of acetone, 16 parts of evil spirits
Taro glue processed material, 4 parts of auxiliary agents, 40 parts of water, 30 parts of composite hydrophobic fiber aeroges, 20 parts of hydrophobic effect material.
A kind of preparation method of compound oil absorption material, includes the following steps:
(1) according to the mass fraction, 13 parts of acetic anhydrides, 12 parts of acetone, 18 parts of konjac glucomannan processed materials, 4 parts of auxiliary agents, 40 parts of water, 30 are taken
Part composite hydrophobic fiber aeroge, 18 parts of hydrophobic effect material；
(2) prior to 45 DEG C, acetic anhydride, acetone, konjac glucomannan processed material, water, composite hydrophobic fiber aeroge is taken to mix in reaction kettle,
With 500r/min magnetic agitation 50min, 80 DEG C are warming up to, hydrophobic effect material, auxiliary agent mixing is added, with 900r/min magnetic agitation
2h is cooled to room temperature, and isogel material takes gel material after -5 DEG C of refrigerator cold-storage 8h, moves to freeze drier in -40 DEG C of dryings
22h obtains composite aerogel, takes composite aerogel under protection of argon gas, in 1000 DEG C of thermal cracking 5h to get compound oil absorption material.
Reagent A: it is that 12% urea liquid is mixed that 3:16 in mass ratio, which takes the NaOH solution that mass fraction is 10%, mass fraction,
It closes, in -10 DEG C of DEG C of refrigerator cold-storages to get reagent A.
Reagent B: 1:3 in mass ratio takes ethyl acetate, castor oil mixing to get reagent B.
Pre-treating fly ash: taking flyash 1:18 in mass ratio that the sodium carbonate liquor that mass fraction is 8% is added and mix, with
600r/min stirs 55min, and filtering takes filter residue 14:2 in mass ratio that polyvinylpyrrolidone mixing is added to get pretreatment powder
Coal ash.
Intercalator: 5:3 in mass ratio takes cetyl trimethylammonium bromide, neopelex mixing to get slotting
Layer agent.
Additive: 1:8 in mass ratio takes lecithin, n-butanol mixing to get additive.
Konjac glucomannan processed material: taking wheat bran to crushed 200 meshes in pulverizer, and sieving particle 1:16:3 in mass ratio is taken to be added
Mass fraction be 8% NaOH solution, konjaku flour mixing, with 700r/min magnetic agitation 55min, be stored at room temperature 4h, filter, take
Filter cake is in the dry 16h of -40 DEG C of freeze driers to get konjac glucomannan processed material.
Auxiliary agent: 1:6 in mass ratio takes bacteria cellulose, microcrystalline wax mixing to get auxiliary agent.
The preparation method of composite hydrophobic fiber aeroge, includes the following steps:
(1) for taking cotton fiber after the dry 12h of 80 DEG C of vacuum ovens, nanometer Fe is added in 3:0.3:25 in mass ratio3O4, reagent A
Mixing is transferred to centrifuge with 800r/min magnetic agitation 60min with 4000r/min centrifugal treating 15min, removal centrifugation object obtains
Cellulose solution takes cellulose solution that the N of cellulose solution quality 4% is added in 50 DEG C of water-bath, and N- methylene-bisacrylamide mixes, with
700r/min magnetic agitation 55min, is stored at room temperature 6h, obtains hydrogel, water intaking gel with after deionized water water washing 4 times, move to-
The dry 6h of 40 DEG C of freeze driers, obtains cross filament hydrogel；
(2) cross filament hydrogel is taken, in closed drier, and one is placed in the drier and contains 3mL methyl three
The open cuvette of chlorosilane for 24 hours by the closed progress Silanization reaction of drier room temperature obtains silanization aeroge, takes silanization gas
After gel 8:0.3:1 in mass ratio pre-treating fly ash, reagent B are coated, the dry 10h of 70 DEG C of vacuum ovens is moved to,
Up to composite hydrophobic fiber aeroge.
The preparation of hydrophobic effect material: in 35 DEG C, it is mixed that formamide, intercalator is added in water intaking talcum 1:15:0.3 in mass ratio
It closes, with 300r/min shaking table stirring 4 days, the MnO of hydrotalcite quality 8% is added2Mixing is stirred 14h with 320r/min shaking table, is added
Enter 40 times of hydrotalcite quality acetone mixing, be stored at room temperature 3h, move to centrifuge with 4000r/min centrifugal treating 16min, take from
Heart object, in 80 DEG C of vacuum drying 12h, obtains dried object with after washes of absolute alcohol 4 times, and dried object 12:1 in mass ratio addition is taken to add
Agent is added to mix to get hydrophobic effect material.
A kind of compound oil absorption material, according to the mass fraction, including following component, 15 parts of acetic anhydrides, 14 parts of acetone, 20 parts of evil spirits
Taro glue processed material, 5 parts of auxiliary agents, 50 parts of water, 50 parts of composite hydrophobic fiber aeroges, 25 parts of hydrophobic effect material.
A kind of preparation method of compound oil absorption material, includes the following steps:
(1) according to the mass fraction, 15 parts of acetic anhydrides, 14 parts of acetone, 20 parts of konjac glucomannan processed materials, 5 parts of auxiliary agents, 50 parts of water, 50 are taken
Part composite hydrophobic fiber aeroge, 25 parts of hydrophobic effect material；
(2) prior to 55 DEG C, acetic anhydride, acetone, konjac glucomannan processed material, water, composite hydrophobic fiber aeroge is taken to mix in reaction kettle,
With 700r/min magnetic agitation 60min, 90 DEG C are warming up to, hydrophobic effect material, auxiliary agent mixing is added, is stirred with 1000r/min magnetic force
3h is mixed, room temperature is cooled to, isogel material takes gel material after -5 DEG C of refrigerator cold-storage 10h, and it is dry in -40 DEG C to move to freeze drier
It is dry to obtain composite aerogel for 24 hours, composite aerogel is taken under protection of argon gas, in 1050 DEG C of thermal cracking 6h to get compound oil suction material
Material.
Comparative example 1: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking composite hydrophobic fiber airsetting
Glue.
Comparative example 2: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking hydrophobic effect material.
Comparative example 3: the compound oil absorption material of company of Gongyi City production.
By compound oil absorption material obtained by embodiment and comparative example according to FZ/T 01130-2016 standard, compound porous suction is taken
Light wood material shape sample size is 5mm × 5mm × 5mm, and is weighed, and M0 is denoted as；Then sample is immersed in vegetable oil at room temperature
In, sample is taken out after 15min, is placed on stainless steel mesh screen, is allowed after its drop 60s that hangs down naturally, is re-weighed, is denoted as M1；Each sample
It repeats above operation 3 times to be averaged, as oil absorption.Test result is as shown in table 1.
Table 1
Compound oil absorption material produced by the present invention has very strong adsorption capacity to oil product, and density is small, good mechanical property, makes
With convenience, high recycling rate, long service life, there are good market prospects.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of compound oil absorption material, according to the mass fraction, including following component, 10 ~ 15 parts of acetic anhydrides, 8 ~ 14 parts of acetone, 12 ~
20 parts of konjac glucomannan processed materials, 2 ~ 5 parts of auxiliary agents, 30 ~ 50 parts of water, which is characterized in that further include: 25 ~ 50 parts of composite hydrophobic fiber gas
Gel, 12 ~ 25 parts of hydrophobic effect material.
2. a kind of compound oil absorption material according to claim 1, which is characterized in that the system of the composite hydrophobic fiber aeroge
Preparation Method includes the following steps:
(1) taking cotton fiber is dry, and nanometer Fe is added in 3:0.1 ~ 0.3:15 in mass ratio ~ 253O4, reagent A be mixed, centrifugation, go
Except centrifugation object, cellulose solution is obtained, in 35 ~ 50 DEG C, takes cellulose solution that the N of cellulose solution quality 1 ~ 4%, N- di-2-ethylhexylphosphine oxide third is added
Acrylamide is mixed, and is stored at room temperature, and obtains hydrogel, water intaking gel washing, and freeze-drying obtains cross filament hydrogel；
(2) it takes cross filament hydrogel in closed drier, one is placed in the drier and contains 1 ~ 3mL methyl trichlorine silicon
The open cuvette of alkane, room temperature close drying device progress Silanization reaction 20 ~ for 24 hours, silanization aeroge is obtained, silanization aeroge is taken
The pre-treating fly ash of 5 ~ 8:0.3:1 in mass ratio, reagent B are coated, and are dried in vacuo to get composite hydrophobic fiber airsetting
Glue.
3. a kind of compound oil absorption material according to claim 2, which is characterized in that the reagent A in the step (1): pressing matter
Amount takes NaOH solution, urea liquid mixing than 3:10 ~ 16, refrigerates to get reagent A.
4. a kind of compound oil absorption material according to claim 2, which is characterized in that the pretreatment fine coal in the step (2)
Ash: it takes flyash 1:12 in mass ratio ~ 18 that sodium carbonate liquor is added and is mixed, filtering takes filter residue 7 ~ 14:2 in mass ratio to add
Enter polyvinylpyrrolidone mixing to get pre-treating fly ash.
5. a kind of compound oil absorption material according to claim 2, which is characterized in that the reagent B in the step (2): pressing matter
Amount takes ethyl acetate, castor oil mixing to get reagent B than 1:1 ~ 3.
6. a kind of compound oil absorption material according to claim 1, which is characterized in that the preparation of the hydrophobic effect material: in 25 ~
35 DEG C, formamide, intercalator mixing is added in water intaking talcum 1:8 ~ 15:0.3 in mass ratio, is stirred with shaking table, hydrotalcite matter is added
The MnO of amount 4 ~ 8%2Mixing, shaking table stirring, be added 25 ~ 40 times of hydrotalcite quality acetone mixing, be stored at room temperature, be centrifuged, take from
Heart object washes of absolute alcohol, it is dry, dried object is obtained, takes dried object 8 ~ 12:1 in mass ratio that additive mixing is added to get dredging
Water makees materials.
7. a kind of compound oil absorption material according to claim 6, which is characterized in that the intercalator: 5:1 ~ 3 take in mass ratio
Cetyl trimethylammonium bromide, neopelex mixing are to get intercalator.
8. a kind of compound oil absorption material according to claim 6, which is characterized in that the additive: 1:4 ~ 8 take in mass ratio
Lecithin, n-butanol mixing are to get additive.
9. a kind of compound oil absorption material according to claim 1, which is characterized in that the konjac glucomannan processed material: take wheatfeed
Broken sieving takes sieving particle 1:10 ~ 16:3 in mass ratio that NaOH solution, konjaku flour mixing is added, is stored at room temperature, filters,
Filter cake is taken to be freeze-dried to get konjac glucomannan processed material.
10. a kind of compound oil absorption material according to claim 1, which is characterized in that the auxiliary agent: 1:4 ~ 6 take in mass ratio
Bacteria cellulose, microcrystalline wax mixing are to get auxiliary agent.
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