CN103061174A - Strong acid pretreatment assisted cellulose nano-filament preparation method - Google Patents
Strong acid pretreatment assisted cellulose nano-filament preparation method Download PDFInfo
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Abstract
A strong acid pretreatment assisted cellulose nano-filament preparation method includes: performing hydrolysis pretreatment for bleached paper pulp fibers for 1.0-1.5 hours at the temperature of 40-60 DEG C by the aid of 60-70wt% of concentrated sulfuric acid or hydrochloric acid, swelling up, dissolving and opening partial cellulose amorphous regions, and performing high-speed homogenizing mechanical shearing so that cellulose nano-filaments are obtained rapidly. The cellulose nano-filaments obtained by the method are low in energy consumption during production, high in fiber crystallization degree, large in filament length-diameter ratio and good in heat stability, and can be widely applied to the fields of reinforced composites, dust absorption filtering materials, ecological environment-friendly materials, biomedical materials and the like.
Description
Technical field
The present invention relates to a kind of string nanofibrils material preparation method, be specially the auxiliary method for preparing the cellulose nanofibrils of a kind of strong acid preliminary treatment.
Background technology
In recent years, the plant base nanofiber is quietly promoting the fast development in the fields such as polymer composites, package decoration material, energy-conserving and environment-protective material, processing biopharmaceutical materials, conduction material.The cellulose nanofibrils often utilizes the method for high speed machine shearing or chemical oxidation as the important nano-fiber material of a class, the cellulose microfibril in the string is separated disassemble into diameter in the elongated fibers of nanoscale (being lower than 100nm).This nanofiber has excellent mechanical property, and elastic modelling quantity is up to 100GPa; Also have simultaneously very high draw ratio, and its draw ratio surpasses 100 usually.With regard to nanostructured, this nanofiber is under drying regime, and nanofibrils forms natural Nanostructure Network, can effectively stop the infiltration of small-molecule substance such as water, oxygen, carbon dioxide, in addition, nanofibrils also has good light transmission and heat endurance.
Because chemical oxidation prepares higher, the complex procedures of cost of cellulose nanofibrils, its large-scale commercial applications production still is processed as the master with mechanical shearing.For common bleached pulp fiber cutting is become nanofibrils, in process, need repeatedly mechanical shearing, cause energy consumption larger, production cost is also higher, and these have become the major technique bottleneck of the rapid development of restriction cellulose nanofibrils.Therefore, raw material paper pulp is carried out suitable preliminary treatment, improve the fiber nanometer and disassemble efficient, be of great immediate significance and application prospect, for the development that promotes nanofiber and biomass nano material immeasurable effect is arranged.
Summary of the invention
Technical problem solved by the invention is to provide a kind of strong acid preliminary treatment the auxiliary method for preparing the cellulose nanofibrils, to solve the shortcoming in the above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
The auxiliary method for preparing the cellulose nanofibrils of a kind of strong acid preliminary treatment, the distinguishing feature that is different from other technique is to introduce strong acid hydrolysis preliminary treatment bleached pulp fiber, swollen, dissolve and open cellulose part amorphous region, then utilize the high speed homogenization mechanical shearing to obtain fast the cellulose nanofibrils, may further comprise the steps:
The 1st step: with bleached pulp fiber swollen 24h in deionized water, then high-speed stirred is disperseed 0.5h, is adjusted to the suspension solution of mass fraction of solids 1.5 ~ 2.0%.This mixed liquor is sheared 3 ~ 5 times repeatedly through ultra-fine colloid mill again, swollenization and cut short raw fiber.The fine grinding fiber solution is again high speed centrifugation drying after removing supernatant liquid after the centrifugation.
The 2nd step: the fiber after the drying carries out the concentrated sulfuric acid or concentrated hydrochloric acid hydrolysis, and the concentration of acid is 60 ~ 70wt%, and acidolysis time 1.0 ~ 1.5h, acidolysis temperature are controlled at 40 ~ 60 ℃, and fiber is 2 ~ 8g/ml with matching well of acid solution of hydrolysis.
The 3rd step: acid hydrolysis solution is washed to neutrality repeatedly, adds first in a certain amount of alkali and unreacted acid, again through Buchner funnel with repeatedly deionized water washing of pretreatment of fiber.Fiber centrifugation after the washing is adjusted to solid content 1.5 ~ 2.0%.
The 4th step: the high-strength mechanical shearing processing of pretreatment of fiber high pressure.Acidolysis pretreatment of fiber solution after washing mechanical shearing in the microjet high pressure homogenizer is processed, and wherein circulation shear 10 times in 200 μ m reaction chambers is sheared 5 times in 87 μ m reaction chambers again, and is namely plastic.
Among the present invention, the running speed of ultra-fine colloid mill is 2000 ~ 3000 rpm in described the 1st step process, and the mill spacing is-0.2 ~ 0.4mm.
Among the present invention, the fine grinding fiber moisture 10 ~ 18% in described the 1st step process behind the process centrifuge dripping.
Among the present invention, acid hydrolytic reaction is finished shaking speed 150 ~ 250rpm in described the 2nd step process in constant-temperature table.
Among the present invention, the fine grinding fiber after fiber refers to respectively dry with acid in described the 2nd step process and hydrochloric acid or the sulfuric acid of 60 ~ 70wt%, its ratio is 2 ~ 8g/ml.
Among the present invention, alkali is sodium hydroxide solution in described the 3rd step process, and alkali concn is 15 ~ 20%.
Among the present invention, the rotating speed of centrifugation is 3000 ~ 35000 rpm in described the 3rd step process, removes upper strata centrifugate.
Among the present invention, during microjet high pressure homogenizer shear treatment, pressure is 35 ~ 40MPa in 200 μ m reaction chambers in described the 4th step process, and pressure is 140 ~ 150MPa in 87 μ m reaction chambers.
Beneficial effect: of the present invention is the auxiliary method for preparing the cellulose nanofibrils of a kind of strong acid preliminary treatment.By strong acid hydrolysis preliminary treatment bleached pulp fiber, swollen, dissolve and open cellulose part amorphous region, then utilize the high speed homogenization mechanical shearing to obtain fast the cellulose nanofibrils.The method not only can reduce the energy consumption of cellulose nanofibrils preparation process, and simultaneously strong acid hydrolysis can improve cellulosic degree of crystallinity, has improved to a certain extent the mechanical strength of nanofiber.Therefore, the cellulose nanofibrils that obtains by the method can be widely used in reinforced polymeric material, dust-absorbing filtering material, Ecosystem environmental protection material, and the field such as bio-medical material.
The specific embodiment
The below gives an actual example and describes the present invention.
For technological means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1:
The 1st step: with bleached pulp fiber swollen 24h in deionized water, then high-speed stirred is disperseed 0.5h, is adjusted to the suspension solution of mass fraction of solids 1.5%.This mixed liquor is sheared 3 times repeatedly through ultra-fine colloid mill again, swollenization and cut short raw fiber; Speed of grinding plate 2500 rpm, the mill spacing is ~ 0.1mm.The pre-grinding fiber solution after removing supernatant liquid after the centrifugation again high speed centrifugation dry to moisture content 12%.
The 2nd step: the fiber after the drying carries out concentrated sulfuric acid hydrolysis, and the concentration of acid is 64wt%, and acidolysis time 1.5h, acidolysis temperature are controlled at 50 ℃, and fiber is 4g/ml with matching well of acid solution of hydrolysis.Acidolysis reaction is finished shaking speed 180rpm in constant temperature (50 ℃ of set temperatures) shaking table.
The 3rd step: acid hydrolysis solution is washed to neutrality repeatedly, adds first in a certain amount of 15% sodium hydroxide solution and unreacted acid, again through Buchner funnel with repeatedly deionized water washing of pretreatment of fiber.Fiber centrifugation after the washing is adjusted to solid content 1.5%.
The 4th step: the high-strength mechanical shearing processing of pretreatment of fiber high pressure.Acidolysis pretreatment of fiber solution after washing mechanical shearing in the microjet high pressure homogenizer is processed, and wherein circulation shear 10 times in 200 μ m reaction chambers is sheared 5 times in 87 μ m reaction chambers again, and is namely plastic.
Embodiment 2:
The 1st step: with bleached pulp fiber swollen 24h in deionized water, then high-speed stirred is disperseed 0.5h, is adjusted to the suspension solution of mass fraction of solids 2.0%.This mixed liquor is sheared 4 times repeatedly through ultra-fine colloid mill again, swollenization and cut short raw fiber; Speed of grinding plate 3000 rpm, the mill spacing is ~ 0.1mm.The pre-grinding fiber solution after removing supernatant liquid after the centrifugation again high speed centrifugation dry to moisture content 16%.
The 2nd step: the fiber after the drying carries out concentrated sulfuric acid hydrolysis, and the concentration of acid is 70wt%, and acidolysis time 1.0h, acidolysis temperature are controlled at 55 ℃, and fiber is 6g/ml with matching well of acid solution of hydrolysis.Acidolysis reaction is finished shaking speed 180rpm in constant temperature (55 ℃ of set temperatures) shaking table.
The 3rd step: acid hydrolysis solution is washed to neutrality repeatedly, adds first in a certain amount of 16% sodium hydroxide solution and unreacted acid, again through Buchner funnel with repeatedly deionized water washing of pretreatment of fiber.Fiber centrifugation after the washing is adjusted to solid content 2.0%.
The 4th step: the high-strength mechanical shearing processing of pretreatment of fiber high pressure.Acidolysis pretreatment of fiber solution after washing mechanical shearing in the microjet high pressure homogenizer is processed, and wherein circulation shear 10 times in 200 μ m reaction chambers is sheared 5 times in 87 μ m reaction chambers again, and is namely plastic.
Embodiment 3:
The 1st step: with bleached pulp fiber swollen 24h in deionized water, then high-speed stirred is disperseed 0.5h, is adjusted to the suspension solution of mass fraction of solids 2%.This mixed liquor is sheared 5 times repeatedly through ultra-fine colloid mill again, swollenization and cut short raw fiber; Speed of grinding plate 3000 rpm, the mill spacing is ~ 0.1mm.The pre-grinding fiber solution after removing supernatant liquid after the centrifugation again high speed centrifugation dry to moisture content 18%.
The 2nd step: the fiber after the drying carries out concentrated hydrochloric acid hydrolysis, and the concentration of acid is 70wt%, and acidolysis time 1.5h, acidolysis temperature are controlled at 50 ℃, and fiber is 8g/ml with matching well of acid solution of hydrolysis.Acidolysis reaction is finished shaking speed 200rpm in constant temperature (50 ℃ of set temperatures) shaking table.
The 3rd step: acid hydrolysis solution is washed to neutrality repeatedly, adds first in a certain amount of 20% sodium hydroxide solution and unreacted acid, again through Buchner funnel with repeatedly deionized water washing of pretreatment of fiber.Fiber centrifugation after the washing is adjusted to solid content %.
The 4th step: the high-strength mechanical shearing processing of pretreatment of fiber high pressure.Acidolysis pretreatment of fiber solution after washing mechanical shearing in the microjet high pressure homogenizer is processed, and wherein circulation shear 10 times in 200 μ m reaction chambers is sheared 5 times in 87 μ m reaction chambers again, and is namely plastic.
More than show and described basic principle of the present invention and principal character and advantage of the present invention; the technical staff of the industry should understand; the present invention is not restricted to the described embodiments; that describes in above-described embodiment and the specification just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications; these changes and improvements all fall in the claimed scope of the invention, and the claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (8)
1. the method for preparing the cellulose nanofibrils is assisted in a strong acid preliminary treatment, and its characteristics are, may further comprise the steps:
The 1st step: with bleached pulp fiber swollen 24h in deionized water, then high-speed stirred is disperseed 0.5h, be adjusted to the suspension solution of mass fraction of solids 1.5 ~ 2.0%, this mixed liquor is sheared 3 ~ 5 times repeatedly through ultra-fine colloid mill again, swollenization and cut short raw fiber, pre-grinding fiber solution after removing supernatant liquid after the centrifugation again high speed centrifugation dry;
The 2nd step: the fiber after the drying carries out the concentrated sulfuric acid or concentrated hydrochloric acid hydrolysis, and the concentration of acid is 60 ~ 70wt%, and acidolysis time 1.0 ~ 1.5h, acidolysis temperature are controlled at 40 ~ 60 ℃, and fiber is 2 ~ 8g/ml with matching well of acid solution of hydrolysis;
The 3rd step: acid hydrolysis solution is washed to neutrality repeatedly, adds first in a certain amount of alkali and unreacted acid, again through Buchner funnel with repeatedly deionized water washing of pretreatment of fiber, the fiber centrifugation after the washing is adjusted to solid content 1.5 ~ 2.0%;
The 4th step: the high-strength mechanical shearing processing of pretreatment of fiber high pressure, acidolysis pretreatment of fiber solution after washing mechanical shearing in the microjet high pressure homogenizer is processed, circulation shear 10 times in 200 μ m reaction chambers wherein, in 87 μ m reaction chambers, shear again 5 times namely plastic.
2. the auxiliary method for preparing the cellulose nanofibrils of a kind of strong acid preliminary treatment according to claim 1 is characterized in that, the running speed of ultra-fine colloid mill is 2000 ~ 3000 rpm in described the 1st step, and the mill spacing is-0.2 ~ 0.4mm.
3. the auxiliary method for preparing the cellulose nanofibrils of a kind of strong acid preliminary treatment according to claim 1 is characterized in that, the fine grinding fiber moisture 10 ~ 18% in described the 2nd step behind the process centrifuge dripping.
4. the auxiliary method for preparing the cellulose nanofibrils of a kind of strong acid preliminary treatment according to claim 1 is characterized in that, acid hydrolytic reaction is finished shaking speed 150 ~ 250rpm in described the 2nd step in constant-temperature table.
5. the auxiliary method for preparing the cellulose nanofibrils of a kind of strong acid preliminary treatment according to claim 1 is characterized in that, the fine grinding fiber after fiber refers to respectively dry with acid in described the 2nd step and hydrochloric acid or the sulfuric acid of 60 ~ 70wt%, and its ratio is 2 ~ 8g/ml.
6. the auxiliary method for preparing the cellulose nanofibrils of a kind of strong acid preliminary treatment according to claim 1 is characterized in that, alkali is sodium hydroxide solution in described the 3rd step, and alkali concn is 10 ~ 20%.
7. the auxiliary method for preparing the cellulose nanofibrils of a kind of strong acid preliminary treatment according to claim 1 is characterized in that, the rotating speed of centrifugation is 3000 ~ 35000 rpm in described the 3rd step, removes upper strata centrifugate.
8. the method for preparing the cellulose nanofibrils is assisted in a kind of strong acid preliminary treatment according to claim 1, it is characterized in that, during microjet high pressure homogenizer shear treatment, pressure is 35 ~ 40MPa in 200 μ m reaction chambers in described the 4th step, and pressure is 140 ~ 150MPa in 87 μ m reaction chambers.
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| CN103952939A (en) * | 2014-05-12 | 2014-07-30 | 南京林业大学 | Wood fiber microfilament dissociation method based on soft nanometer paper base material |
| CN104955848A (en) * | 2012-11-30 | 2015-09-30 | 阿普艾知识产权控股有限责任公司 | Processes and apparatus for producing nanocellulose, and compositions and products produced therefrom |
| CN105492669A (en) * | 2013-09-11 | 2016-04-13 | 日东纺绩株式会社 | Cellulose nanofibers, method for producing same, aqueous dispersion using cellulose nanofibers, and fiber-reinforced composite material |
| CN106592311A (en) * | 2016-12-13 | 2017-04-26 | 华南理工大学 | Preparation method of nanofibril cellulose |
| CN106638091A (en) * | 2016-12-13 | 2017-05-10 | 华南理工大学 | Method for preprocessing high crystallinity plant fiber in preparation of micro-nano fibril |
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