CN106750368A - A kind of preparation method of wood fibre oil absorption material - Google Patents
A kind of preparation method of wood fibre oil absorption material Download PDFInfo
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- CN106750368A CN106750368A CN201611202403.XA CN201611202403A CN106750368A CN 106750368 A CN106750368 A CN 106750368A CN 201611202403 A CN201611202403 A CN 201611202403A CN 106750368 A CN106750368 A CN 106750368A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H8/00—Macromolecular compounds derived from lignocellulosic materials
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/32—Materials not provided for elsewhere for absorbing liquids to remove pollution, e.g. oil, gasoline, fat
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Abstract
The invention provides a kind of preparation method of wood fibre oil absorption material, wood fibre and esterifying reagent are carried out into esterification under pyridine catalytic action and ball milling condition, wood fibre oil absorption material is obtained, without using organic solvent in course of reaction, product separation and purification treatment is simple, and preparation technology is easy to operate, modification time is short, and the extent of reaction is high, there is preferable oil absorbing effect, adsorption rate to diesel oil is 9.86g/g, and the adsorption rate to soybean oil is 10.21g/g.
Description
Technical field
The present invention relates to biorefinery technical field, more particularly to a kind of preparation method of wood fibre oil absorption material.
Background technology
Wood fibre is a kind of environment-friendly renewable resource, the features such as possess rich reserves and fast reproduction speed.Its
Middle wood raw material has been widely used in the fields such as construction industry, house fitting-up and paper industry, and wheat straw, agricultural crop straw, fruit
The agricultural residues such as shell pollute of a relatively high due to its slurrying, are progressively eliminated by paper industry, and its process problem is still urgently solved
Certainly.
Wood fibre plant cell wall is made up of three big main components, i.e. cellulose, hemicellulose and lignin, cellulose
On hydroxyl there is hydrophily, therefore in the case where there is moisture, non-modified wood fiber biomass raw material mechanicalness
Can easily be changed with mode of appearance, be also easy to be degraded by microorganisms or corrode.By chemical modification by hydrophobic alkane group
Cellulose surface is incorporated into, its hydrophily can be improved and it is possessed preferable oil absorbency.
The preparation method of wood fibre oil absorption material is broadly divided into homogeneous modified and traditional heterogeneous modification in the prior art
Two kinds.Homogeneous modified system is that wood fibre is dissolved in into the cellulose solvent system such as organic solvent, so that effectively disperse fiber,
And then reaction efficiency is improved, but have that consumption of organic solvent is high and price is prohibitively expensive, and it is harmful, be not suitable for industry
What metaplasia was produced.
The content of the invention
In view of this, it is an object of the invention to provide a kind of preparation method of wood fibre oil absorption material, using ball milling
The high-energy of generation provides activation energy for reaction, while effectively disperse fiber, so as to improve reaction efficiency.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
A kind of preparation method of wood fibre oil absorption material, comprises the following steps：
Wood fibre and esterifying reagent are carried out into esterification under pyridine catalytic action and ball milling condition, wooden fibre is obtained
Dimension oil absorption material.
Preferably, the temperature of the ball milling is 20~30 DEG C.
Preferably, the rotating speed of the ball milling is 800~1200rpm, and the time of the ball milling is 2~4h.
Preferably, the esterifying reagent includes acid anhydrides or acyl chlorides.
Preferably, the acid anhydrides includes acetic anhydride, propionic andydride or butyric anhydride.
Preferably, the acyl chlorides includes chloroacetic chloride, propionyl chloride or butyl chloride.
Preferably, the esterifying reagent and the mass ratio of wood fibre are 0.25~3.5：1.
Preferably, the pyridine and the mass ratio of wood fibre are 0.25~3：1.
Preferably, the wood fibre is obtained by the extracting of wood fiber biomass raw material, and the solvent for using that extracts is
The volume ratio of toluene and alcohol mixed solvent, the toluene and ethanol is 2:1.
Preferably, the wood fiber biomass raw material includes Eucalyptus, poplar, pine, bamboo, bagasse, straw, corn
The mixture of one or more in bar and straw.
Preferably, also include after the esterification：The product of the esterification is washed and dried successively.
Preferably, the dry temperature is 50~110 DEG C, and the dry time is 24~48h.
The invention provides a kind of preparation method of wood fibre oil absorption material, by wood fibre and esterifying reagent in pyridine
Esterification is carried out under catalytic action and ball milling condition, wood fibre oil absorption material is obtained, without using organic in course of reaction
Solvent, product separation and purification treatment is simple, and preparation technology is easy to operate, and modification time is short, and the extent of reaction is high, there is preferably suction
Oily effect, the adsorption rate to diesel oil is 9.86g/g, and the adsorption rate to soybean oil is 10.21g/g.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is bagasse, the scanning electron microscope (SEM) photograph of differential responses time bagasse after the embodiment of the present invention 1 is extracted；
Fig. 2 is the infrared spectrum spectrogram of bagasse and bagasse acetic acid esters after the ball milling of the embodiment of the present invention 1；
Fig. 3 is the infrared spectrum spectrogram of bagasse and bagasse propionic ester after the ball milling of the embodiment of the present invention 2；
Fig. 4 is the infrared spectrum spectrogram of bagasse and bagasse butyrate after the ball milling of the embodiment of the present invention 3；
Fig. 5 is the infrared spectrum spectrogram of bagasse and bagasse acetic acid esters after the ball milling of the embodiment of the present invention 4.
Specific embodiment
The invention provides a kind of preparation method of wood fibre oil absorption material, comprise the following steps：
Wood fibre and esterifying reagent are carried out into esterification under pyridine catalytic action and ball milling condition, wooden fibre is obtained
Dimension oil absorption material.
The present invention does not have any specifically limited to the source of the wood fibre, using wood well known to those skilled in the art
The source or commercial goods of matter fiber；Institute is preferably obtained by the extracting of wood fiber biomass raw material in embodiments of the present invention
State wood fibre, the solvent that the extracting is used is toluene and alcohol mixed solvent, the volume ratio of the toluene and ethanol is 2:
1。
In the present invention, the time of the extracting be preferably 10~12h, more preferably 11~11.5h；The temperature of the extracting
Degree is preferably 85~95 DEG C, more preferably 88~90 DEG C.
The present invention does not have any special limitation to the device of the extracting, using extracting well known to those skilled in the art
Device；Preferably it is stripped in Soxhlet extractor in embodiments of the present invention.
In the present invention, the wood fiber biomass raw material include Eucalyptus, poplar, pine, bamboo, bagasse, straw,
The mixture of one or more in cornstalk and straw, the present invention is to each wood fiber biomass raw material in the mixture
Mass ratio does not have any special limitation, and those skilled in the art can according to actual needs select the wood fibre of any mass ratio
The mixture of biomass material.
In the present invention, the temperature of the ball milling is preferably 20~30 DEG C, more preferably 25~28 DEG C.
In the present invention, the rotating speed of the ball milling is preferably 800~1200rpm, more preferably 1000~1100rpm.
In the present invention, the time of the ball milling be preferably 2~4h, more preferably 3~3.5h.
In the present invention, the ball of the ball milling is preferably sized to 5~15mm, more preferably 7~10mm；The ratio of grinding media to material of ball milling
Preferably 40~60：1, more preferably 45~55：1.
The present invention does not have any special limitation to the equipment of the ball milling, using ball milling well known to those skilled in the art
Device；Carried out preferably in ball grinder in embodiments of the present invention.
In the present invention, the esterifying reagent is preferably 0.25~3.5 with the mass ratio of wood fibre：1, more preferably 1
~3：1, most preferably 2.5~2.8：1.
In the present invention, the pyridine is preferably 0.25~3 with the mass ratio of wood fibre：1, more preferably 1~2.5：
1, most preferably 1.5~2：1.
In the present invention, the esterifying reagent preferably includes acid anhydrides and/or acyl chlorides, when the esterifying reagent include acid anhydrides and
During two kinds of materials of acyl chlorides, the present invention does not have any special limitation to the mass ratio of acid anhydrides and acyl chlorides in the esterifying reagent, this
Art personnel can according to actual needs select the acid anhydrides of any mass ratio and the mixture of acyl chlorides.
In the present invention, the acid anhydrides preferably includes the one kind in acetic anhydride, propionic andydride and butyric anhydride.
In the present invention, the acyl chlorides preferably includes the one kind in chloroacetic chloride, propionyl chloride and butyl chloride.
After the esterification, the product of esterification is washed and dried successively described in preferred pair of the present invention, is obtained
Wood fibre oil absorption material.
In the present invention, it is described to wash one kind that the detergent for using is preferably included in deionized water, methyl alcohol and ethanol.
In the present invention, the pH value of the product of esterification is neutrality after the washing.
In the present invention, the dry temperature is preferably 50~110 DEG C, more preferably 70~100 DEG C, most preferably 90
~95 DEG C；The dry time is preferably 24~48h, most preferably more preferably 30~45h, 35~40h.
Obtained wood fibre oil absorption material of the invention can be used to eliminate the abandoned oil in environment.
The invention provides a kind of preparation method of wood fibre oil absorption material, by wood fibre and esterifying reagent in pyridine
Esterification is carried out under catalytic action and ball milling condition, wood fibre oil absorption material is obtained, without using organic in course of reaction
Solvent, product separation and purification treatment is simple, and preparation technology is easy to operate, and modification time is short, and the extent of reaction is high, there is preferably suction
Oily effect, the adsorption rate to diesel oil is 9.86g/g, and the adsorption rate to soybean oil is 10.21g/g.
The preparation method of the wood fibre oil absorption material provided the present invention with reference to embodiment is described in detail,
But they can not be interpreted as limiting the scope of the present invention.
Embodiment 1
It is 2 with the volume ratio of toluene and ethanol:1 mixed solution extracting bagasse, obtains bagasse raw material, takes 3mL second
The bagasse raw material that acid anhydrides, 3mL pyridines and 1g are crushed is placed in ball grinder, sets rotational speed of ball-mill as 1200rpm, in a continuous manner
Carry out 4h ball millings, using deionized water product wash repeatedly after prior to drying 12h in 70 DEG C of baking ovens, after be transferred to 105 DEG C of baking ovens
In continue to dry 12h and obtain bagasse acetic acid esters oil absorption material.
Bagasse after bagasse, reaction 4h after bagasse, reaction 2h after bagasse, reaction 0.5h after extracting is carried out respectively
Scanning electron microscope analysis, as a result as shown in figure 1, by after ball milling modification, the surface topography of bagasse there occurs change, bagasse quilt
Crush completely, fully increase bagasse surface area.
Through weighing, bagasse acetic acid esters oil absorption material rate of body weight gain is 33.3%, and the adsorption rate to diesel oil is 8.94g/g, right
The adsorption rate of soybean oil is 9.32g/g, and infrared spectrum detection is carried out to it, and acquired results are as shown in Figure 2.1745cm-1Place's ester bond
In C=O stretching vibration absworption peaks, 1375cm-1The characteristic absorption peak of methyl in place's acetyl group, and 1248cm-1In place's ester bond
The absworption peak of C-O keys substantially strengthen, show to be successfully introduced into acetyl group in sample, so as to reach oil absorbing effect.
Embodiment 2
It is 2 with the volume ratio of toluene and ethanol:1 mixed solution extracting bagasse, obtains bagasse raw material, takes 3.5mL
The bagasse raw material that propionic andydride, 2.1mL pyridines and 1g are crushed is placed in ball grinder, rotational speed of ball-mill as 800rpm is set, with continuous
Mode carries out 2h ball millings, using methyl alcohol by products therefrom wash repeatedly after prior to drying 12h in 90 DEG C of baking ovens, after be transferred to 110
Continue to dry 24h in DEG C baking oven and obtain bagasse propionic ester oil absorption material.
Through weighing, bagasse propionic ester oil absorption material rate of body weight gain is 33.6%, and the adsorption rate to diesel oil is 9.35g/g, right
The adsorption rate of soybean oil is 9.72g/g, and infrared spectrum detection is carried out to it, and acquired results are as shown in Figure 3.1745cm-1Place's ester bond
In C=O stretching vibration absworption peaks, 1462cm-1Locate the characteristic absorption peak of propiono, and 2985~2888cm-1Place occurs two
Individual saturation c h bond absworption peak, shows to be successfully introduced into propiono in sample, so as to reach oil absorbing effect.
Embodiment 3
It is 2 with the volume ratio of toluene and ethanol:1 mixed solution extracting bagasse, obtains bagasse raw material, takes 3.5mL
The bagasse raw material that butyric anhydride, 1.75mL pyridines and 1g are crushed is placed in ball grinder, sets rotational speed of ball-mill as 1000r/min, with
Continuation mode carries out 4h ball millings, using ethanol by products therefrom wash repeatedly after prior to drying 6h in 90 DEG C of baking ovens, after be transferred to
Continue to dry 24h in 95 DEG C of baking ovens and obtain bagasse butyrate oil absorption material.
Through weighing, bagasse butyrate oil absorption material rate of body weight gain is 32.4%, and the adsorption rate to diesel oil is 9.86g/g, right
The adsorption rate of soybean oil is 10.21g/g, and infrared spectrum detection is carried out to it, and acquired results are as shown in Figure 4.1745cm-1Place's ester bond
In C=O stretching vibration absworption peaks, 1462cm-1Locate the characteristic absorption peak of bytyry, and 2967~2888cm-1Place occurs three
Individual saturation c h bond absworption peak, shows to be successfully introduced into bytyry in sample, so as to reach oil absorbing effect.
Embodiment 4
It is 2 with the volume ratio of toluene and ethanol:1 mixed solution extracting bagasse, obtains bagasse raw material, takes 1mL second
The bagasse raw material that acyl chlorides, 1mL pyridines and 1g are crushed is placed in ball grinder, sets rotational speed of ball-mill as 1200r/min, with continuous side
Formula carries out 4h ball millings, using ethanol by products therefrom wash repeatedly after prior to drying 6h in 90 DEG C of baking ovens, after be transferred to 95 DEG C of bakings
Continue to dry 24h in case and obtain bagasse acetic acid esters oil absorption material.
Through weighing, bagasse acetic acid esters oil absorption material rate of body weight gain is 32.1%, and the adsorption rate to diesel oil is 8.97g/g, right
The adsorption rate of soybean oil is 9.43g/g, and infrared spectrum detection is carried out to it, and acquired results are as shown in Figure 5.1745cm-1Place's ester bond
In C=O stretching vibration absworption peaks, 1375cm-1The characteristic absorption peak of methyl is substantially strengthened in place's acetyl group, show in sample into
Work(introduces acetyl group, so as to reach oil absorbing effect.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of wood fibre oil absorption material, comprises the following steps：
Wood fibre and esterifying reagent are carried out into esterification under pyridine catalytic action and ball milling condition, wood fibre suction is obtained
Light wood material.
2. preparation method according to claim 1, it is characterised in that the temperature of the ball milling is 20~30 DEG C.
3. preparation method according to claim 1 and 2, it is characterised in that the rotating speed of the ball milling is 800~1200rpm,
The time of the ball milling is 2~4h.
4. preparation method according to claim 1, it is characterised in that the esterifying reagent includes acid anhydrides and/or acyl chlorides.
5. preparation method according to claim 4, it is characterised in that the acid anhydrides includes acetic anhydride, propionic andydride or butyric acid
Acid anhydride；
The acyl chlorides includes chloroacetic chloride, propionyl chloride or butyl chloride.
6. the preparation method according to claim 1,4 or 5, it is characterised in that the matter of the esterifying reagent and wood fibre
Amount is than being 0.25~3.5：1；
The pyridine is 0.25~3 with the mass ratio of wood fibre：1.
7. preparation method according to claim 1, it is characterised in that the wood fibre is by wood fiber biomass raw material
Extracting is obtained, and for toluene and alcohol mixed solvent, the volume ratio of the toluene and ethanol is 2 to the solvent that uses of extracting:1.
8. preparation method according to claim 7, it is characterised in that the wood fiber biomass raw material include Eucalyptus,
The mixture of one or more in poplar, pine, bamboo, bagasse, straw, cornstalk and straw.
9. preparation method according to claim 1, it is characterised in that also include after the esterification：To the esterification
The product of reaction is washed and dried successively.
10. preparation method according to claim 9, it is characterised in that the dry temperature is 50~110 DEG C, described
The dry time is 24~48h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108794799A (en) * | 2018-07-06 | 2018-11-13 | 佛山市陵谐环保科技有限公司 | A kind of preparation method of porous absorption oil absorption material |
| CN109295710A (en) * | 2018-08-07 | 2019-02-01 | 湖南省长沙市爱晚亭家纺用品有限公司 | A kind of method of cotton fiber modification |
| CN109988318A (en) * | 2019-03-27 | 2019-07-09 | 广州市天河区车陂亚贝思烘焙店 | A kind of preparation method of lignin-base fuel thickener |
| CN115300985A (en) * | 2022-06-17 | 2022-11-08 | 华电电力科学研究院有限公司 | Efficient deacidification regeneration treatment method for oil used for power equipment |
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| CN102050952A (en) * | 2010-11-11 | 2011-05-11 | 华南理工大学 | Homogeneous method for preparing wood fiber derivative under room temperature |
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|---|---|---|---|---|
| CN102050952A (en) * | 2010-11-11 | 2011-05-11 | 华南理工大学 | Homogeneous method for preparing wood fiber derivative under room temperature |
| CN102964605A (en) * | 2012-11-30 | 2013-03-13 | 南京林业大学 | Esterification modification method for wood fiber biomasses |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108794799A (en) * | 2018-07-06 | 2018-11-13 | 佛山市陵谐环保科技有限公司 | A kind of preparation method of porous absorption oil absorption material |
| CN109295710A (en) * | 2018-08-07 | 2019-02-01 | 湖南省长沙市爱晚亭家纺用品有限公司 | A kind of method of cotton fiber modification |
| CN109988318A (en) * | 2019-03-27 | 2019-07-09 | 广州市天河区车陂亚贝思烘焙店 | A kind of preparation method of lignin-base fuel thickener |
| CN115300985A (en) * | 2022-06-17 | 2022-11-08 | 华电电力科学研究院有限公司 | Efficient deacidification regeneration treatment method for oil used for power equipment |
| CN115300985B (en) * | 2022-06-17 | 2023-11-24 | 华电电力科学研究院有限公司 | Efficient acid removal regeneration treatment method for oil for power equipment |
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Application publication date: 20170531 |