CN102899950B - A kind of ultrasonic-microwave is the auxiliary method preparing nano-cellulose simultaneously - Google Patents
A kind of ultrasonic-microwave is the auxiliary method preparing nano-cellulose simultaneously Download PDFInfo
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Abstract
The invention discloses a kind of ultrasonic-microwave auxiliary method preparing nano-cellulose simultaneously, belong to biomass nano Material Field.This nano material take liquid acid as catalyst, impels the effectively hydrolyzing of cellulose amorphous region simultaneously, realize preparing nano-cellulose fast by plant fiber material under ultrasonic wave and microwave are assisted.This preparation method comprises the acid hydrolysis of plant cellulose, the centrifugal recovery of liquid acid, the centrifugation of nano-cellulose.The present invention makes full use of hyperacoustic mechanical dispersion effect, ultrasound cavitation effect, microwave homogeneous heating effect, the catalytic action of liquid acid and the synergy that produces between them, the hydrolytic process of resistant cellulose, thus realize nano-cellulose efficient, prepare fast.The nano cellulose material of preparation can be used for food additives, drug excipient, engineering material additive, speciality paper additive etc.
Description
Technical field
The present invention relates to a kind of ultrasonic-microwave auxiliary method preparing nano-cellulose simultaneously, belong to biomass nano Material Field.
Background technology
Nano-cellulose typically refers to size in a certain dimension in space and reaches the high molecular cellulose of 1-100 nm.Compared with native cellulose, nano cellulose crystal has many premium properties, as larger specific area, high-crystallinity, high-hydrophilic, high-modulus, high strength, hyperfine structure and high transparent etc.Therefore, nano-cellulose has good using value in the wild phase of food additives, composite, tissue engineering bracket and filter medium are prepared etc.At present, the preparation method of nano-cellulose is mainly divided into chemical method, Physical, bioanalysis three kinds.Chemical method normally with liquid acid or alkali for catalyst, prepare nano-cellulose by the hydrolysis of cellulosic material; Physical mainly impels cellulose to become nano level cellulose by heating explosion, homogenizer, the physical method such as high-pressure homogeneous; Biological rule mainly utilizes bacterium to prepare nano-cellulose to cellulosic biochemical action.In above-mentioned three kinds of methods, the energy ezpenditure of Physical is higher, product purity is low; Biological preparation complexity, length consuming time, cost are high, price; Though chemical method is easy to surface-modified nano cellulose, but usually need strong acid or highly basic as catalyst, require higher to consersion unit, catalyst recovery is also more difficult.Therefore, the research emphasis in the further preparation method of research and improvement nano-cellulose still this field.In recent years, ultrasonic assistant is adopted to prepare the method for nanofiber by wide coverage through acid hydrolysis.The method is that the one of chemical method and Physical organically combines, and takes full advantage of hyperacoustic mechanical dispersion, ultrasound cavitation effect, and the cooperative effect between ultrasonic wave and acid catalysis, presents good application prospect.But ultrasonic assistant is prepared nanofiber and still be there are some defects, as sour large usage quantity, preparation time is also longer, and step is relatively many, mostly also needs to carry out high-pressure homogeneous or acid hydrolysis preliminary treatment to plant fiber material, etc.Therefore, on the basis of ultrasonic assistant, if adopt further reinforcement technique, overcome or improve the defect that ultrasonic assistant prepares nano-cellulose, be then expected to develop a kind of more efficient, clean, energy-conservation nano-cellulose preparation method.In recent years, the development of ultrasonic-microwave associating ancillary technique is swift and violent, application particularly in chemical reaction, extract and separate field has received the concern of numerous researcher, pertinent literature also demonstrate that in this associating ancillary technique can produce synergy between ultrasonic wave and microwave, can strengthen chemical process further, but it is preparing the also rarely seen report of the application in biomass nano Material Field.
Summary of the invention
The object of the present invention is to provide a kind of by the ultrasonic-microwave auxiliary method preparing nano-cellulose simultaneously.The present invention makes full use of hyperacoustic mechanical dispersion effect, ultrasound cavitation effect, microwave homogeneous heating effect, the catalytic action of liquid acid and the synergy that produces between them, the hydrolytic process of resistant cellulose, thus realize nano-cellulose efficient, prepare fast.
For achieving the above object, the present invention adopts following technical scheme:
Ultrasonic-microwave is the auxiliary method preparing nano-cellulose simultaneously, and concrete steps are as follows:
1) acid hydrolysis of plant cellulose: take string as raw material, after fully mixing with the liquid acid of mass concentration 10-60%, be placed in microwave and ultrasonic wave synergic extraction instrument, at 50-80 DEG C and ultrasonic-microwave auxiliary lower hydrolysis 0.5-2.0h simultaneously, gained mixture is for subsequent use;
2) the centrifugal recovery of liquid acid: by step 1) gained mixture centrifugation 5-10min under 4000-7000rad/min, the supernatant liquor of collection is aq acid soln, recycle after concentrated, bottom solid phase is for subsequent use;
3) centrifugation of nano-cellulose: by step 2) bottom solid phase mix with deionized water, and adjust ph is to neutral, centrifugation 5-10min under 4000-7000rad/min, collects upper phase; Repeat above-mentioned dilution, centrifugation step 2-6 time, merging upper phase is nano-cellulose colloidal solution, obtains white nano-cellulose powder after freeze drying.
String described in step 1) is the one in all kinds of filter paper, wood pulp fibre, bamboo pulp fiber.
Liquid acid described in step 1) is the one in sulfuric acid, phosphoric acid, hydrochloric acid.
Adjust ph described in step 3) to neutrality is by adding calcium oxide to be adjusted to neutrality.
The technological parameter of step (1) described ultrasonic-microwave is: ultrasonic wave 40KHz, 50W; Microwave 2450MHz, 10-800W.
More preferably, the acid hydrolysis of step 1) plant cellulose: take string as raw material, after fully mixing with the liquid acid of mass concentration 30-55%, be placed in microwave and ultrasonic wave synergic extraction instrument, at 60-80 DEG C and ultrasonic-microwave auxiliary lower hydrolysis 1.0-2.0h simultaneously, gained mixture is for subsequent use.
Described nano cellulose material can be used for food additives, drug excipient, engineering material additive, speciality paper additive etc.
Remarkable advantage of the present invention is: the present invention prepares nano-cellulose under ultrasonic-microwave is simultaneously auxiliary, make full use of hyperacoustic mechanical dispersion effect, ultrasound cavitation effect, microwave homogeneous heating effect, the catalytic action of liquid acid and the synergy that produces between them, the hydrolytic process of resistant cellulose, thus realize nano-cellulose efficient, prepare fast.Obtained material nano cellulosic material can be used for food additives, drug excipient, engineering material additive, speciality paper additive etc.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope figure of nano-cellulose of the present invention.
Fig. 2 is the X-ray diffraction spectrogram of filter paper raw material of the present invention and nano-cellulose product: a filter paper; B nano-cellulose.
Fig. 3 is Fourier transform infrared spectroscopy figure: a filter paper of filter paper raw material of the present invention and nano-cellulose product; B nano-cellulose.
Detailed description of the invention
The preparation method of nano-cellulose of the present invention, comprises the acid hydrolysis of plant cellulose, the centrifugal recovery of liquid acid, the centrifugation of nano-cellulose; Specifically comprise the following steps:
1) acid hydrolysis of plant cellulose: getting 0.5-3.0g sponge is raw material, after fully mixing with mass concentration 10-60%, volume 40-60mL liquid acid, be placed in microwave and ultrasonic wave synergic extraction instrument, for subsequent use after 50-80 DEG C and ultrasonic-microwave assist lower hydrolysis 0.5-2.0h simultaneously.
2) the centrifugal recovery of liquid acid: by the mixture of step 1) centrifugation 5-10min under 4000-7000rad/min, the supernatant liquor of collection is aq acid soln, can be recycled after rotary evaporation anhydrates, and bottom solid phase is for subsequent use.
3) centrifugation of nano-cellulose: by step 2) solid product mix with 50-200mL deionized water, by adding a small amount of CaO adjust ph to neutral, centrifugation 5-10min under 4000-7000rad/min, collect upper phase; Without the need to adjust ph, repeat above-mentioned dilution, centrifugation step 2-6 time.The upper phase of collecting is milky white nano-cellulose colloidal solution, can obtain white nano-cellulose powder after freeze drying.
Embodiment 1
Ultrasonic-microwave is the auxiliary method preparing nano-cellulose simultaneously, comprises the following steps:
1) acid hydrolysis of plant cellulose: get after 0.5g filter paper fragment fully mixes with mass concentration 50%, 40mL sulfuric acid, in ultrasonic-microwave combined extraction instrument at 65 DEG C ultrasonic-microwave (ultrasonic wave: 40KHz, 50W; Microwave: 2450MHz, 10-800W are according to establishing temperature automatic adjustment) simultaneously for subsequent use after assisted reaction 1.5h.
2) the centrifugal recovery of liquid acid: by the mixture of step 1) centrifugation 7min under 6000rad/min, the supernatant liquor of collection is sulfuric acid solution, can be recycled after rotary evaporation anhydrates, and bottom solid phase is for subsequent use.
3) centrifugation of nano-cellulose: by step 2) solid product mix with 100mL deionized water, by adding a small amount of CaO adjust ph to neutral, centrifugation 7min under 6000rad/min, collect upper phase; Without the need to adjust ph, repeat above-mentioned dilution, centrifugation step 3 times.The upper phase of collecting is milky white nano-cellulose colloidal solution, can obtain white nano-cellulose powder after freeze drying.
Embodiment 2
Ultrasonic-microwave is the auxiliary method preparing nano-cellulose simultaneously, comprises the following steps:
1) acid hydrolysis of plant cellulose: get after 1.5g wood pulp fibre fully mixes with mass concentration 55%, 50mL phosphoric acid, in ultrasonic-microwave combined extraction instrument at 60 DEG C ultrasonic-microwave (ultrasonic wave: 40KHz, 50W; Microwave: 2450MHz, 10-800W are according to establishing temperature automatic adjustment) simultaneously for subsequent use after assisted reaction 2.0h.
2) the centrifugal recovery of liquid acid: by the mixture of step 1) centrifugation 8min under 5000rad/min, the supernatant liquor of collection is phosphoric acid solution, can be recycled after rotary evaporation anhydrates, and bottom solid phase is for subsequent use.
3) centrifugation of nano-cellulose: by step 2) solid product mix with 150mL deionized water, by adding a small amount of CaO adjust ph to neutral, centrifugation 8min under 5000rad/min, collect upper phase; Without the need to adjust ph, repeat above-mentioned dilution, centrifugation step 4 times.The upper phase of collecting is milky white nano-cellulose colloidal solution, can obtain white nano-cellulose powder after freeze drying.
Embodiment 3
Ultrasonic-microwave is the auxiliary method preparing nano-cellulose simultaneously, comprises the following steps:
1) acid hydrolysis of plant cellulose: get after 1.0g bamboo pulp fiber fully mixes with mass concentration 50%, 50mL sulfuric acid, in ultrasonic-microwave combined extraction instrument at 70 DEG C ultrasonic-microwave (ultrasonic wave: 40KHz, 50W; Microwave: 2450MHz, 10-800W are according to establishing temperature automatic adjustment) simultaneously for subsequent use after assisted reaction 1.0h.
2) the centrifugal recovery of liquid acid: by the mixture of step 1) centrifugation 5min under 7000rad/min, the supernatant liquor of collection is phosphoric acid solution, can be recycled after rotary evaporation anhydrates, and bottom solid phase is for subsequent use.
3) centrifugation of nano-cellulose: by step 2) solid product mix with 150mL deionized water, by adding a small amount of CaO adjust ph to neutral, centrifugation 5min under 7000rad/min, collect upper phase; Repeat above-mentioned dilution, centrifugation step 2 times.The upper phase of collecting is milky white nano-cellulose colloidal solution, can obtain white nano-cellulose powder after freeze drying.
Embodiment 4
Ultrasonic-microwave is the auxiliary method preparing nano-cellulose simultaneously, comprises the following steps:
1) acid hydrolysis of plant cellulose: get after 3.0g filter paper fragment fully mixes with mass concentration 30%, 60mL hydrochloric acid, in ultrasonic-microwave combined extraction instrument at 80 DEG C ultrasonic-microwave (ultrasonic wave: 40KHz, 50W; Microwave: 2450MHz, 10-800W are according to establishing temperature automatic adjustment) simultaneously for subsequent use after assisted reaction 2.0h.
2) the centrifugal recovery of liquid acid: by the mixture of step 1) centrifugation 10min under 4000rad/min, the supernatant liquor of collection is hydrochloric acid solution, can be recycled after rotary evaporation anhydrates, and bottom solid phase is for subsequent use.
3) centrifugation of nano-cellulose: by step 2) solid product mix with 200mL deionized water, by adding a small amount of CaO adjust ph to neutral, centrifugation 10min under 4000rad/min, collect upper phase; Without the need to adjust ph, repeat above-mentioned dilution, centrifugation step 6 times.The upper phase of collecting is milky white nano-cellulose colloidal solution, can obtain white nano-cellulose powder after freeze drying.
Embodiment 5
The microscopic appearance of Japanese JEOL JEM-1010 transmission electron microscope (TEM) to sample is adopted to characterize.As shown in Figure 1, nano-cellulose is beard shape, and diameter and length are comparatively even, and diameter is about 30-50nm, and length is about 200-500nm, and local complexity, intersection are in netted.This characterization result confirms intuitively and adopts ultrasonic-microwave simultaneously ancillary technique, can lower acid concentration, without feed pretreatment step and the condition of shorter reaction time under can prepare nano-cellulose.The nano-cellulose that the present invention prepares compared with ultrasonic assistive technologies is more efficient, clean, energy-conservation.
Embodiment 6
Dutch Philip X'Pert Pro MPD X-ray powder diffractometer is adopted to characterize filter paper raw material and nano-cellulose powder, the filtering of characteristic ray Co-Ka, Ni sheet, accelerating potential 80 Kv, sweep speed 0.2
o/ sec, sweep limits 10
o-90
o.As seen from Figure 2, the X-ray diffraction spectrogram broadly similar of nano-cellulose and filter paper, proves that cellulosic crystalline form does not change in preparation process, still remains the crystal formation feature of cellulose Ⅰ.But the peak width of nano-cellulose diffraction maximum obviously narrows, peak becomes by force large, illustrates that its crystal grain is less.In addition, from the diffraction peak intensity of 002 crystal face and 001 crystal face, the X-ray degree of crystallinity of nano-cellulose increases to 68% by 52% of filter paper raw material.Comprehensive transmission electron microscope picture and X-ray diffraction spectrogram known, ultrasonic wave, microwave, acid-hydrolyzed cooperative effect mainly act on cellulosic part amorphous district, thus cause cellulosic material to be peeled off, rupture, broken etc., impel cellulosic length and rugosity to be tending towards nano-scale.
Embodiment 7
Thermo electro company of U.S. Nicolet 380 type Fourier transform infrared spectrometer adopts KBr pressed disc method to carry out spectrum analysis (Fig. 3) to filter paper raw material and nano-cellulose powder, and sample quality accounts for 0.7% of tablet quality.3345 cm in collection of illustrative plates
-1absworption peak belongs to the characteristic absorption peak of hydroxyl in cellulose; 2902 cm
-1that corresponding is methylene (-CH
2-) C-H symmetrical stretching vibration absworption peak; 1055 cm
-1absworption peak belongs to C-O stretching vibration of cellulose alcohol, and 1112 near it and 1160 cm
-1acromion belongs to C-O stretching vibration absworption peak of cellulosic molecule inner ether and the stretching vibration absworption peak of C-C framework respectively.At 1429 cm
-1near have the flexural vibrations absworption peak of saturated C-H, 899 cm
-1then correspond to cellulose anomeric carbon (C
1) vibration absorption peak.Compared with filter paper, the absworption peak wave number of nano-cellulose is without significant change, and the surface functional group kind of both explanations is basically identical, and the intensity of nano-cellulose absworption peak be more greatly contain more horn of plenty because of its high-specific surface area surface functional group caused by.The nano-cellulose that in the IR Characterization result of this sample and document, ultrasonic assistant is prepared is basically identical, illustrate that the application of ancillary technique while of ultrasonic-microwave does not change the surface functional group of nano-cellulose, just enhance the forming process of nano-cellulose.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (4)
1. the ultrasonic-microwave auxiliary method preparing nano-cellulose simultaneously, is characterized in that: the concrete steps of described method are as follows:
1) acid hydrolysis of plant cellulose: take string as raw material, after fully mixing with the liquid acid of mass concentration 30%, be placed in microwave and ultrasonic wave synergic extraction instrument, at 60-80 DEG C and ultrasonic-microwave auxiliary lower hydrolysis 1.0-2.0h simultaneously, gained mixture is for subsequent use;
2) the centrifugal recovery of liquid acid: by step 1) gained mixture centrifugation 5-10min under 4000-7000rad/min, the supernatant liquor of collection is aq acid soln, recycle after concentrated, bottom solid phase is for subsequent use;
3) centrifugation of nano-cellulose: by step 2) bottom solid phase mix with deionized water, and adjust ph is to neutral, centrifugation 5-10min under 4000-7000rad/min, collects upper phase; Repeat above-mentionedly to mix with deionized water, centrifugation step 2-6 time, merging upper phase is nano-cellulose colloidal solution, obtains white nano-cellulose powder after freeze drying;
The technological parameter of ultrasonic-microwave described in step 1) is: ultrasonic wave 40KHz, 50W; Microwave 2450MHz, 10-800W.
2. the preparation method of nano-cellulose according to claim 1, is characterized in that: the string described in step 1) is the one in all kinds of filter paper, wood pulp fibre, bamboo pulp fiber.
3. the preparation method of nano-cellulose according to claim 1, is characterized in that: the liquid acid described in step 1) is the one in sulfuric acid, phosphoric acid, hydrochloric acid.
4. the preparation method of nano-cellulose according to claim 1, is characterized in that: the adjust ph described in step 3) to neutrality is by adding calcium oxide to be adjusted to neutrality.
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| JP7232072B2 (en) | 2019-02-15 | 2023-03-02 | 第一工業製薬株式会社 | MODIFIED CELLULOSE NANOFIBER, GAS BARRIER MATERIAL AND GAS BARRIER MOLDED PRODUCT |
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| CN107417797A (en) * | 2017-06-12 | 2017-12-01 | 福建农林大学 | It is a kind of to prepare the method for being esterified nano-cellulose by transesterification |
| CN108371237A (en) * | 2018-03-19 | 2018-08-07 | 上海同化新材料科技有限公司 | Feed addictive preparation method and product |
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| IT202200007589A1 (en) | 2022-04-15 | 2023-10-15 | Pabif Srl | PROCESS AND APPARATUS FOR THE PRODUCTION OF LEVULINIC ACID FROM CELLULOSE OBTAINED FROM BIOMASS |
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