CN114685812A - Method for efficiently concentrating and redispersing micro/nano cellulose - Google Patents
Method for efficiently concentrating and redispersing micro/nano cellulose Download PDFInfo
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- CN114685812A CN114685812A CN202210252463.1A CN202210252463A CN114685812A CN 114685812 A CN114685812 A CN 114685812A CN 202210252463 A CN202210252463 A CN 202210252463A CN 114685812 A CN114685812 A CN 114685812A
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Abstract
The invention discloses a method for efficiently concentrating and redispersing micro/nano cellulose, belonging to the field of redispersion of micro/nano cellulose. The method comprises the following steps: adding polyvinylpyrrolidone into the micro/nano cellulose suspension, and uniformly stirring to obtain a mixed suspension; and concentrating and dehydrating the suspension, supplementing polyvinylpyrrolidone into the concentrated micro/nano cellulose to the initial adding amount, then adding water for dilution, and then grinding and redispersing ultrafine particles to obtain stable micro/nano cellulose suspension and keep the nano size of the suspension. The invention can effectively improve the stability of the redispersed micro/nano cellulose suspension, maintain the original structural characteristics of the suspension and provide technical support for the storage, transportation and application of high-concentration micro/nano cellulose.
Description
Technical Field
The invention belongs to the field of micro/nano cellulose redispersion, and particularly relates to a method for efficiently concentrating and redispersing micro/nano cellulose.
Background
The micro/nano cellulose is a natural high molecular polymer separated and prepared from plant fiber raw materials, has the diameter of less than 100nm, has the advantages of good mechanical property and optical property, high specific surface area, high length-diameter ratio, reproducibility, biodegradability and the like, and shows great application prospect in the fields of papermaking, foods, cosmetics, electronic equipment and the like. Cellulose pulp, transported in the form of pulp sheets, generally has a solids content higher than 90% by weight and is easily re-dispersible in water, while micro/nanocellulose is transported in the form of a suspension, generally having a solids content lower than 3% by weight, increasing the storage and transportation costs of the micro/nanocellulose, limiting its application. The method explores a proper micro/nano cellulose concentration and redispersion process, improves the concentration and dehydration efficiency, reduces the change of structure and performance in the concentration process, reduces irreversible flocculation, and has important significance for industrial production and commercial application of the micro/nano cellulose.
At present, the concentration of the micro/nano cellulose is mainly improved by adopting a drying method, such as freeze drying, oven drying, spray drying, supercritical drying and other methods, strong hydrogen bonding is generated between the micro/nano cellulose in an absolute dry state, so that the micro/nano cellulose is difficult to redisperse to an original state. Therefore, the concentration and dehydration mode is commonly used for improving the concentration of the micro/nano cellulose, the abundant hydroxyl on the surface of the micro/nano cellulose enables the micro/nano cellulose to form stable suspension in a water system, the dehydration efficiency is low, how to improve the dehydration efficiency is achieved, and the original structural characteristics of the redispersed suspension are maintained, so that the method has important significance for industrial production and commercial application.
Disclosure of Invention
The invention aims to provide a method for efficiently concentrating and redispersing micro/nano cellulose. The method is based on the filtration assisting and dispersing effects of polyvinylpyrrolidone, improves the concentration of the micro/nano cellulose, and inhibits irreversible flocculation in the concentration process, thereby improving the stability of the micro/nano cellulose suspension after redispersion.
The purpose of the invention is realized by the following technical scheme.
A method for efficiently concentrating and re-dispersing micro/nano cellulose comprises the following steps:
adding polyvinylpyrrolidone into the micro/nano cellulose suspension, and uniformly stirring to obtain a mixed suspension; and (3) concentrating and dehydrating the mixed suspension, supplementing polyvinylpyrrolidone into the concentrated micro/nano cellulose to the initial addition amount, then adding water for dilution, and then grinding and redispersing the superfine particles.
Preferably, the addition amount of the polyvinylpyrrolidone is 2-8 wt% of the micro/nano cellulose.
Preferably, the concentration dehydration mode is centrifugal dehydration, the centrifugation speed is 1500-5000 r/min, and the centrifugation time is 10-20 min.
Preferably, the disc grinding gap for grinding and redispersing the ultrafine particles is 0 to-50 μm.
Preferably, the disc grinding gap for grinding and redispersing the ultrafine particles is-20 to-50 μm.
Preferably, the rotation speed for grinding and redispersing the ultrafine particles is 600 to 2000 r/min.
Preferably, the concentration of the micron/nanometer cellulose for grinding and redispersing the ultrafine particles is 0.2 to 2.0 wt%.
Preferably, the micro/nano-cellulose suspension has a concentration of 0.5 to 1.0 wt%.
Preferably, the micro/nano cellulose suspension is prepared by the steps of carrying out enzyme pretreatment/mechanical grinding on plant fiber raw materials; the mechanical grinding is to grind the mixture to a stable suspension state by adopting at least one of an ultramicron grinder, a nanometer micro-jet homogenizer and a high-pressure homogenizer; the enzyme pretreatment is endo-cellulase pretreatment.
Preferably, the ultrafine particle grinding is performed by an ultrafine particle grinder, wherein the grinding concentration is 0.5 to 1.0 wt%, and the grinding is performed 15 to 25 times.
Preferably, after the polyvinylpyrrolidone is added into the micro/nano cellulose suspension, a mechanical stirring mode is adopted until the system is uniform, and the stirring speed is 200-1000 r/min.
Compared with the prior art, the invention has the following beneficial effects:
(1) the shape and size of the re-dispersed micro/nano cellulose obtained by the invention are similar to the original micro/nano cellulose size.
(2) The invention fully utilizes the filtration-assisting function of polyvinylpyrrolidone, obtains concentrated micro/nano-cellulose with higher concentration, utilizes the hydrogen bond function between the polyvinylpyrrolidone and the micro/nano-cellulose, reduces the formation of hydrogen bonds between fibers in the concentration process, effectively improves the stability of suspension, and can greatly reduce the storage and transportation cost of low-concentration micro/nano-cellulose.
Drawings
FIG. 1 is an AFM image of the micro/nanocellulose after redispersion of comparative example 1 and example 2; where a is no polyvinylpyrrolidone (comparative example 1) and b is polyvinylpyrrolidone (example 2) addition.
FIG. 2 is a histogram of the frequency distribution of diameters of the micro/nanocellulose after redispersion of comparative example 1 and example 2; where a is no polyvinylpyrrolidone (comparative example 1) and b is polyvinylpyrrolidone (example 2) addition.
Detailed Description
The following examples are intended to further illustrate the embodiments of the present invention, but the embodiments of the present invention are not limited thereto.
The present invention is not particularly limited with respect to the kind and source of the plant cellulose raw material, and bleached softwood pulp is exemplified below.
Example 1
(1) Preparing micro/nano cellulose: fully defibering bleached softwood pulp, then carrying out endo cellulase pretreatment and ultramicron grinder mechanical treatment, wherein the dosage of the endo cellulase is 9mg/g of matrix, the pH value is 5.2 at 50 ℃, and the treatment lasts for 2 hours. The mechanical grinding treatment adopts an ultrafine particle grinder, the concentration is 1.0 wt%, the grinding is carried out for 15 times to obtain a micro/nano cellulose suspension, the light transmittance of the suspension under the irradiation of visible light with the wavelength of 700nm is 14.45%, and the fiber diameter is 42.57 nm.
(2) Concentration of micro/nanocellulose: 2 wt% (relative to the absolute dry micro/nano cellulose) of polyvinylpyrrolidone is added into the prepared micro/nano cellulose suspension, and the mixture is mechanically stirred uniformly at 300 r/min. Centrifuging at 2500r/min for 20min in a centrifuge to obtain the solid content of the micro/nano cellulose of 9.95 wt%.
(3) Redispersion of micro/nanocellulose: polyvinylpyrrolidone is added into the concentrated micro/nano-cellulose to 2 wt% (relative to the absolute dry micro/nano-cellulose), and then the concentrated micro/nano-cellulose is diluted to 0.5 wt% and passes through a gap of ultra-micro particles with the diameter of 20 mu m, and the rotating speed is 800 r/min. The stable micro/nano cellulose suspension with the light transmittance of 9.72 percent under the irradiation of visible light with the wavelength of 700nm is obtained, the fiber diameter is 50.74nm, which shows that the solid content of the concentrated micro/nano cellulose is effectively improved by adding the polyvinylpyrrolidone, and the size of the redispersed micro/nano cellulose is smaller.
Example 2
(1) Preparing micro/nano cellulose: a micro/nanocellulose suspension was prepared as in example 1.
(2) Concentration of micro/nanocellulose: to the prepared micro/nanocellulose suspension 8 wt% (relative to the oven dried micro/nanocellulose) of polyvinylpyrrolidone was added and mechanically stirred homogeneously at 500 r/min. Centrifuging at 2500r/min for 20min in a centrifuge to obtain the solid content of the micro/nano cellulose of 11.07 wt%.
(3) Polyvinylpyrrolidone is added into the concentrated micro/nano-cellulose to 8 wt% (relative to the absolute dry micro/nano-cellulose), and then the concentrated micro/nano-cellulose is diluted to 0.5 wt% and passes through a gap of ultra-micro particles with the diameter of 20 mu m, and the rotating speed is 800 r/min. The stable micro/nano cellulose suspension with the light transmittance of 12.30 percent under the irradiation of visible light with 700nm is obtained, the fiber diameter is 48.82nm, and the addition of polyvinylpyrrolidone is illustrated as b in figures 1 and 2, so that the concentration of the micro/nano cellulose is effectively improved, the flocculation of the micro/nano cellulose in the concentration process is inhibited, and the stability of the suspension is improved.
Example 3
(1) Preparing micro/nano cellulose: a micro/nanocellulose suspension was prepared as in example 1.
(2) Concentration of micro/nanocellulose: 0 wt% (relative to the absolute dry micro/nano cellulose) of polyvinylpyrrolidone is added into the prepared micro/nano cellulose suspension, and the mixture is mechanically stirred uniformly at 500 r/min. Centrifuging for 15min at 2500r/min in a centrifuge to obtain the solid content of the micro/nano cellulose of 9.00 wt%.
(3) Polyvinylpyrrolidone is added into the concentrated micro/nano-cellulose to 0 wt% (relative to the absolute dry micro/nano-cellulose), and then the concentrated micro/nano-cellulose is diluted to 0.5 wt% and passes through a gap of ultra-micro particles with the diameter of 50 mu m, and the rotating speed is 800 r/min. The stable micro/nano cellulose suspension with the light transmittance of 18.64 percent under the irradiation of visible light at 700nm is obtained, the fiber diameter is 42.27nm, and the result shows that the micro/nano cellulose with the clearance of-50 mu m can effectively disperse flocculated micro/nano cellulose to form stable suspension, and the fiber size is smaller.
Example 4
(1) Preparing micro/nano cellulose: a micro/nanocellulose suspension was prepared as in example 1.
(2) Concentration of micro/nanocellulose: 5 wt% (relative to the absolutely dry micro/nano cellulose) of polyvinylpyrrolidone is added into the prepared micro/nano cellulose suspension, and the mixture is mechanically stirred uniformly at 500 r/min. Centrifuging at 2500r/min for 10min in a centrifuge to obtain the solid content of the micro/nano cellulose of 4.28 wt%.
(3) And (3) adding polyvinylpyrrolidone into the concentrated micro/nano cellulose to 5 wt%, diluting to 0.5 wt%, and passing through a gap of ultrafine particles with the diameter of-20 μm at the rotation speed of 800 r/min. The stable micro/nano cellulose suspension with the light transmittance of 14.03 percent under the irradiation of visible light with the wavelength of 700nm is obtained, the fiber diameter is 46.68nm, which shows that the flocculation degree of the micro/nano cellulose is lower, the suspension is more stable and the fiber size is smaller under the condition of shorter centrifugation time.
Comparative example 1
(1) Preparing micro/nano cellulose: a micro/nanocellulose suspension was prepared as in example 1.
(2) Concentration of micro/nanocellulose: to the prepared micro/nanocellulose suspension was added 0 wt% (relative to oven dried micro/nanocellulose) of polyvinylpyrrolidone and mechanically stirred homogeneously at 500 r/min. Centrifuging at 2500r/min for 20min in a centrifuge to obtain the solid content of the micro/nano cellulose of 9.00 wt%.
(3) Adding polyvinylpyrrolidone into the concentrated micro/nano cellulose to 0 wt%, diluting to 0.5 wt%, and passing through the gap of ultramicron-20 μm at rotation speed of 800 r/min. A micro/nanocellulose suspension with a light transmission of 12.53% under visible light irradiation at 700nm was obtained, with a fibre diameter of 57.45nm, as in fig. 1, a in fig. 2. As can be seen from the comparison of this comparative example with example 2, during the concentration and dehydration process, no polyvinylpyrrolidone was added, and agglomeration occurred between the micro/nanocellulose, and the fiber size increased.
Comparative example 2
(1) Preparing micro/nano cellulose: a micro/nanocellulose suspension was prepared as in example 1.
(2) Concentration of micro/nanocellulose: to the prepared micro/nanocellulose suspension was added 0 wt% (relative to oven dried micro/nanocellulose) of polyvinylpyrrolidone and mechanically stirred homogeneously at 500 r/min. Centrifuging for 15min at 2500r/min in a centrifuge to obtain the solid content of the micro/nano cellulose of 9.00 wt%.
(3) The concentrated micro/nano cellulose is supplemented and added with polyvinylpyrrolidone to 0 wt%, then diluted to 0.5 wt%, and passed through the gaps of 0 μm of ultramicron with the rotation speed of 800 r/min. A micro/nanocellulose suspension with a light transmission of 15.99% under irradiation with visible light at 700nm was obtained, the fibre diameter being 66.60 nm. As can be seen from the comparison of this comparative example with example 3, at low gap, the concentrated micro/nanocellulose could not be effectively redispersed, the light transmittance of the suspension was low, and the fiber size was large.
Comparative example 3
(1) Preparing micro/nano cellulose: a micro/nanocellulose suspension was prepared as in example 1.
(2) Concentration of micro/nanocellulose: 10 wt% (relative to the absolutely dry micron/nano cellulose) of polyvinylpyrrolidone is added into the prepared micron/nano cellulose suspension, and the mixture is mechanically stirred uniformly at 500 r/min. And centrifuging the mixture for 20min at 2500r/min in a centrifuge to obtain the solid content of the micro/nano cellulose of 11.63 wt%.
(3) Adding polyvinylpyrrolidone into the concentrated micro/nano cellulose to 10 wt%, diluting to 0.5 wt%, and passing through the gap of ultramicron-20 μm at rotation speed of 800 r/min. A micro/nanocellulose suspension with a light transmission of 10.63% under irradiation with visible light at 700nm was obtained, the fibre diameter being 52.81 nm. As can be seen from the comparison of the comparative example and example 2, the concentration of the micro/nano cellulose can be increased under the condition of high consumption of the polyvinylpyrrolidone, but the micro/nano cellulose is seriously flocculated, the dispersion degree is low, the light transmittance of the suspension is low, and the fiber size is large.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A method for efficiently concentrating and re-dispersing micro/nano cellulose is characterized by comprising the following steps:
adding polyvinylpyrrolidone into the micro/nano cellulose suspension, and uniformly stirring to obtain a mixed suspension; and (3) concentrating and dehydrating the mixed suspension, supplementing polyvinylpyrrolidone into the concentrated micro/nano cellulose to the initial addition amount, then adding water for dilution, and then grinding and redispersing the superfine particles.
2. The method according to claim 1, wherein the disc-grinding gap for the ultra-fine particle grinding and redispersion is 0 to-50 μm.
3. The method according to claim 2, wherein the disc-grinding gap for the ultra-fine particle grinding and redispersion is from-20 to-50 μm.
4. The method according to any one of claims 1 to 3, wherein the polyvinylpyrrolidone is added in an amount of 2 to 8 wt% of the micro/nanocellulose.
5. The method according to any one of claims 1 to 3, wherein the concentration dehydration is centrifugal dehydration, the centrifugation rate is 1500 to 5000r/min, and the centrifugation time is 10 to 20 min.
6. The method according to any one of claims 1 to 3, wherein the rotation speed for grinding and redispersing the ultrafine particles is 600 to 2000 r/min.
7. The method according to any one of claims 1 to 3, wherein the concentration of the micro/nanocellulose obtained by grinding and redispersing the ultrafine particles is 0.2 to 2.0 wt%.
8. A method according to any one of claims 1-3, characterised in that the micro/nano-cellulose suspension has a concentration of 0.5-1.0 wt%.
9. The method according to claim 8, wherein the micro/nanocellulose suspension is prepared from a vegetable fibre raw material by an enzymatic pre-treatment/mechanical grinding process; the mechanical grinding is to grind the mixture to a stable suspension state by adopting at least one of an ultramicron grinder, a nanometer micro-jet homogenizer and a high-pressure homogenizer; the enzyme pretreatment is endonuclease pretreatment.
10. The method according to any one of claims 1 to 3, wherein the polyvinylpyrrolidone is added to the micro/nano cellulose suspension, and then mechanically stirred until the system is uniform, wherein the stirring speed is 200 to 1000 r/min.
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