CN106065081B - The preparation method and products obtained therefrom of a kind of high-dispersion nano cellulose gum and application - Google Patents
The preparation method and products obtained therefrom of a kind of high-dispersion nano cellulose gum and application Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of high-dispersion nano cellulose gum and products obtained therefrom and application, step to be:By coconut palm fruit ultramicro grinding at paste, washed with impurities obtain the nanometer bacteria cellulose lotion tentatively to clean;The dispersion cleaner with hydroxyl radical free radical is added into the nanometer bacteria cellulose lotion after preliminary removal of impurities to be handled, washed with impurities again after processing;It is 0.5% 10% that nanometer bacteria cellulose lotion after cleaning again, which is dehydrated to nanometer bacteria cellulose content, and secure satisfactory grades scattered nano-cellulose glue.The method of the present invention is simple, at low cost, environmentally protective, gained high-dispersion nano bacteria cellulose glue good dispersion, high-performance modified dose of coating, rubber, sponge, food, medical material etc. be can be used as to improve product structure and improve product physicochemical property, there should be range in industrial aspect to expand nanometer bacteria cellulose, the added value for improving coconut palm fruit may advantageously facilitate China's coconut palm fruit processing and its development of related industry.
Description
Technical field
The present invention relates to a kind of preparation method of high-dispersion nano cellulose gum and products obtained therefrom and applications, and in particular to one
Method and products obtained therefrom and the application of high-dispersion nano cellulose gum kind are prepared using coconut palm fruit or compressed coconut as raw material.
Background technology
Coconut palm fruit(nata)It is a kind of nanometer bacteria cellulose with unique gel structure made of being fermented by acetobacter xylinum.
Nanometer bacteria cellulose (nano bacterial cellulose) is connected by the microfibril of diameter 1.78nm, by hydrogen bond
At a diameter of 3-4nm microfibril bundle then the nanofiber of the certain length being further formed mutually is wound by microfibril bundle
Silk ribbon, thickness are generally 3-8nm, are interweaved between filament band, form three-dimensional netted porous structure.Due to nanometer bacteria
Cellulose have excellent molecularly oriented, significant stability, excellent mechanical performance and higher crystallinity and by
Extensive concern, nanometer bacteria cellulose and its derivative are in fields such as papermaking, weaving, food, coating, filter membrane and medical materials
It is used widely.
By the dispersion of three-dimensional netted porous structure, the dissociation of coconut palm fruit, unordered nanometer bacteria cellulose staple fiber is become
It is the committed step that the high molecular materials such as itself and plant fiber, natural rubber, polyvinyl alcohol prepare composite material, and nanometer bacteria
The degree of scatter of cellulose and the stability of dispersion are directly influenced and are efficiently used to nanometer bacteria cellulose.If nanometer
Bacteria cellulose dispersion is bad, and hydrogen bond association will occur for the hydroxyl on cellulose molecular chain to be encapsulated in fibre bundle
Portion, this will influence the Hydrogenbond between cellulose and composite material, and its bad coacervation that also results in of dispersion is serious,
To the combination of obstruction and composite material, the physicochemical property of composite material is reduced.At present for the dispersion of nanometer bacteria cellulose
Mainly using the methods of soda acid processing dispersion, ultrasonic disperse, mechanical homogenisation dispersion.Soda acid processing dispersion reduces nanometer bacteria fibre
The crystallinity of element is tieed up, and generates a large amount of pollution;Nanometer bacteria cellulose prepared by ultrasonic disperse, mechanical homogenisation dispersion is for a long time
Placement still suffers from precipitation, suspension phenomenon, and ultrasonic disperse, mechanical homogenisation cannot remove the impurity such as albumen, fat, thalline,
The nanometer bacteria cellulose of gained is placed have peculiar smell for a long time, its application is influenced.In addition, through fully dispersed nanometer bacteria fiber
With higher surface energy, it is easy to happen wadding in aqueous medium and gathers, bacterial fibers dispersion stable is influenced, to limit nanometer
Extensive use of the bacteria cellulose in industrial aspect.
Invention content
The object of the present invention is to provide a kind of preparation method of high-dispersion nano cellulose gum and gained high-dispersion nano are fine
The plain glue of dimension, this method is simple for process, at low cost, environmentally protective, and gained nano-cellulose glue is added to the water can rapid dispersion Cheng Jun
Even nano-cellulose lotion, dispersibility is high, can be used as paper, coating, rubber, sponge, food, medical material, textile etc.
High-performance modified dose, improve product structure, improve product physicochemical property, expanded the application range of nanometer bacteria cellulose,
The added value for improving coconut palm fruit may advantageously facilitate China's coconut palm fruit processing and its development of related industry.
It is a further object of the present invention to provide the high-dispersion nano cellulose gums as paper, coating, rubber, sponge, food
The application of the modifying agent of product, medical material, textile etc..
Specific technical solution of the present invention is as follows:
A kind of preparation method of high-dispersion nano cellulose gum, includes the following steps:
(1)By coconut palm fruit ultramicro grinding at paste, nanometer bacteria cellulose lotion is obtained;
(2)Nanometer bacteria cellulose lotion is put into filter device, adds and is washed to neutrality, completes preliminary removal of impurities;
(3)Be added into the nanometer bacteria cellulose lotion after preliminary removal of impurities the dispersion cleaner with hydroxyl radical free radical into
Row processing, places into filter device after processing, adds and be washed to neutrality, and completion cleans again;
(4)It is 0.5%- that nanometer bacteria cellulose lotion after cleaning again, which is dehydrated to nanometer bacteria cellulose content,
10%, secure satisfactory grades scattered nano-cellulose glue.
The present invention obtains the nano-cellulose glue of good dispersion using coconut palm fruit as raw material, by the operations such as crushing, disperseing.It is above-mentioned
Step(1)In, coconut palm fruit is first crushed to granularity≤300 μm, coconut palm fruit in the pasty state, is removed convenient for subsequent dispersion in the particle size range
Reason is lived together, so that nanometer bacteria cellulose is preferably disperseed, is dissociated into nano short fiber.Coconut palm fruit used is fresh coconut palm fruit or compression
Coconut palm fruit, nanometer bacteria cellulose content about 0.5%-5% therein.Coconut palm fruit is crushed to using grinding devices such as liquid micronizers
Designated size needs to carry out washed with impurities, the impurity on its surface is removed before coconut palm fruit crushes.Coconut palm is compressed when using
When fruit, it is also necessary to which it is first carried out rehydration, then washed with impurities.
Above-mentioned steps(1)In, when coconut palm fruit addition grinding device crushes, it is preferably first cut into strip or square shape, in this way
More conducively crush.
The above method carries out washed with impurities twice, is for the first time step(2), second is step(3), cleaning twice is
Impurity is removed from bacteria cellulose lotion by way of washing, impurity enters with dampening in filtrate, completes removal of impurities.Removal of impurities
Filter device used preferably uses filter cloth formula filter device, filter cloth used to be preferably made of multi-layer fiber material, remove in this way
Miscellaneous effect is more preferable, is also avoided that the loss of nanometer bacteria cellulose.
Further, step(2)It filters in the filtrate of gained and contains impurity, direct emission pollutes the environment, preferably
By step(2)With(3)The filtrate mixing that filtering generates, utilizes step(3)In hydroxyl radical free radical to step(2)It is miscellaneous in filtrate
Matter carries out oxidative degradation processing, and waste liquid makes full use of, more conducively environmentally friendly.
Above-mentioned steps(3)In, dispersion cleaner carries hydroxyl radical free radical, has the function of oxidation, degradation of organic substances, can drop
Hydrogen bond activity between low bacteria cellulose fibre, in fiber surface generating portion carboxyl, the hydrophily of increased fiber, to improve
The stability of its dispersibility and dispersion in water, while disperseing cleaner can be miscellaneous by organic matters such as albumen, fat on fiber
Matter degradation removes, and improves the purity of product, avoids peculiar smell harmful effect caused by application of these organic impurities.Dispersion
After removal of impurities, nanometer bacteria cellulose lotion is subjected to washed with impurities, the organic impurities and dispersion cleaner of degradation are washed away, into one
Step improves product purity.
Further, the dispersion cleaner is hydrogen peroxide or ozone.The dosage of hydrogen peroxide or ozone in hydrogen peroxide
For the 0.5%-10% of nanometer bacteria cellulose quality of the emulsion.
Further, disperseing the mode that cleaner is handled is:Nanometer bacteria cellulose lotion to after preliminary removal of impurities
Middle addition disperses cleaner, handles 3h~5d at room temperature(It), nanometer bacteria cellulose lotion color presentation milky.
Further, dispersion cleaner is preferably alkaline hydrogen peroxide, and the alkaline hydrogen peroxide is the hydrogen peroxide that pH is alkalinity.
When it is alkaline hydrogen peroxide to disperse cleaner, processing time can be reduced significantly, handling 3h at room temperature can meet the requirements, and
Processing time when using neutral hydrogen peroxide and ozone needs 1-5d.Alkaline hydrogen peroxide may be used into hydrogen peroxide plus alkali is adjusted
The mode of pH obtains.
Above-mentioned steps(4)In, the concentration of nanometer bacteria cellulose is controlled in 0.5-10% by way of dehydration, such as
1-10%、2-10%、3-10%、5-10%、7-10%.Concentration is lower, is more conducive to dispersion, but can increase transportation cost, concentration mistake
Height, product dispersion is bad, influences to apply.Within this range, nanometer bacteria cellulose purity is not only increased, it is increased and contains
Amount, alleviates transportation cost, the nanometer bacteria cellulose in product also can be quickly distributed in water, and will not wad a quilt with cotton poly-, granulating.
Further, can also include by step for the ease of transporting and storing(4)High dispersive bacteria cellulose obtained
The step of being packed after glue high-temperature sterilization.The product handled in this way can be readily transported, be stored up with direct marketing, shelf-life limit for length
It deposits and uses.
Further, high-temperature sterilization is carried out at 105-120 DEG C.
High-dispersion nano cellulose gum obtained by according to the method described above is also within the scope of the present invention.The product is white
Color, nanometer bacteria cellulose content are 0.5-10%, and other compositions are mainly water.Products obtained therefrom good dispersion of the present invention, is using
When, add water stirring power rapid dispersion to form nanometer bacteria cellulose lotion, uniform and stable, no poly- phenomenon of wadding.Because of its polymolecularity
Good stability in water, the high-dispersion nano cellulose gum can be used as paper, sponge, food, medical material, rubber
The modifying agent of glue, textile etc. has widened the application of bacteria cellulose.
The present invention first crushes to obtain paste nanometer bacteria cellulose breast using fresh coconut palm fruit or compressed coconut as raw material
It liquid and then is handled with the dispersion cleaner with hydroxyl radical free radical after preliminary removal of impurities, nanometer bacteria cellulose is carried out
Processing, carries out washed with impurities, is then dehydrated to nanometer bacteria cellulose to a certain concentration, secure satisfactory grades scattered Nanowire again after processing
The plain glue of dimension.This method is simple for process, at low cost, environmentally protective, and gained nano-cellulose glue impurity is few, nanometer bacteria cellulose divides
Scattered property is good, stability is high, can do the modifying agent of paper, sponge, food, medical material, rubber and textile etc., improves product knot
Structure improves product physicochemical property, has expanded nanometer bacteria cellulose in the application range of industrial aspect, has improved the additional of coconut palm fruit
Value may advantageously facilitate China's coconut palm fruit processing and its development of related industry.
Description of the drawings
Fig. 1 is high-dispersion nano cellulose gum preparation technology flow chart of the present invention.
Fig. 2 is high-dispersion nano cellulose gum product of the present invention.
Fig. 3 is the design sketch that high-dispersion nano cellulose gum of the present invention disperses in water.
Specific implementation mode
Below by specific embodiment, invention is further explained, and following the description is merely exemplary, not right
Its content is defined.
Embodiment 1
1, raw material:Compressed coconut chankings is taken, adds tap water rehydration, washing, remove coconut palm fruit surface irregularities, obtain nano-cellulose
The coconut palm fruit chankings of content about 1%.
2, cutting and grinding:Into strips using cutting machine cutting, it is added in liquid micronizer and is ground into paste, obtain
The nanometer bacteria cellulose lotion that about 10 μm of material size.
3, it filters:Nanometer bacteria cellulose lotion is transferred in multi-layer fiber filter-cloth filtering device, using originally washing
It washs to neutrality, completes preliminary removal of impurities.
4, dispersion removal of impurities:The nanometer bacteria cellulose lotion tentatively to clean is transferred in dispersion removal of impurities processing pond, is added
Hydrogen peroxide is to H2O2Content is the 0.5% of nanometer bacteria cellulose quality of the emulsion, and room temperature handles 3d.
5 filterings:Will dispersion removal of impurities treated that nanometer bacteria cellulose lotion is transferred to multi-layer fiber filter-cloth filtering device
In, add tap water filter to wash away hydrogen peroxide and other impurities, and clean again using 3 extremely neutrality, completions of pure water.Dehydration
It is 2% to nanometer bacteria cellulose content, obtains white high-dispersion nano cellulose gum.This step gained filtrate and the filtrate in step 3
Mixing is transferred in treatment tank, utilizes unreacted hydrogen peroxide oxidation treated sewage.
6 packagings:By nano-cellulose glue in 105 DEG C of high-temperature sterilizations, pack content be 2% nanometer bacteria cellulose
High-dispersion nano cellulose gum finished product, as shown in Figure 2.The finished product is added to the water stirring, nano-cellulose glue can quickly
Even is dispersed in water, and no poly- phenomenon of wadding is shown in Fig. 3.
Embodiment 2
1, raw material:It takes fresh coconut palm fruit originally water washing, remove coconut palm fruit surface irregularities, obtain coconut palm fruit chankings.
2, cutting and grinding:Coconut palm fruit chankings is cut into strips using cutting machine, is added in liquid micronizer and crushes
At paste, the nanometer bacteria cellulose lotion of about 50 μm of material size is obtained.
3, it filters:Nanometer bacteria cellulose lotion is transferred in multi-layer fiber filter-cloth filtering device, using originally washing
It washs to neutrality, completes preliminary removal of impurities.
4, dispersion removal of impurities:The nanometer bacteria cellulose lotion tentatively to clean is transferred in dispersion removal of impurities processing pond, interval
It is passed through ozone, it is the 0.5% of nanometer bacteria cellulose quality to make the dosage of ozone, and room temperature is handled 1 day.
5 filterings:Nanometer bacteria cellulose lotion after dispersion is cleaned is transferred in multi-layer fiber filter-cloth filtering device, is added
Tap water filter removes ozone and other impurities, reuses pure water 3 times to neutrality, completion cleans again.It is dehydrated to nanometer
Bacterial fibers cellulose content is 3%, obtains white high-dispersion nano cellulose gum.This step gained filtrate mixes with the filtrate in step 3 to be turned
It moves on to and utilizes unreacted ozone Oxidation Treatment sewage in treatment tank.
6 packagings:By nano-cellulose glue in 110 DEG C of high-temperature sterilizations, pack nanometer bacteria cellulose content be 3%
High-dispersion nano cellulose gum finished product.The finished product is added to the water stirring, nano-cellulose glue can be rapidly and uniformly dispersed in
In water, no poly- phenomenon of wadding.
Embodiment 3
1, raw material:Compressed coconut chankings is taken, adds tap water rehydration, washing, remove coconut palm fruit surface irregularities, obtain nanometer bacteria fibre
Tie up the coconut palm fruit chankings of cellulose content about 2%.
2, cutting and grinding:Using the cutting machine side of cutting into shape, it is added in liquid micronizer and is ground into paste, obtain object
The nanometer bacteria cellulose lotion that about 100 μm of material granularity.
3, it filters:Paste nanometer bacteria cellulose lotion is transferred in multi-layer fiber filter-cloth filtering device, using originally
Water washing completes preliminary removal of impurities to neutrality.
4, dispersion removal of impurities:The nanometer bacteria cellulose lotion tentatively to clean is transferred to dispersion removal of impurities processing pond, is added double
Oxygen water is to H2O2Content is the 4% of nanometer bacteria cellulose quality of the emulsion, and room temperature handles 2d.
5 filterings:Will dispersion removal of impurities treated that nanometer bacteria cellulose lotion is transferred to multi-layer fiber filter-cloth filtering device
In, add tap water filter to remove hydrogen peroxide and other impurities, reuses pure water 3 times to neutrality, completion cleans again.Dehydration
It is 7% to nanometer bacteria cellulose content, obtains white high-dispersion nano cellulose gum.This step filtrate is mixed with the filtrate in step 3
Conjunction is transferred in treatment tank, utilizes unreacted hydrogen peroxide oxidation treated sewage.
6 packagings:By nano-cellulose glue in 115 DEG C of high-temperature sterilizations, pack nanometer bacteria cellulose content be 4%
High-dispersion nano cellulose gum finished product.The finished product is added to the water stirring, nano-cellulose glue can be rapidly and uniformly dispersed in
In water, no poly- phenomenon of wadding.
Embodiment 4
1, raw material:Compressed coconut chankings is taken, adds tap water rehydration, washing, remove coconut palm fruit surface irregularities, obtain nano-cellulose
The coconut palm fruit chankings of content about 3%.
2, cutting and grinding:Using the cutting machine side of cutting into shape, it is added in liquid micronizer and is ground into paste, obtain object
The nanometer bacteria cellulose lotion that about 200 μm of material granularity.
3, it filters:Paste nano-cellulose lotion is transferred in multi-layer fiber filter-cloth filtering device, using originally washing
It washs to neutrality.
4, dispersion removal of impurities:Nanometer bacteria cellulose lotion is transferred to dispersion removal of impurities processing pond, the alkalinity that pH=10 are added is double
Oxygen water adjusts H2O2Content is the 1% of nanometer bacteria cellulose quality of the emulsion, and room temperature handles 3h.
5 filterings:Will dispersion removal of impurities treated that nanometer bacteria cellulose lotion is transferred to multi-layer fiber filter-cloth filtering device
In, add tap water filter to remove hydrogen peroxide and other impurities, reuses pure water 3 times to neutrality, completion cleans again.Dehydration
It is 5% to nanometer bacteria cellulose content, obtains white nano-cellulose glue.This step filtrate is mixed into transfer with the filtrate in step 3
Into treatment tank, unreacted hydrogen peroxide oxidation treated sewage is utilized.
6 packagings:By nano-cellulose glue in 120 DEG C of high-temperature sterilizations, pack content be 5% nanometer bacteria cellulose
High-dispersion nano cellulose gum finished product.The finished product is added to the water stirring, nano-cellulose glue can be rapidly and uniformly dispersed in
In water, no poly- phenomenon of wadding.
Embodiment 5
1, raw material:Compressed coconut chankings is taken, adds tap water rehydration, washing, remove coconut palm fruit surface irregularities, obtain nano-cellulose
The coconut palm fruit chankings of content about 2%.
2, cutting and grinding:Using the cutting machine side of cutting into shape, it is added in liquid micronizer and is ground into paste, obtain object
The nanometer bacteria cellulose lotion that about 10 μm of material granularity.
3, it filters:Paste nano-cellulose lotion is transferred in multi-layer fiber filter-cloth filtering device, using originally washing
It washs to neutrality.
4, dispersion removal of impurities:Nanometer bacteria cellulose lotion is transferred to dispersion removal of impurities processing pond, pH is added>9 alkalinity is double
Oxygen water adjusts H2O2Content is the 10% of nanometer bacteria cellulose quality of the emulsion, and room temperature handles 3h.
5 filterings:Will dispersion removal of impurities treated that nanometer bacteria cellulose lotion is transferred to multi-layer fiber filter-cloth filtering device
In, add tap water filter to remove hydrogen peroxide and other impurities, reuse pure water 3 times, completion cleans again.It is dehydrated to nanometer
Bacterial fibers cellulose content is 10%, obtains white nanometer bacteria cellulose glue.This step filtrate is mixed into transfer with the filtrate in step 3
Into treatment tank, unreacted hydrogen peroxide oxidation treated sewage is utilized.
6 packagings:By nano-cellulose glue in 115 DEG C of high-temperature sterilizations, pack content be 10% nanometer bacteria cellulose
High-dispersion nano cellulose gum finished product.The finished product is added to the water stirring, nano-cellulose glue can be rapidly and uniformly dispersed in
In water, no poly- phenomenon of wadding.
Comparative example 1
Nanometer bacteria cellulose glue finished product is prepared according to the method for embodiment 1, unlike:Coconut palm fruit is crushed in step 2
To about 500 μm of granularity.
Comparative example 2
Nanometer bacteria cellulose glue finished product is prepared according to the method for embodiment 1, unlike:Step 4 dispersion removal of impurities according to
Following manner carries out:The nanometer bacteria cellulose lotion tentatively to clean is transferred in dispersion removal of impurities processing pond, pH=5 are added
To its content is nanometer bacteria cellulose quality of the emulsion 2%, room temperature is handled 3 days ammonium persulfate.
Comparative example 3
Nanometer bacteria cellulose glue finished product is prepared according to the method for embodiment 1, unlike:It is dehydrated to nanometer in step 5
Bacterial fibers cellulose content is packed again for 20%.
In order to verify the performance of products obtained therefrom, following experiment is carried out:
Above-described embodiment and comparative example resulting product 100g are taken, is added separately in 500ml water, according to identical stirring
Speed quickly stirs, until product is evenly dispersed at lotion in water, the record product evenly dispersed required time stands two days later
Dispersity and smell variation, as a result as shown in table 1 below.
Claims (12)
1. a kind of preparation method of high-dispersion nano cellulose gum, it is characterized in that including the following steps:
(1)By coconut palm fruit ultramicro grinding at paste, nanometer bacteria cellulose lotion is obtained;
(2)Nanometer bacteria cellulose lotion is put into filter device, adds and is washed to neutrality, completes preliminary removal of impurities;
(3)It is added at the dispersion cleaner with hydroxyl radical free radical into the nanometer bacteria cellulose lotion after preliminary removal of impurities
Reason, places into filter device after processing, adds and be washed to neutrality, and completion cleans again;
(4)It is 0.5%-10% that nanometer bacteria cellulose lotion after cleaning again, which is dehydrated to nanometer bacteria cellulose content, is obtained
High-dispersion nano cellulose gum.
2. preparation method according to claim 1, it is characterized in that:Step(1)In, coconut palm fruit is crushed to granularity≤300 μm.
3. preparation method according to claim 1, it is characterized in that:Step(3)In, the dispersion cleaner be hydrogen peroxide or
Ozone.
4. preparation method according to claim 3, it is characterized in that:Step(3)In, the dispersion cleaner is alkaline dioxygen
Water, the alkaline hydrogen peroxide are the hydrogen peroxide that pH is alkalinity.
5. preparation method according to claim 3, it is characterized in that:Step(3)In, the hydrogen peroxide in hydrogen peroxide or ozone
Dosage be nanometer bacteria cellulose quality of the emulsion 0.5%-10%;After dispersion cleaner is added, 3h~5d is handled at room temperature.
6. preparation method according to claim 1, it is characterized in that:Step(1)In, powder is carried out using liquid micronizer
It is broken;Step(2)With(3)In, it is filtered using filter-cloth filtering device.
7. preparation method according to claim 6, it is characterized in that:The filter cloth is made of multi-layer fiber material.
8. preparation method according to claim 1, it is characterized in that:By step(2)With(3)The filter that middle filtering, washing generate
Liquid mixes, using undecomposed dispersion cleaner to step(2)Filtrate carry out oxidative degradation processing.
9. according to the preparation method described in any one of claim 1-8, it is characterized in that:In order to extend high-dispersion nano cellulose
The service life of glue further includes the steps that packing high dispersive cellulose gum high-temperature sterilization.
10. preparation method according to claim 9, it is characterized in that:High-temperature sterilization temperature is 105-120 DEG C.
11. high dispersive made from the preparation method according to the high-dispersion nano cellulose gum described in any one of claim 1-10
Nano-cellulose glue.
12. the high-dispersion nano cellulose gum described in claim 11 is as paper, sponge, food, medical material, rubber or spinning
The application of fabric modifying agent.
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