CN102182087A - Method for preparing nano cellulose by alkali/toluene method - Google Patents
Method for preparing nano cellulose by alkali/toluene method Download PDFInfo
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Abstract
The invention discloses a method for preparing nano cellulose by an alkali/toluene method, and relates to a preparation method of nano cellulose. The method disclosed by the invention solves the problems of low reaction speed and environmental pollution of acid waste liquid in the existing preparation process of nano cellulose. The preparation method comprises the following steps: dissolving a fiber raw material in a mixed solution of sodium hydroxide, urea and water, stirring and centrifuging to obtain a clear sticky solution; mixing tween-80 with toluene, stirring under the action of magnetic force, and adding the clear sticky solution obtained in the previous step; stirring, and dropwisely adding a hydrochloric acid solution until the pH value is 6-7; adding distilled water and centrifuging; and carrying out rotary evaporation, and concentrating to obtain the nano cellulose. The method disclosed by the invention enables easy implementation of equipment, has simple steps, does not need sulfuric acid or high-pressure filtration through a dialysis membrane, is simple to operate and easy for industrialization, and brings little pollution to environment.
Description
Technical field
The present invention relates to a kind of preparation method of nano-cellulose.
Background technology
China is a Shaolin country, can reach 20% to afforestation rate in 2010.Can be still less for the overmature forest of felling, the natural woodland productivity descends simultaneously, and the timber imbalance between supply and demand is becoming increasingly acute.In addition, people are to the excessive use of non-renewable resources such as natural gas, oil, mineral products, and energy scarcity becomes the significant problem that needs to be resolved hurrily that human society faces, and the development and use of new resources become a top priority of countries in the world.But cellulose be nature mainly by the natural polymer of plant by the synthetic continuous utilization of photosynthesis, be the abundantest in the world natural polymer, extensively be present in the tunica of natural plants and pygochord class animal.It is a kind of renewable resource inexhaustible, nexhaustible on the earth.Because the needs of sustainable development and environmental protection; in the past few decades; be subjected to domestic and international researcher and manufacturing enterprise more and more payes attention to based on the biodegradation material of natural reproducible resource, nano-cellulose also has been applied in the middle of the research of polymer composite.The advantage that nano-cellulose is compared with other nano-filled things be inexpensive, be easy to get, renewable, bio-compatible, preparation are simple, can chemistry or physical modification or the like, its crystal structure high-sequential, obviously electricity, optics, magnetics, insulating properties even the superconductivity of change material.Domestic disclosed nano-cellulose preparation method reaction speed in preparation nano-cellulose process is slow at present, and the acid waste liquid environmental pollution when the acid hydrolyzation hydrolysis prepares nano-cellulose is bigger.
Because dimensional effect, nano level fiber is compared with general fibre, and special physics and chemical characteristic are arranged, and huge specific area and surface atom number make it have special skin effect.In addition, the surface-activity of nanofiber is very big, thus also enhancing greatly of respond, so nano-cellulose is a kind of new material that has application prospect.
Summary of the invention
The objective of the invention is in order to solve in the existing preparation nano-cellulose process reaction speed slowly, the problem of acid waste liquid environmental pollution provides a kind of alkali/toluene method to prepare the method for nano-cellulose.
The method that alkali/toluene method prepares nano-cellulose is as follows: one, under subzero 8 ℃～subzero 15 ℃ condition, fibrous raw material is dissolved in the mixed solution of NaOH, urea and water, stir 3min～5min, use centrifuge with the centrifugal 8min of the centrifugal speed of 9000r/min then, obtain clarifying viscous solution, wherein the volume ratio of the mixed solution of the quality of fibrous raw material and NaOH, urea and water is 1g: 25mL, and the mass ratio of NaOH, urea and water is 7: 12: 81 in the mixed solution of NaOH, urea and water; Two, Tween-80 is mixed according to 1: 18～20 volume ratio with toluene, and at room temperature behind the magnetic agitation 30min～35min with 1000r/min, the clarification viscous solution that adds the step 1 gained, the volume ratio of clarification viscous solution and toluene is 2: 15, at room temperature stir 3h, obtain the oyster white turbid solution; Three, be that the hydrochloric acid solution of 1mol/L is added drop-wise in the oyster white turbid solution with concentration, and to be stirred to the pH value while dripping be 6～7, obtain white turbid liquid; Four, white turbid liquid is mixed according to 1: 10 volume ratio with distilled water, centrifugal 10min under the 10000r/min condition obtains nano-cellulose after rotary evaporation concentrates again; Fibrous raw material described in the step 1 is reed pulp, absorbent cotton or microcrystalline cellulose.
The present invention directly utilizes paper mill paper pulp (reed pulp), commodity microcrystalline cellulose and absorbent cotton as fibrous raw material, by alkali, urea preliminary treatment dissolving, add toluene and surfactant Tween-80, again in conjunction with rational last handling process such as centrifugal grade, solved prior art problem of slow response in preparation nano-cellulose process, finally made graininess nano-cellulose with torispherical.
The present invention utilizes organic facies toluene and surfactant to impel rapidly-soluble fibrous raw material further to be dispersed in organic facies and aqueous phase, a large amount of toluene molecules combine with the cellulose amides skeleton and are dispersed in the solution system, simultaneously also make part toluene molecule enter in the fibre bundle space hydrogen bond between the considerable damage cellulosic molecule; Along with the increase of time, the hydrogen bond between crystal region in the cellulose and crystal region, fibre bundle and the fibre bundle continues destroyed, under stirring action, isolates increasing single fibre bundle gradually, is dispersed in the mixed solution; After adding hydrochloric acid, amide group is reduced into hydroxyl, obtains nano-cellulose.
The inventive method has that equipment operation is easy to implement, and step is succinct, need not to use sulfuric acid, dialysis membrane high-pressure filteration, and simple to operate, environmental pollution is little, is easy to industrialization.The torispherical nano-cellulose particle diameter that the present invention makes is less than 500nm, but advantage with the big natural degradation of specific area, good dispersion, good biocompatibility, can be improved significantly at aspects such as heat endurances by its preparation nano composite material, also can be used as a kind of packing material of excellent performance.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the nano-cellulose of the specific embodiment eight preparations; Fig. 2 is the transmission electron microscope photo of the nano-cellulose of the specific embodiment nine preparations; Fig. 3 is the transmission electron microscope photo of the nano-cellulose of the specific embodiment ten preparations.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: to prepare the method for nano-cellulose as follows for alkali/toluene method in the present embodiment: one, under subzero 8 ℃～subzero 15 ℃ condition, fibrous raw material is dissolved in NaOH, in the mixed solution of urea and water, stir 3min～5min, use centrifuge with the centrifugal 8min of the centrifugal speed of 9000r/min then, obtain clarifying viscous solution, the wherein quality of fibrous raw material and NaOH, the volume ratio of the mixed solution of urea and water is 1g: 25mL, NaOH, NaOH in the mixed solution of urea and water, the mass ratio of urea and water is 7: 12: 81; Two, Tween-80 is mixed according to 1: 18～20 volume ratio with toluene, and at room temperature behind the magnetic agitation 30min～35min with 1000r/min, the clarification viscous solution that adds the step 1 gained, the volume ratio of clarification viscous solution and toluene is 2: 15, at room temperature stir 3h, obtain the oyster white turbid solution; Three, be that the hydrochloric acid solution of 1mol/L is added drop-wise in the oyster white turbid solution with concentration, and to be stirred to the pH value while dripping be 6～7, obtain white turbid liquid; Four, white turbid liquid is mixed according to 1: 10 volume ratio with distilled water, centrifugal 10min under the 10000r/min condition obtains nano-cellulose after rotary evaporation concentrates again.
The nano-cellulose of the present embodiment preparation ball shaped nano cellulose that is as the criterion, particle diameter is less than 500nm.
The specific embodiment two: what present embodiment and the specific embodiment one were different is that the fibrous raw material described in the step 1 is reed pulp, absorbent cotton or microcrystalline cellulose.Other step is identical with the specific embodiment one with parameter.
Reed pulp described in the present embodiment derives from the paper mill, and described absorbent cotton and microcrystalline cellulose are commercially available absorbent cotton and microcrystalline cellulose.
The specific embodiment three: present embodiment is different with the specific embodiment one or two be in the step 1 under subzero 12 ℃ condition, fibrous raw material is dissolved in the mixed solution of NaOH, urea and water.Other step is identical with the specific embodiment one or two with parameter.
The specific embodiment four: what present embodiment was different with one of specific embodiment one to three is in the step 2 Tween-80 to be mixed according to 1: 19 volume ratio with toluene.Other step is identical with one of specific embodiment one to three with parameter.
The specific embodiment five: to prepare the method for nano-cellulose as follows for alkali/toluene method in the present embodiment: one, under subzero 10 ℃ condition, fibrous raw material is dissolved in the mixed solution of NaOH, urea and water, stir 3minn, use centrifuge with the centrifugal 8min of the centrifugal speed of 9000r/min then, obtain clarifying viscous solution, wherein the volume ratio of the mixed solution of the quality of fibrous raw material and NaOH, urea and water is 1g: 25mL, and the mass ratio of NaOH, urea and water is 7: 12: 81 in the mixed solution of NaOH, urea and water; Two, Tween-80 is mixed according to 1: 18 volume ratio with toluene, and at room temperature behind the magnetic agitation 30min with 1000r/min, add the clarification viscous solution of step 1 gained, the volume ratio of clarification viscous solution and toluene is 2: 15, at room temperature stir 3h, obtain the oyster white turbid solution; Three, be that the hydrochloric acid solution of 1mol/L is added drop-wise in the oyster white turbid solution with concentration, and to be stirred to the pH value while dripping be 6, obtain white turbid liquid; Four, white turbid liquid is mixed according to 1: 10 volume ratio with distilled water, centrifugal 10min under the 10000r/min condition obtains nano-cellulose after rotary evaporation concentrates again.
The nano-cellulose of the present embodiment preparation ball shaped nano cellulose that is as the criterion, particle diameter is less than 500nm.
The specific embodiment six: to prepare the method for nano-cellulose as follows for alkali/toluene method in the present embodiment: one, under subzero 15 ℃ condition, fibrous raw material is dissolved in the mixed solution of NaOH, urea and water, stir 5min, use centrifuge with the centrifugal 8min of the centrifugal speed of 9000r/min then, obtain clarifying viscous solution, wherein the volume ratio of the mixed solution of the quality of fibrous raw material and NaOH, urea and water is 1g: 25mL, and the mass ratio of NaOH, urea and water is 7: 12: 81 in the mixed solution of NaOH, urea and water; Two, Tween-80 is mixed according to 1: 20 volume ratio with toluene, and at room temperature behind the magnetic agitation 35min with 1000r/min, add the clarification viscous solution of step 1 gained, the volume ratio of clarification viscous solution and toluene is 2: 15, at room temperature stir 3h, obtain the oyster white turbid solution; Three, be that the hydrochloric acid solution of 1mol/L is added drop-wise in the oyster white turbid solution with concentration, and to be stirred to the pH value while dripping be 7, obtain white turbid liquid; Four, white turbid liquid is mixed according to 1: 10 volume ratio with distilled water, centrifugal 10min under the 10000r/min condition obtains nano-cellulose after rotary evaporation concentrates again.
The nano-cellulose of the present embodiment preparation ball shaped nano cellulose that is as the criterion, particle diameter is less than 500nm.
The specific embodiment seven: to prepare the method for nano-cellulose as follows for alkali/toluene method in the present embodiment: one, under subzero 12 ℃ condition, fibrous raw material is dissolved in the mixed solution of NaOH, urea and water, stir 4min, use centrifuge with the centrifugal 8min of the centrifugal speed of 9000r/min then, obtain clarifying viscous solution, wherein the volume ratio of the mixed solution of the quality of fibrous raw material and NaOH, urea and water is 1g: 25mL, and the mass ratio of NaOH, urea and water is 7: 12: 81 in the mixed solution of NaOH, urea and water; Two, Tween-80 is mixed according to 1: 19 volume ratio with toluene, and at room temperature behind the magnetic agitation 33min with 1000r/min, add the clarification viscous solution of step 1 gained, the volume ratio of clarification viscous solution and toluene is 2: 15, at room temperature stir 3h, obtain the oyster white turbid solution; Three, be that the hydrochloric acid solution of 1mol/L is added drop-wise in the oyster white turbid solution with concentration, and to be stirred to the pH value while dripping be 6.5, obtain white turbid liquid; Four, white turbid liquid is mixed according to 1: 10 volume ratio with distilled water, centrifugal 10min under the 10000r/min condition obtains nano-cellulose after rotary evaporation concentrates again.
The nano-cellulose of the present embodiment preparation ball shaped nano cellulose that is as the criterion, particle diameter is less than 500nm.
The specific embodiment eight: to prepare the method for nano-cellulose as follows for alkali/toluene method in the present embodiment: one, under subzero 15 ℃ condition, the 8g reed pulp is dissolved in the mixed solution of 200mL NaOH, urea and water, stir 4min, use centrifuge with the centrifugal 8min of the centrifugal speed of 9000r/min then, obtain clarifying viscous solution, wherein the mass ratio of NaOH, urea and water is 7: 12: 81 in the mixed solution of NaOH, urea and water; Two, the 8mL Tween-80 is mixed with 150mL toluene, and at room temperature behind the magnetic agitation 30min with 1000r/min, add the clarification viscous solution of 20mL step 1 gained, at room temperature stir 3h, obtain the oyster white turbid solution; Three, be that the hydrochloric acid solution of 1mol/L is added drop-wise in the oyster white turbid solution with concentration, and to be stirred to the pH value while dripping be 6, obtain white turbid liquid; Four, white turbid liquid is mixed according to 1: 10 volume ratio with distilled water, centrifugal 10min under the 10000r/min condition obtains nano-cellulose after rotary evaporation concentrates again.
The nano-cellulose of the present embodiment preparation ball shaped nano cellulose that is as the criterion, particle diameter is less than 500nm.
The specific embodiment nine: to prepare the method for nano-cellulose as follows for alkali/toluene method in the present embodiment: one, under subzero 15 ℃ condition, 8g absorbent cotton is dissolved in the mixed solution of 200mL NaOH, urea and water, stir 4min, use centrifuge with the centrifugal 8min of the centrifugal speed of 9000r/min then, obtain clarifying viscous solution, wherein the mass ratio of NaOH, urea and water is 7: 12: 81 in the mixed solution of NaOH, urea and water; Two, the 8mL Tween-80 is mixed with 150mL toluene, and at room temperature behind the magnetic agitation 30min with 1000r/min, add the clarification viscous solution of 20mL step 1 gained, at room temperature stir 3h, obtain the oyster white turbid solution; Three, be that the hydrochloric acid solution of 1mol/L is added drop-wise in the oyster white turbid solution with concentration, and to be stirred to the pH value while dripping be 6, obtain white turbid liquid; Four, white turbid liquid is mixed according to 1: 10 volume ratio with distilled water, centrifugal 10min under the 10000r/min condition obtains nano-cellulose after rotary evaporation concentrates again.
The nano-cellulose of the present embodiment preparation ball shaped nano cellulose that is as the criterion, particle diameter is less than 500nm.
The specific embodiment ten: to prepare the method for nano-cellulose as follows for alkali/toluene method in the present embodiment: one, under subzero 15 ℃ condition, the 8g microcrystalline cellulose is dissolved in the mixed solution of 200mL NaOH, urea and water, stir 4min, use centrifuge with the centrifugal 8min of the centrifugal speed of 9000r/min then, obtain clarifying viscous solution, wherein the mass ratio of NaOH, urea and water is 7: 12: 81 in the mixed solution of NaOH, urea and water; Two, the 8mL Tween-80 is mixed with 150mL toluene, and at room temperature behind the magnetic agitation 30min with 1000r/min, add the clarification viscous solution of 20mL step 1 gained, at room temperature stir 3h, obtain the oyster white turbid solution; Three, be that the hydrochloric acid solution of 1mol/L is added drop-wise in the oyster white turbid solution with concentration, and to be stirred to the pH value while dripping be 6, obtain white turbid liquid; Four, white turbid liquid is mixed according to 1: 10 volume ratio with distilled water, centrifugal 10min under the 10000r/min condition obtains nano-cellulose after rotary evaporation concentrates again.
The nano-cellulose of the present embodiment preparation ball shaped nano cellulose that is as the criterion, particle diameter is less than 500nm.
The specific embodiment 11: to prepare the method for nano-cellulose as follows for alkali/toluene method in the present embodiment: one, under subzero 12 ℃ condition, the 12g reed pulp is dissolved in 300mL NaOH, in the mixed solution of urea and water, stir 3min, use centrifuge with the centrifugal 8min of the centrifugal speed of 9000r/min then, obtain clarifying viscous solution, the wherein quality of fibrous raw material and NaOH, the volume ratio of the mixed solution of urea and water is 1g: 25mL, NaOH, NaOH in the mixed solution of urea and water, the mass ratio of urea and water is 7: 12: 81; Two, the 15mL Tween-80 is mixed with 300mL toluene, and at room temperature behind the magnetic agitation 35min with 1000r/min, add the clarification viscous solution of 40mL step 1 gained, at room temperature stir 3h, obtain the oyster white turbid solution; Three, be that the hydrochloric acid solution of 1mol/L is added drop-wise in the oyster white turbid solution with concentration, and to be stirred to the pH value while dripping be 6～7, obtain white turbid liquid; Four, white turbid liquid is mixed according to 1: 10 volume ratio with distilled water, centrifugal 10min under the 10000r/min condition obtains nano-cellulose after rotary evaporation concentrates again.
The nano-cellulose of the present embodiment preparation ball shaped nano cellulose that is as the criterion, particle diameter is less than 500nm.
The specific embodiment 12: to prepare the method for nano-cellulose as follows for alkali/toluene method in the present embodiment: one, under subzero 12 ℃ condition, 12g absorbent cotton is dissolved in 300mL NaOH, in the mixed solution of urea and water, stir 3min, use centrifuge with the centrifugal 8min of the centrifugal speed of 9000r/min then, obtain clarifying viscous solution, the wherein quality of fibrous raw material and NaOH, the volume ratio of the mixed solution of urea and water is 1g: 25mL, NaOH, NaOH in the mixed solution of urea and water, the mass ratio of urea and water is 7: 12: 81; Two, the 15mL Tween-80 is mixed with 300mL toluene, and at room temperature behind the magnetic agitation 35min with 1000r/min, add the clarification viscous solution of 40mL step 1 gained, at room temperature stir 3h, obtain the oyster white turbid solution; Three, be that the hydrochloric acid solution of 1mol/L is added drop-wise in the oyster white turbid solution with concentration, and to be stirred to the pH value while dripping be 6～7, obtain white turbid liquid; Four, white turbid liquid is mixed according to 1: 10 volume ratio with distilled water, centrifugal 10min under the 10000r/min condition obtains nano-cellulose after rotary evaporation concentrates again.
The nano-cellulose of the present embodiment preparation ball shaped nano cellulose that is as the criterion, particle diameter is less than 500nm.
The specific embodiment 13: to prepare the method for nano-cellulose as follows for alkali/toluene method in the present embodiment: one, under subzero 12 ℃ condition, the 12g microcrystalline cellulose is dissolved in 300mL NaOH, in the mixed solution of urea and water, stir 3min, use centrifuge with the centrifugal 8min of the centrifugal speed of 9000r/min then, obtain clarifying viscous solution, the wherein quality of fibrous raw material and NaOH, the volume ratio of the mixed solution of urea and water is 1g: 25mL, NaOH, NaOH in the mixed solution of urea and water, the mass ratio of urea and water is 7: 12: 81; Two, the 15mL Tween-80 is mixed with 300mL toluene, and at room temperature behind the magnetic agitation 35min with 1000r/min, add the clarification viscous solution of 40mL step 1 gained, at room temperature stir 3h, obtain the oyster white turbid solution; Three, be that the hydrochloric acid solution of 1mol/L is added drop-wise in the oyster white turbid solution with concentration, and to be stirred to the pH value while dripping be 6～7, obtain white turbid liquid; Four, white turbid liquid is mixed according to 1: 10 volume ratio with distilled water, centrifugal 10min under the 10000r/min condition obtains nano-cellulose after rotary evaporation concentrates again.
The nano-cellulose of the present embodiment preparation ball shaped nano cellulose that is as the criterion, particle diameter is less than 500nm.
Claims (4)
1. alkali/toluene method prepares the method for nano-cellulose, it is as follows to it is characterized in that alkali/toluene method prepares the method for nano-cellulose: one, under subzero 8 ℃～subzero 15 ℃ condition, fibrous raw material is dissolved in NaOH, in the mixed solution of urea and water, stir 3min～5min, use centrifuge with the centrifugal 8min of the centrifugal speed of 9000r/min then, obtain clarifying viscous solution, the wherein quality of fibrous raw material and NaOH, the volume ratio of the mixed solution of urea and water is 1g: 25mL, NaOH, NaOH in the mixed solution of urea and water, the mass ratio of urea and water is 7: 12: 81; Two, Tween-80 is mixed according to 1: 18～20 volume ratio with toluene, and at room temperature behind the magnetic agitation 30min～35min with 1000r/min, the clarification viscous solution that adds the step 1 gained, the volume ratio of clarification viscous solution and toluene is 2: 15, at room temperature stir 3h, obtain the oyster white turbid solution; Three, be that the hydrochloric acid solution of 1mol/L is added drop-wise in the oyster white turbid solution with concentration, and to be stirred to the pH value while dripping be 6～7, obtain white turbid liquid; Four, white turbid liquid is mixed according to 1: 10 volume ratio with distilled water, centrifugal 10min under the 10000r/min condition obtains nano-cellulose after rotary evaporation concentrates again.
2. the method for preparing nano-cellulose according to the described alkali/toluene method of claim 1 is characterized in that the fibrous raw material described in the step 1 is reed pulp, absorbent cotton or microcrystalline cellulose.
3. the method for preparing nano-cellulose according to claim 1 or 2 described alkali/toluene methods is characterized in that in the step 1 fibrous raw material being dissolved in the mixed solution of NaOH, urea and water under subzero 12 ℃ condition.
4. the method for preparing nano-cellulose according to the described alkali/toluene method of claim 3 is characterized in that in the step 2 Tween-80 being mixed according to 1: 19 volume ratio with toluene.
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| CN103304824A (en) * | 2013-06-15 | 2013-09-18 | 浙江理工大学 | Preparation method of high-concentration nano microcrystalline cellulose gel |
| CN103821021A (en) * | 2014-02-27 | 2014-05-28 | 中国科学院金属研究所 | Nano cellulose extracted from shuck of xanthoceras sorbifolia and extraction method |
| CN104105827A (en) * | 2012-02-10 | 2014-10-15 | 芬欧汇川集团 | Method for pretreating cellulose pulp |
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| CN104105827B (en) * | 2012-02-10 | 2016-10-26 | 芬欧汇川集团 | The method of pretreatment of fiber element slurry |
| CN103304824A (en) * | 2013-06-15 | 2013-09-18 | 浙江理工大学 | Preparation method of high-concentration nano microcrystalline cellulose gel |
| CN103821021A (en) * | 2014-02-27 | 2014-05-28 | 中国科学院金属研究所 | Nano cellulose extracted from shuck of xanthoceras sorbifolia and extraction method |
| CN103821021B (en) * | 2014-02-27 | 2016-01-20 | 中国科学院金属研究所 | A kind of nano-cellulose from shinyleaf yellowhorn fruit shell extraction and extracting method thereof |
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