CN110437494A - A kind of preparation method of super hydrophilic super oleophylic luffa sponge - Google Patents
A kind of preparation method of super hydrophilic super oleophylic luffa sponge Download PDFInfo
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- CN110437494A CN110437494A CN201910661168.XA CN201910661168A CN110437494A CN 110437494 A CN110437494 A CN 110437494A CN 201910661168 A CN201910661168 A CN 201910661168A CN 110437494 A CN110437494 A CN 110437494A
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- luffa
- sponge
- super
- preparation
- oleophylic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21D—TREATMENT OF THE MATERIALS BEFORE PASSING TO THE PAPER-MAKING MACHINE
- D21D1/00—Methods of beating or refining; Beaters of the Hollander type
- D21D1/02—Methods of beating; Beaters of the Hollander type
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
- C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08J2301/02—Cellulose; Modified cellulose
Abstract
The invention discloses a kind of preparation methods of super hydrophilic super oleophylic luffa sponge, vacuum drying is dehydrated it completely after luffa is removed seed and epidermis by this method, it is then ground to powder and successively removes hemicellulose with hydrogen peroxide removing lignin, with alkali, obtain pure biology cellulose, it is mixed later with water and carries out mechanical pulp, gained slurry makes it possess microcellular structure abundant through vacuum freeze drying condensation-crystallization subliming water, obtains the luffa sponge for having super hydrophilic super oil-wet behavior.Raw material of the present invention is easy to get, cost is relatively low, easy to operate, whole process it is pollution-free, without discharge under conditions of complete, prepared luffa sponge has excellent super hydrophilic super-oleophilic, has broad application prospects in the fields such as absorption, removal of impurities, filtering or damping, noise elimination.
Description
Technical field
The invention belongs to environment-friendlyplant plant material applied technical fields, and in particular to a kind of super hydrophilic super oleophylic luffa sponge
Preparation method.
Background technique
The luffa that the present invention uses is a kind of common plant, is a kind of not only hydrophilic but also oleophylic the extraordinary fibre of toughness
Endoplasmic reticular tissue is tieed up, can be applied by pre-treatment in industries such as life, industry, medicines and health protections.It can be as clear in life
The quality material of wash up can make the insole of sweat-absorbing breathable;Can industrially be fabricated to absorption, filtering, damping it is new
Type environment-friendly materials.At abroad, very widely used for luffa, excellent performance makes researcher in scientific research
It is favored to have and is added.But the utilization of luffa hydrophilic and oleophilic property is but rarely reported.
Currently, the application about luffa, mainly utilizes the performance of reticular structure, it is usually to use physical method
Raw material is carried out to the change of form, for example is prepared into insole, mattress etc. daily necessity;Some researchers are by pre-treatment to silk
Melon network is processed, but this processing method is excessively coarse, just with the hole of the original reticular structure of luffa, not
There is the property using its hydrophilic and oleophilic;It is industrial then be to be modified luffa, it is assigned by the method for physics and chemistry
His property, for example prepare oleophilic oil material and be used for the industrial material of the absorption of Crude oil from CNOOC leakage, water quality pollutant absorption etc.
Material, there is no parents' performances excellent using its script well for this treating method.And modification can destroy luffa
Good intrinsic performance can also generate waste water, waste material during the preparation process, and certain damage is caused to environment.
Summary of the invention
The purpose of the present invention is overcoming the hydrophilic and oleophilic material used on the market to belong to organic synthesis material, to environment and people
Class health has certain harm, and has the shortcomings that at high cost, preparation process is complicated, residual sample is difficult to degrade, provides one
Kind of raw material is easy to get, low cost, the preparation method for being simple to operate and friendly to environment type hydrophilic and oleophilic luffa sponge.
Technical solution used by above-mentioned technical problem is solved to comprise the steps of:
1, it pre-processes
It is blocking by being sheared after luffa removal seed and epidermis, it is rinsed 2~3 times with deionized water, then vacuum drying makes
It is dehydrated completely, then pulverizes, and obtains luffa vegetable sponge.
2, lignin is removed
The H that mass concentration is 2%~7% is added in luffa vegetable sponge2O2In aqueous solution and adjust pH value be faintly acid, In
Stewing process 30~60 minutes at 40~85 DEG C;It repeats the operation 3~5 times.
3, hemicellulose is removed
The luffa vegetable sponge that step 2 obtains is rinsed well with deionized water and is placed on mass concentration as 1%~10%
In sodium hydroxide or potassium hydroxide aqueous solution, stewing process 2~5 hours at 60~100 DEG C.
4, it purifies
The luffa vegetable sponge that step 3 is obtained continues the operation of step 2 and step 3, and repetitive operation 2~3 times, into one
Step removing lignin and hemicellulose;Then the pH of solution is adjusted to neutrality, and is rinsed luffa vegetable sponge with deionized water
Completely, loofah fiber element powder is obtained.
5, it is beaten
The loofah fiber element powder that step 4 is obtained is added deionized water and carries out mechanical pulp, and gained slurry carries out true
Vacuum freecing-dry obtains luffa sponge.
In above-mentioned steps 1, preferably vacuum drying temperature is 70~90 DEG C, and the time is 12~24 hours.
In above-mentioned steps 1, the size of the luffa vegetable sponge is 30~50 mesh.
In above-mentioned steps 2, the H that mass concentration is 3%~5% preferably is added in luffa vegetable sponge2O2In aqueous solution and adjust
PH value is faintly acid, stewing process 30~60 minutes at 65~80 DEG C, wherein the luffa vegetable sponge and H2O2The matter of aqueous solution
Amount-volume ratio is preferably 1g:15~30mL.
It is further preferably 4~5 with citric acid or acetic acid or salt acid for adjusting pH value in above-mentioned steps 2.
In above-mentioned steps 3 well, luffa vegetable sponge that step 2 obtains preferably rinsed to be placed on quality dense with deionized water
In the aqueous alkali that degree is 2%~5%, stewing process 2~3 hours at 80~90 DEG C.
In above-mentioned steps 3, quality-volume ratio of preferably luffa vegetable sponge and sodium hydroxide or potassium hydroxide aqueous solution is
1g:15~30mL.
In above-mentioned steps 5, preferably quality-volume ratio of loofah fiber element powder and deionized water is 1g:15~25mL.
In above-mentioned steps 5, the time of the machinery pulp is 10~30 minutes, and the time of vacuum freeze drying is 24~48
Hour.
The invention has the following outstanding advantages:
The luffa that the present invention uses is a kind of natural porous structure material, itself has the characteristic of hydrophilic and oleophilic, base
It is beaten and freezes dry after passing it through pretreatment and removing lignin, hemicellulose in the property for keeping luffa originally excellent
It is dry to make it that spongiform form be presented.The luffa green non-pollution that the present invention uses, and it is common in life be easy to get, it is low at
This, the method for use is easy to operate, no waste pollution, and no noxious material generates, and realizes environmentally protective natural super hydrophilic
The preparation of super oleophylic luffa sponge.Gained luffa sponge quality of the invention is small, and density is light, equal for the absorbability of grease
It is very good, there is higher absorption property compared with luffa itself.
Detailed description of the invention
Fig. 1 is the infrared spectrogram of the luffa sponge of luffa raw material and the preparation of embodiment 1.
Fig. 2 is the XRD diagram of luffa sponge prepared by embodiment 1.
Fig. 3 is the scanning electron microscope (SEM) photograph of luffa raw material in embodiment 1.
Fig. 4 is the scanning electron microscope (SEM) photograph of luffa sponge prepared by embodiment 1.
Fig. 5 is the contact angle test figure of luffa sponge prepared by embodiment 1.
Fig. 6 is figure compared with luffa sponge prepared by embodiment 1 absorbs water oil suction multiplying power with cotton.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to
These embodiments.
Embodiment 1
1, it pre-processes
After the seed of column luffa and epidermis removal, the fritter of 3cm × 3cm × 0.5cm or so is cut into scissors, and
With deionized water repeated flushing 2~3 times, until free from admixture.Then the blocky luffa rinsed well vacuum is put into do
It is dried in vacuo 12 hours in dry case at 90 DEG C, is dehydrated it completely.Finally by dewatered blocky luffa in plant pulverizer
In be polished into 30 mesh powders, i.e., acquisition luffa vegetable sponge.
2, lignin is removed
It weighs 5g luffa vegetable sponge to be added in beaker, the H that 100mL mass concentration is 3% is added2O2Aqueous solution, and use lemon
Acid for adjusting pH value is 4.5, stewing process 60 minutes under the conditions of 75 DEG C in constent temperature heater.Suction filtration, gained sponge gourd after having handled
Network powder uses H in this way again2O2Reprocessing 4 times, makes luffa vegetable sponge become white, and lignin removes substantially.
3, hemicellulose is removed
Luffa vegetable sponge that step 2 obtains is rinsed with deionized water after being neutrality to pH value, is placed in 100mL mass concentration
For in 3% NaOH aqueous solution, stewing process 3 hours, removes hemicellulose substantially under the conditions of 90 DEG C.
4, it purifies
The luffa vegetable sponge that step 3 is obtained repeats the behaviour of step 2 and step 3 removing lignin and hemicellulose
Make, repetitive operation 2 times, obtains loofah fiber element powder.
5, it is beaten
100mL deionized water is added in the loofah fiber element powder that step 4 is obtained, and mechanical pulp is carried out in beater
30 minutes, until slurry is uniformly without layering;Gained slurry pours into vacuum freeze drying 48 hours in beaker, obtains luffa sea
It is continuous.
Luffa sponge is characterized using infrared spectrometer, X-ray diffractometer, scanning electron microscope.In the infrared light of Fig. 1
In spectrum, luffa sponge is in 1503cm-1Locate corresponding lignin molecule phenyl ring C=C double bond stretching vibration peak and 1732cm-1Place
The C=O stretching vibration peak of corresponding lignin and hemicellulose obviously weakens, and illustrates that most of hemicellulose and lignin are removed
It goes.The cellulose crystal form of luffa sponge belongs to cellulose I type it can be seen from the XRD spectrum of Fig. 2.Comparison diagram 3 and Fig. 4's
Scanning electron microscope result as it can be seen that luffa individual fiber surface has porous structure, and it is internal there is hollow duct, fiber it
Between also there is interval abundant, gained luffa sponge maintains the original structure of luffa, and it is excellent that this is to confer to luffa sponge
The basis of good absorption property.Next, carry out contact angle test to luffa sponge, as a result visible Fig. 5, as the result is shown its
Jiang Shui and oil fully absorb in 3s, illustrate it with excellent parents' performance.
Embodiment 2
1, it pre-processes
After the seed of column luffa and epidermis removal, the fritter of 4cm × 4cm × 0.5cm or so is cut into scissors, and
With deionized water repeated flushing 2~3 times, until free from admixture.Then the blocky luffa rinsed well vacuum is put into do
It is dried in vacuo 18 hours in dry case at 80 DEG C, is dehydrated it completely.Finally by dewatered blocky luffa in plant pulverizer
In be polished into 40 mesh powders, i.e., acquisition luffa vegetable sponge.
2, lignin is removed
It weighs 3g luffa vegetable sponge to be added in beaker, the H that 60mL mass concentration is 4% is added2O2Aqueous solution, and use lemon
Acid for adjusting pH value is 4.8, stewing process 50 minutes under the conditions of 80 DEG C in constent temperature heater.Suction filtration, gained sponge gourd after having handled
Network powder uses H in this way again2O2Reprocessing 3 times, makes luffa vegetable sponge become white, and lignin removes substantially.
3, hemicellulose is removed
Luffa vegetable sponge that step 2 obtains is rinsed with deionized water after being neutrality to pH value, is placed in 60mL mass concentration
For in 4% NaOH aqueous solution, stewing process 2.5 hours, removes hemicellulose substantially under the conditions of 80 DEG C.
4, it purifies
The luffa vegetable sponge that step 3 is obtained repeats the behaviour of step 2 and step 3 removing lignin and hemicellulose
Make, repetitive operation 2 times, obtains loofah fiber element powder.
5, it is beaten
50mL deionized water is added in the loofah fiber element powder that step 4 is obtained, and mechanical pulp is carried out in beater
20 minutes, until slurry is uniformly without layering;Gained slurry pours into vacuum freeze drying 36 hours in beaker, obtains luffa sea
It is continuous.
Embodiment 3
1, it pre-processes
After the seed of column luffa and epidermis removal, the fritter of 5cm × 5cm × 0.5cm or so is cut into scissors, and
With deionized water repeated flushing 2~3 times, until free from admixture.Then the blocky luffa rinsed well vacuum is put into do
It is dried in vacuo 24 hours in dry case at 70 DEG C, is dehydrated it completely.Finally by dewatered blocky luffa in plant pulverizer
In be polished into 30 mesh powders, i.e., acquisition luffa vegetable sponge.
2, lignin is removed
It weighs 4g luffa vegetable sponge to be added in beaker, the H that 80mL mass concentration is 5% is added2O2Aqueous solution, and use lemon
Acid for adjusting pH value is 5, stewing process 40 minutes under the conditions of 70 DEG C in constent temperature heater.Suction filtration, gained luffa after having handled
Powder uses H in this way again2O2Reprocessing 3 times, makes luffa vegetable sponge become white, and lignin removes substantially.
3, hemicellulose is removed
Luffa vegetable sponge that step 2 obtains is rinsed with deionized water after being neutrality to pH value, is placed in 80mL mass concentration
For in 5% NaOH aqueous solution, stewing process 2.5 hours, removes hemicellulose substantially under the conditions of 90 DEG C.
4, it purifies
The luffa vegetable sponge that step 3 is obtained repeats the behaviour of step 2 and step 3 removing lignin and hemicellulose
Make, repetitive operation 2 times, obtains loofah fiber element powder.
5, it is beaten
80mL deionized water is added in the loofah fiber element powder that step 4 is obtained, and mechanical pulp is carried out in beater
25 minutes, until slurry is uniformly without layering;Gained slurry pours into vacuum freeze drying 48 hours in beaker, obtains luffa sea
It is continuous.
In order to prove beneficial effects of the present invention, luffa sponge and luffa that inventor prepares above-described embodiment 1
Raw material carries out grease absorption property contrast test, the results are shown in Table 1 and table 2.
The oil absorbency test and comparison of luffa raw material and luffa sponge in 1 embodiment 1 of table
The water absorbing properties test and comparison of luffa raw material and luffa sponge in 2 embodiment 1 of table
As can be seen from the table, the water absorbent rate of luffa sponge and oil suction multiplying power are above luffa raw material, illustrate silk
Melon network sponge is improved significantly than the grease absorption property of luffa raw material.
Inventor further compares test to the grease absorption property of 1 gained luffa sponge of embodiment and cotton,
As a result visible Fig. 6.As seen from the figure, luffa sponge is apparently higher than cotton to the absorbency of different solvents, further confirms it
The property of super hydrophilic super oleophylic.
Claims (10)
1. a kind of preparation method of super hydrophilic super oleophylic luffa sponge, it is characterised in that:
(1) it pre-processes
It is blocking by being sheared after luffa removal seed and epidermis, it is rinsed 2~3 times with deionized water, then vacuum drying keeps its complete
Full dehydration, then pulverize, obtain luffa vegetable sponge;
(2) lignin is removed
The H that mass concentration is 2%~7% is added in luffa vegetable sponge2O2In aqueous solution and to adjust pH value be faintly acid, 40~
Stewing process 30~60 minutes at 85 DEG C;It repeats the operation 3~5 times;
(3) hemicellulose is removed
The luffa vegetable sponge that step (2) obtains is rinsed well with deionized water and is placed on the hydrogen that mass concentration is 1%~10%
In sodium oxide molybdena or potassium hydroxide aqueous solution, stewing process 2~5 hours at 60~100 DEG C;
(4) it purifies
The luffa vegetable sponge that step (3) obtains continues to the operation of step (2) and step (3), repetitive operation 2~3 times, into
One-step removal lignin and hemicellulose;Then the pH of solution is adjusted to neutrality, and is rushed luffa vegetable sponge with deionized water
Wash clean obtains loofah fiber element powder;
(5) it is beaten
The loofah fiber element powder that step (4) is obtained is added deionized water and carries out mechanical pulp, and gained slurry carries out vacuum
Freeze-drying, obtains luffa sponge.
2. the preparation method of super hydrophilic super oleophylic luffa sponge according to claim 1, it is characterised in that: step (1)
In, vacuum drying temperature is 70~90 DEG C, and the time is 12~24 hours.
3. the preparation method of super hydrophilic super oleophylic luffa sponge according to claim 1, it is characterised in that: step (1)
In, the size of the luffa vegetable sponge is 30~50 mesh.
4. the preparation method of super hydrophilic super oleophylic luffa sponge according to claim 1, it is characterised in that: step (2)
In, the H that mass concentration is 3%~5% is added in luffa vegetable sponge2O2In aqueous solution and pH value is adjusted for faintly acid, 65~80
Stewing process 30~60 minutes at DEG C.
5. the preparation method of super hydrophilic super oleophylic luffa sponge according to claim 1 or 4, it is characterised in that: step
(2) in, the luffa vegetable sponge and H2O2Quality-volume ratio of aqueous solution is 1g:15~30mL.
6. the preparation method of super hydrophilic super oleophylic luffa sponge according to claim 1 or 4, it is characterised in that: step
It (2) is 4~5 with citric acid or acetic acid or salt acid for adjusting pH value in.
7. the preparation method of super hydrophilic super oleophylic luffa sponge according to claim 1, it is characterised in that: step (3)
In, the luffa vegetable sponge that step (2) obtains is rinsed well with deionized water and is placed on the hydrogen-oxygen that mass concentration is 2%~5%
Change in sodium or potassium hydroxide aqueous solution, stewing process 2~3 hours at 80~90 DEG C.
8. the preparation method of super hydrophilic super oleophylic luffa sponge according to claim 1 or claim 7, it is characterised in that: step
(3) in, the luffa vegetable sponge is 1g:15~30mL with quality-volume ratio of sodium hydroxide or potassium hydroxide aqueous solution.
9. the preparation method of super hydrophilic super oleophylic luffa sponge according to claim 1, it is characterised in that: step (5)
In, quality-volume ratio of the loofah fiber element powder and deionized water is 1g:15~25mL.
10. according to claim 1 or the preparation method of super hydrophilic super oleophylic luffa sponge described in 9, it is characterised in that: step
(5) in, the time of the machinery pulp is 10~30 minutes, and the time of vacuum freeze drying is 24~48 hours.
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Cited By (3)
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CN112169379A (en) * | 2020-10-22 | 2021-01-05 | 陕西师范大学 | Biomass airbag/TiO with floating oil absorption2Composite material |
CN114369959A (en) * | 2021-12-27 | 2022-04-19 | 中恒大耀纺织科技有限公司 | Anti-leakage multilayer composite fabric capable of actively eliminating old people odor and preparation method thereof |
CN115449902A (en) * | 2022-09-02 | 2022-12-09 | 香港中文大学(深圳) | Natural fiber and preparation method and application thereof |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112169379A (en) * | 2020-10-22 | 2021-01-05 | 陕西师范大学 | Biomass airbag/TiO with floating oil absorption2Composite material |
CN112169379B (en) * | 2020-10-22 | 2022-04-12 | 陕西师范大学 | Biomass airbag/TiO with floating oil absorption2Composite material |
CN114369959A (en) * | 2021-12-27 | 2022-04-19 | 中恒大耀纺织科技有限公司 | Anti-leakage multilayer composite fabric capable of actively eliminating old people odor and preparation method thereof |
CN114369959B (en) * | 2021-12-27 | 2023-11-10 | 中恒大耀纺织科技有限公司 | Anti-seepage multilayer composite fabric capable of actively eliminating odor of old people and preparation method thereof |
CN115449902A (en) * | 2022-09-02 | 2022-12-09 | 香港中文大学(深圳) | Natural fiber and preparation method and application thereof |
CN115449902B (en) * | 2022-09-02 | 2023-10-10 | 香港中文大学(深圳) | Natural fiber and preparation method and application thereof |
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