CN108641114A - A kind of preparation method of nanometer bacteria cellulose whisker - Google Patents
A kind of preparation method of nanometer bacteria cellulose whisker Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of nanometer bacteria cellulose whisker, include the following steps：The bacteria cellulose sterilizing and washing that culture is obtained is for use；The bacteria cellulose cleaned up is dried；Bacteria cellulose after drying is put into acid solution and is stood；Constant temperature stirs after the bacteria cellulose complete swelling of above-mentioned standing；Above-mentioned reactant ultrasound is continued into assisted reaction again；By reaction terminate product with deionized water centrifuge washing for several times after, dialysed, ultrasonic disperse, finally obtain nanometer bacteria cellulose whisker colloid.The nanometer bacteria cellulose whisker of the present invention program preparation is at low cost, yield is high, reaction is mild, speed is fast, and draw ratio is big, and good dispersibility is presented in water.
Description
Technical field
The invention belongs to technical field of biological materials, and in particular to a kind of nanometer bacteria cellulose polyvinyl alcohol poly- second two
Porous compound hydrogel material of alcohol and preparation method thereof.
Background technology
Bacteria cellulose (Bacterial Cellulose, abbreviation BC) is by the bacteriogenic a kind of producing high-molecular in part
Object is closed, plant cellulose is superior in terms of the physicochemical properties such as purity, tensile strength, Young's modulus, and there is higher biology
Adaptability can directly degrade in nature.As a kind of novel biomaterial, bacteria cellulose is in medicine, papermaking, biology doctor
It learns, there is wide application prospect in food.
Cellulosic molecule and its supermolecule aggregation are manipulated in nano-scale range, designs and assembles stable multiple flower
The new nanometer fine chemical product of excellent function, new nano material are provided in sample, thus initiative, become the forward position neck of Cellulose Science
Domain.Compared with powder cellulose and microcrystalline cellulose, nano-cellulose there are many excellent performance, as high-purity, high polymerization degree,
High-crystallinity, high-hydrophilic, high Young's modulus, high intensity, hyperfine structure and high transparency etc..Therefore, nano-cellulose
The research of preparation, properity and application is being currently the emphasis and hot spot of domestic and international cellulose chemistry research.
Document 1 (Li Jinling, Zhou Liujia, leaf prepare nano-cellulose whisker South China Science ＆ Engineering University for brave copper sulphate co-catalysis)
Report a kind of method preparing nano-cellulose whisker using copper sulphate co-catalysis, hydrolysis absorbent cotton.Although can be faster
Nano-cellulose whisker is prepared, but its draw ratio is general, it is not particularly pertinent.
Patent 1 (201611202906.7) discloses a kind of method preparing nano-cellulose whisker using Ramulus Mori, makes
Acidolysis twice is carried out respectively with the ethanol solution of nitric acid and sulfuric acid solution, and nano-cellulose whisker is finally prepared.However this
Nano-cellulose whisker obtained by kind method, not only distribution of lengths is wide, and diameter distribution is very wide, and draw ratio is not high.
Patent 2 (201310610082.7) discloses a kind of method preparing nano-cellulose whisker using garlic skin, passes through
One systems such as swelling, lye boiling degumming, Polyose extraction, bleaching, sanded treatment, acidification hydrolization, washing dialysis/freeze-drying
Row process, is prepared a diameter of 20nm~30nm, and length is the nano-cellulose whisker of 300nm~2 μm.It is this to utilize garlic skin
Preparation method process it is complicated, and easily introduce impurity, the impurity of script also necessarily has residual in garlic skin.
Invention content
Technical problem：In order to solve the defects of prior art, the present invention provides a kind of nanometer bacteria cellulose whiskers
Preparation method.
Technical solution：The preparation method of nanometer bacteria cellulose whisker provided by the invention includes the following steps：
Step 1：The bacteria cellulose sterilizing and washing that culture is obtained is for use；
Step 2：The bacteria cellulose cleaned up in above-mentioned steps is dried；
Step 3：Bacteria cellulose after being dried in above-mentioned steps is put into acid solution and is stood；
Step 4：It is stirred after the bacteria cellulose complete swelling stood in above-mentioned steps, then by its constant temperature；
Step 5：Reactant in above-mentioned steps ultrasound is continued into assisted reaction；
Step 6：The product that above-mentioned reaction is terminated with deionized water centrifuge washing for several times after, then dialysed, ultrasound point
It dissipates, finally obtains nanometer bacteria cellulose whisker colloid.
As a kind of prioritization scheme：Bacteria cellulose is the bacteria cellulose that acetobacter xylinum ferments, sterilizing in step 1
The pure bacteria cellulose obtained afterwards is cotton-shaped or membranaceous.
As advanced optimizing scheme：Sterilizing and washing concrete operation step is in step 1：With mass fraction 0.1%~4%
NaOH and 0.1%~4%H2O2After 60~90 DEG C of immersion treatments 1~5 hour, cleaned up with deionized water.
As advanced optimizing scheme：Drying temperature described in step 2 is 47-54 DEG C, and the time is 2~8 hours.
As advanced optimizing scheme：Acid solution described in step 3 is in sulfuric acid, hydrochloric acid, nitric acid, acetic acid and ethanedioic acid
It is one or more of；And the mass concentration of each acid solution is all 50%~65%.
As advanced optimizing scheme：Constant temperature whipping temp described in step 4 is 45~60 DEG C, and the time is 2~8h.
As advanced optimizing scheme：The time that ultrasonic wave added described in step 5 reacts is 2~8h.
As advanced optimizing scheme：Bacteria cellulose is put into acid solution according to the ratio of 0.01-0.05g/mL in step 3
In.
Advantageous effect：The nanometer bacteria cellulose whisker of the present invention program preparation is at low cost, yield is high, reaction is mild, speed
Degree is fast, and draw ratio is big, and good dispersibility is presented in water.
Description of the drawings
Fig. 1 is the preparation flow figure of nanometer bacteria cellulose whisker；
Fig. 2 is the transmission electron microscope picture of the nanometer bacteria cellulose whisker hydrolyzed in embodiment 1；
Fig. 3 is the infrared comparison diagram of nanometer bacteria cellulose whisker and bacteria cellulose original film that embodiment 1 is prepared；
Fig. 4 is the XRD comparison diagrams of nanometer bacteria cellulose whisker and bacteria cellulose original film that embodiment 2 is prepared；
Fig. 5 is the grain size and Zeta point distribution maps for the nanometer bacteria fibrous crystal palpus that embodiment 3 is prepared.
Specific implementation mode
In the following with reference to the drawings and specific embodiments, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate
It the present invention rather than limits the scope of the invention, after having read the present invention, those skilled in the art are to of the invention each
The modification of kind equivalent form falls within the application range as defined in the appended claims.
Technical solution：The preparation method of nanometer bacteria cellulose whisker provided by the invention includes the following steps：
Step 1：The bacteria cellulose sterilizing and washing that culture is obtained is for use；
Step 2：The bacteria cellulose cleaned up in above-mentioned steps is dried；
Step 3：Bacteria cellulose after being dried in above-mentioned steps is put into acid solution and is stood；
Step 4：It is stirred after the bacteria cellulose complete swelling stood in above-mentioned steps, then by its constant temperature；
Step 5：Reactant in above-mentioned steps ultrasound is continued into assisted reaction；
Step 6：The product that above-mentioned reaction is terminated with deionized water centrifuge washing for several times after, then dialysed, ultrasound point
It dissipates, finally obtains nanometer bacteria cellulose whisker colloid.
As a kind of prioritization scheme：Bacteria cellulose is the bacteria cellulose that acetobacter xylinum ferments in step 1.
As advanced optimizing scheme：Sterilizing and washing concrete operation step is in step 1：With mass fraction 0.1%~4%
NaOH and 0.1%~4%H2O2After 60~90 DEG C of immersion treatments 1~5 hour, cleaned up with deionized water.
As advanced optimizing scheme：Drying temperature described in step 2 is 47-54 DEG C, and the time is 2~8 hours.
As advanced optimizing scheme：Acid solution described in step 3 is in sulfuric acid, hydrochloric acid, nitric acid, acetic acid and ethanedioic acid
It is one or more of；Its mass concentration is 50%~65%.
As advanced optimizing scheme：Constant temperature whipping temp described in step 4 is 45~60 DEG C, and the time is 2~8h.
As advanced optimizing scheme：The time that ultrasonic wave added described in step 5 reacts is 2~8h.
As advanced optimizing scheme：Bacteria cellulose is put into acid solution according to the ratio of 0.01-0.05g/mL in step 3
In.
Embodiment 1
The bacteria cellulose film for taking acetobacter xylinum dynamic fermentation, with the NaOH and 0.2%H of mass fraction 0.2%2O280
It handles 2 hours under the conditions of DEG C, is cleaned up later with deionized water, obtain pure bacteria cellulose raw material.It will handle clean
Bacterial cellulose wet-coating be cut into the fritter of 1cm × 1cm, be placed in baking oven and dried, drying temperature is 47 DEG C, the time 8
Hour, remove most moisture.The sulfuric acid solution of configuration 50%, the bacteria cellulose that second step obtains is added by 0.01g/mL
Enter and stood in sulfuric acid solution liquid, waits for its swelling.After bacteria cellulose complete swelling, places it under 45 DEG C of constant temperatures and stirs,
Reaction 6h is hydrolyzed.Above-mentioned reactant is put into ultrasonic cleaning machine, the reaction was continued 3h.After reaction, the production after hydrolysis
Object for several times, then is dialysed, ultrasonic disperse with deionized water centrifuge washing, obtains nanometer bacteria cellulose whisker colloid.
Embodiment 2
The bacteria cellulose film for taking acetobacter xylinum dynamic fermentation, with the NaOH and 0.2%H of mass fraction 0.2%2O280
It handles 2 hours under the conditions of DEG C, is cleaned up later with deionized water, obtain pure bacteria cellulose raw material.It will handle clean
Bacterial cellulose wet-coating be cut into the fritter of 1cm × 1cm, be placed in baking oven and dried, drying temperature is 54 DEG C, the time 2
Hour, remove most moisture.The sulfuric acid solution of configuration 50%, the bacteria cellulose that second step obtains is added by 0.05g/mL
Enter and stood in sulfuric acid solution liquid, waits for its swelling.After bacteria cellulose complete swelling, places it under 50 DEG C of constant temperatures and stirs,
Reaction 6h is hydrolyzed.Above-mentioned reactant is put into ultrasonic cleaning machine, the reaction was continued 3h.After reaction, the production after hydrolysis
Object for several times, then is dialysed, ultrasonic disperse with deionized water centrifuge washing, obtains nanometer bacteria cellulose whisker colloid.
Embodiment 3
The bacteria cellulose film for taking acetobacter xylinum dynamic fermentation, with the NaOH and 0.3%H of mass fraction 0.3%2O280
It handles 2 hours under the conditions of DEG C, is cleaned up later with deionized water, obtain pure bacteria cellulose raw material.It will handle clean
Bacterial cellulose wet-coating be cut into the fritter of 1cm × 1cm, be placed in baking oven and dried, drying temperature is 50 DEG C, the time 5
Hour, remove most moisture.The sulfuric acid solution of configuration 65%, the bacteria cellulose that second step obtains is added by 0.01g/mL
Enter and stood in sulfuric acid solution liquid, waits for its swelling.After bacteria cellulose complete swelling, places it under 50 DEG C of constant temperatures and stirs,
Reaction 6h is hydrolyzed.Above-mentioned reactant is put into ultrasonic cleaning machine, the reaction was continued 3h.After reaction, the production after hydrolysis
Object for several times, then is dialysed, ultrasonic disperse with deionized water centrifuge washing, obtains nanometer bacteria cellulose whisker colloid.
Embodiment 4
The bacteria cellulose film for taking acetobacter xylinum dynamic fermentation, with the NaOH and 0.3%H of mass fraction 0.3%2O280
It handles 2 hours under the conditions of DEG C, is cleaned up later with deionized water, obtain pure bacteria cellulose raw material.It will handle clean
Bacterial cellulose wet-coating be cut into the fritter of 1cm × 1cm, be placed in baking oven and dried, drying temperature is 49 DEG C, the time 7
Hour, remove most moisture.The sulfuric acid solution of configuration 65%, the bacteria cellulose that second step obtains is added by 0.01g/mL
Enter and stood in sulfuric acid solution liquid, waits for its swelling.After bacteria cellulose complete swelling, places it under 50 DEG C of constant temperatures and stirs,
Reaction 6h is hydrolyzed.Above-mentioned reactant is put into ultrasonic cleaning machine, the reaction was continued 3h.After reaction, the production after hydrolysis
Object for several times, then is dialysed, ultrasonic disperse with deionized water centrifuge washing, obtains nanometer bacteria cellulose whisker colloid.
Embodiment 5
The bacteria cellulose film for taking acetobacter xylinum dynamic fermentation, with the NaOH and 0.1%H of mass fraction 0.1%2O260
It handles 5 hours under the conditions of DEG C, is cleaned up later with deionized water, obtain pure bacteria cellulose raw material.It will handle clean
Bacterial cellulose wet-coating be cut into the fritter of 1cm × 1cm, be placed in baking oven and dried, drying temperature is 52 DEG C, the time 3
Hour, remove most moisture.The hydrochloric acid solution of configuration 60%, the bacteria cellulose that second step obtains is added by 0.01g/mL
Enter and stood in sulfuric acid solution liquid, waits for its swelling.After bacteria cellulose complete swelling, places it under 60 DEG C of constant temperatures and stirs,
Reaction 2h is hydrolyzed.Above-mentioned reactant is put into ultrasonic cleaning machine, the reaction was continued 2h.After reaction, the production after hydrolysis
Object for several times, then is dialysed, ultrasonic disperse with deionized water centrifuge washing, obtains nanometer bacteria cellulose whisker colloid.
Embodiment 6
The bacteria cellulose film for taking acetobacter xylinum dynamic fermentation, with the NaOH and 4%H of mass fraction 4%2O2In 90 DEG C of items
It handles 1 hour under part, is cleaned up later with deionized water, obtain pure bacteria cellulose raw material.Totally thin will be handled
Fungin wet film is cut into the fritter of 1cm × 1cm, is placed in baking oven and is dried, and drying temperature is 50 DEG C, and the time is 5 hours,
Remove most moisture.Sulphur is added by 0.03g/mL in the salpeter solution of configuration 60%, the bacteria cellulose that second step is obtained
It is stood in sour acid solution, waits for its swelling.It after bacteria cellulose complete swelling, places it under 55 DEG C of constant temperatures and stirs, carry out
Hydrolysis 8h.Above-mentioned reactant is put into ultrasonic cleaning machine, the reaction was continued 8h.After reaction, the product after hydrolysis is used
Deionized water centrifuge washing for several times, then dialysed, ultrasonic disperse, obtains nanometer bacteria cellulose whisker colloid.
Embodiment 7
The bacteria cellulose film for taking acetobacter xylinum dynamic fermentation, with the NaOH and 2%H of mass fraction 2%2O2In 80 DEG C of items
It handles 2 hours under part, is cleaned up later with deionized water, obtain pure bacteria cellulose raw material.Totally thin will be handled
Fungin wet film is cut into the fritter of 1cm × 1cm, is placed in baking oven and is dried, and drying temperature is 50 DEG C, and the time is 6 hours,
Remove most moisture.Configuration 60% acetic acid and ethanedioic acid mixed solution, the bacteria cellulose that second step is obtained by
0.04g/mL is added in sulfuric acid solution liquid and stands, and waits for its swelling.After bacteria cellulose complete swelling, 55 DEG C of constant temperature items are placed it in
It is stirred under part, reaction 8h is hydrolyzed.Above-mentioned reactant is put into ultrasonic cleaning machine, the reaction was continued 8h.After reaction, water
Product after solution for several times, then is dialysed, ultrasonic disperse with deionized water centrifuge washing, obtains nanometer bacteria cellulose whisker glue
Body.
Nanometer bacteria cellulose whisker after transmission electron microscope observing hydrolysis, the results are shown in Figure 2.After hydrolyzing as can be seen from Figure 2
Nanometer bacteria cellulose length be 300-1000nm, width is in 10-25nm.
As shown in figure 3, a, b curve are respectively the red of bacteria cellulose film (BC) and nanometer bacteria cellulose whisker (NCW)
External spectrum figure compares us and can be found that b curves compare a curves in 1730cm-1Left and right and 920cm-1There is new suction in left and right
Peak is received, they are respectively belonging to C=O stretching vibrations and the O-H out-of-plane bending vibrations of carboxylic acid, illustrate BC in sulphuric acid hydrolysis process
In oxidation reaction has occurred.
As shown in figure 4, a, b curve are respectively the XRD spectra of BC and NCW, two curves at 14.7 °, 16.8 ° and
22.7 ° nearby produce diffraction maximum, correspond to respectively (11-0) of BC, (110) and (020) crystal face.By calculating, we can send out
It is 97% that the crystallization index of existing BC, which is 74%, NCW crystallization indexs, shows that sulphuric acid hydrolysis produces influence, sulfuric acid to its crystallinity
Hydrocellulose occurs mainly in amorphous region.
As shown in Figure 5 a, there are two ranges for size distribution, respectively in 80nm and 500nm or so, illustrate that NCW in water may be used
There can be nanocrystalline and two kinds of forms of nanocrystal aggregates.Shown in Fig. 5 b, the Zeta points of NCW are -40.8mV, illustrate to hydrolyze
Keep its negatively charged, absolute value is more than 30mV, illustrates its energy stable dispersion in water.
Nanometer bacteria cellulose whisker prepared by technical solution of the present invention, length is about 300-1000nm or so, and diameter is about
For 10-25nm, draw ratio is very high.
The nanometer bacteria cellulose colloidal stability that the method for the present invention obtains is high, is not observed under conditions of standing 10 days
To it is any layering or precipitation sediment phenomena such as, illustrate its in water dispersibility it is fabulous.
Due to the high-purity of raw material bacteria cellulose itself, high-crystallinity, nanometer bacteria cellulose whisker that this method obtains
Very high purity, yield are also higher than being obtained with general raw material.
Claims (8)
1. a kind of preparation method of nanometer bacteria cellulose whisker, it is characterised in that：Include the following steps：
Step 1：The bacteria cellulose sterilizing and washing that culture is obtained is for use；
Step 2：The bacteria cellulose cleaned up in above-mentioned steps is dried；
Step 3：Bacteria cellulose after being dried in above-mentioned steps is put into acid solution and is stood；
Step 4：It is stirred after the bacteria cellulose complete swelling stood in above-mentioned steps, then by its constant temperature；
Step 5：Reactant in above-mentioned steps ultrasound is continued into assisted reaction；
Step 6：The product that above-mentioned reaction is terminated with deionized water centrifuge washing for several times after, then dialysed, ultrasonic disperse, most
Nanometer bacteria cellulose whisker colloid is obtained eventually.
2. the preparation method of nanometer bacteria cellulose whisker according to claim 1, it is characterised in that：It is thin described in step 1
Fungin is the bacteria cellulose that acetobacter xylinum ferments.
3. the preparation method of nanometer bacteria cellulose whisker according to claim 1, it is characterised in that：It goes out described in step 1
Bacterium cleans concrete operation step：With the NaOH and 0.1%~4%H of mass fraction 0.1%~4%2O2In 60~90 DEG C of immersions
After processing 1~5 hour, cleaned up with deionized water.
4. the preparation method of nanometer bacteria cellulose whisker according to claim 1, it is characterised in that：Described in step 2
Drying temperature is 47-54 DEG C, and the time is 2~8 hours.
5. the preparation method of nanometer bacteria cellulose whisker according to claim 1, it is characterised in that：Described in step 3
Acid solution is one or more of sulfuric acid, hydrochloric acid, nitric acid, acetic acid and ethanedioic acid；And the mass concentration of each acid solution is all
It is 50%~65%.
6. the preparation method of nanometer bacteria cellulose whisker according to claim 1, it is characterised in that：Described in step 4
Constant temperature whipping temp is 45~60 DEG C, and the time is 2~8h.
7. the preparation method of nanometer bacteria cellulose whisker according to claim 1, it is characterised in that：Surpass described in step 5
The time of sound assisted reaction is 2~8h.
8. the preparation method of nanometer bacteria cellulose whisker according to claim 1, it is characterised in that：Bacterium in step 3
Cellulose is put into according to the ratio of 0.01-0.05g/mL in acid solution.
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Cited By (1)
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| CN106620832A (en) * | 2016-12-27 | 2017-05-10 | 华中科技大学 | Transparent antibacterial hydrogel dressing as well as preparation method and application thereof |
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| CN103102547A (en) * | 2013-01-28 | 2013-05-15 | 南京理工大学 | XNBR (Carboxy Terminated Nitrile Rubber) vulcanized rubber containing bacterial cellulose whisker and preparation method of XNBR vulcanized rubber |
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| CN103102547A (en) * | 2013-01-28 | 2013-05-15 | 南京理工大学 | XNBR (Carboxy Terminated Nitrile Rubber) vulcanized rubber containing bacterial cellulose whisker and preparation method of XNBR vulcanized rubber |
| CN103665439A (en) * | 2013-11-22 | 2014-03-26 | 东华大学 | Stimuli-responsive composite material made from bacterial nano cellulose as well as preparation method and application of stimuli-responsive composite material |
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Application publication date: 20181012 |
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