CN106638087B - A kind of natural high-crystallinity plant cellulose and preparation method thereof - Google Patents
A kind of natural high-crystallinity plant cellulose and preparation method thereof Download PDFInfo
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- CN106638087B CN106638087B CN201611100734.2A CN201611100734A CN106638087B CN 106638087 B CN106638087 B CN 106638087B CN 201611100734 A CN201611100734 A CN 201611100734A CN 106638087 B CN106638087 B CN 106638087B
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/04—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
Abstract
The invention discloses a kind of natural high-crystallinity plant cellulose and preparation method thereof, this method is one of the effective way that Efficient Development utilizes biomass algae resource.Specially by the algae raw material washes clean of acquisition, impurity, natural air drying, mechanical crushing are removed.Under acid condition, colour component is removed using hypochlorite oxidation, reaction terminates to be washed till neutrality, be separated by solid-liquid separation.Solid residue removes its protein component using alkali sodium hydroxide processing, and reaction terminates to be washed till neutrality, be separated by solid-liquid separation.Continue to use component of inorganic salts, the reactions such as the calcium salt in dilute hydrochloric acid solution unhydrolyzed solids residue to terminate, be washed till neutrality, is separated by solid-liquid separation, it is dry, purity and the higher cellulose of crystallinity is made.The present invention is extracted from natural biomass to be obtained with fine, network intertexture microstructure high-purity, high crystalline cellulose, and the exploitation for renewable high-crystallinity fibrous material provides technical support.
Description
Technical field
The present invention relates to renewable biomass sill fields, and in particular to a kind of natural high-crystallinity plant cellulose and
Preparation method.
Background technology
Natural plant fibre is usually made of crystal region and noncrystalline domain.Crystallite arrangement is close in crystal region, between each other
Binding force it is big, macroscopically performance is the high fiber in crystal region, the better performances such as wearability, intensity and rigidity.High-crystallinity
Micro-nano fiber special optical property is also shown in composite material nanometer material.In addition, the fiber surface that crystallinity is high
Great amount of hydroxy group group constitutes huge hydrogen bond network by hydrogen bond, and the hydrogen bond action combined with outside water molecule is reduced, hygroscopicity
It can be lower, thermal stability improves, and is to develop the renewable nano material of high-performance or the important source material of pharmaceutical carrier.
It is distributed widely in the green alga of freshwater lake, river or coastal shallow water area, is made of single-row cell or many cells
, multiple-limb biomass, complicated components are mainly made of protein, minerals, carbohydrate, pigment etc..Frond cell is equal
With splitting ability, but the cell at usually only top largely generates new cell, to quickly form point in great numbers in water
Subsystem destroys the ecological balance of water body environment.The advantage for how utilizing green alga quickly to breed, Efficient Development green alga base height are additional
It is worth product, it has also become the multiple national urgent problems in the whole world.Research finds that characteristic fibrous structure and high-purity are thin in frond
Fungin has more similarity, is mainly made of crystal region, therefore efficiently removes impurity composition, and it is fine to obtain high-purity green alga
Dimension element becomes the important channel that separation prepares natural high-crystallinity plant cellulose.The present invention will pass through the work of a series of complex
Skill, extraction prepare high-purity, high-crystallinity plant cellulose, for renewable fiber-based material development and utilization provide it is novel
Cellulose origin.
Invention content
The object of the present invention is to provide a kind of natural high-crystallinity plant celluloses and preparation method thereof, and this method includes algae
The techniques such as the mineral constituents such as body pigment removal, removal of protein, calcareous removal, efficiently remove impurity composition, obtain high-purity
Green alga base cellulose, the development and utilization for renewable fiber-based material provide cellulose origin.
To achieve the above object, the present invention uses following technical scheme.
A kind of preparation method of natural high-crystallinity plant cellulose, includes the following steps：
（1）Green alga is washed, impurity, natural air drying are removed, machinery is ground, and obtains green alga powder；
（2）In acid condition, the pigment in green alga powder is removed using hypochlorite oxidation, it after reaction will reaction
Liquid is washed till neutrality, then is separated by solid-liquid separation；
（3）By step（2）Separating obtained solid residue is placed in sodium hydroxide solution, and isolating protein, reaction knot are removed in reaction
Reaction solution is washed till neutrality after beam, then is separated by solid-liquid separation；
（4）Using dilute hydrochloric acid solution acidic hydrolysis step（3）The inorganic salts such as the calcium salt in obtained solid residue, hydrolysis terminate
Hydrolyzate is washed till neutrality afterwards, it is dry, obtain that purity is higher, the higher plant cellulose of crystallinity.
Preferably, step（1）The green alga comes from freshet, lake or the shallow water along the coast.
Preferably, step（1）The green alga is single-row cell or the raw green alga of many cells, specially Cladophora, water
The algae such as continuous category, Scenedesmus, Chlorella.
Preferably, step（2）The step of hypochlorite oxidation is：At 40 ~ 70 DEG C, by green alga powder, hypochlorous acid
Sodium, the NaAc_HAc buffer solution that pH is 4.0 ~ 5.0 are with solid-to-liquid ratio for 1:5~1:20 stir evenly, and react 3 ~ 6 h, described
The dosage of sodium hypochlorite is 10 ~ 40 wt% of green alga powder.
Preferably, step（2）During the sodium chlorate oxidation color of raw material by green or yellow green be bleached to
White or milky.
Preferably, step（3）In, the solid-to-liquid ratio of solid residue and sodium hydroxide solution is 1:8~1:15, the hydroxide
Sodium hydroxide in sodium solution is 10 ~ 25 wt% of solid residue quality, and the temperature of reaction is 50 ~ 70 DEG C, and the time of reaction is 3
~6 h。
Preferably, step（3）The removal degree of protein detects nitrogen by elemental analyser in the solid residue
Content calculation obtain, removal rate be more than 96 %.
Preferably, step（4）The step of acidic hydrolysis is：Into solid residue with solid-to-liquid ratio for 1:3~1:5 are added
The hydrochloric acid solution of a concentration of 3 ~ 6 wt%, it is lasting to stir, it is heated to boiling, keeps 1 ~ 5 min of boiling, remove heat source, room temperature
12 ~ 24 h of lower standing.
A kind of natural high-crystallinity plant cellulose made from above-described preparation method.
Preferably, which has fine network intertexture appearance structure（Using scanning electricity
Mirror is analyzed, this structure is conducive to develop the renewable porous fibrous material of high added value）, crystallinity is more than 92.0 %（Using X-ray
Diffraction detects）, ash value is less than 4.0 %（Using 575 DEG C of calcining detections of Muffle furnace）.
Compared with prior art, the invention has the advantages that and technique effect：
1, the present invention is extracted from natural biomass green alga obtains with fine, network intertexture microstructure high-purity
Degree, high crystalline cellulose, the exploitation for renewable high-crystallinity fibrous material provide technical support.
2, the present invention, can feedback regulation optimization using the removal efficiency of protein in accurate nitrogen analyzer analysis green alga
Green alga removal of protein technique, ensures the removal of protein component depth, and technical support is provided for efficiently separating for green alga component.
Description of the drawings
Fig. 1 is the scanning electron microscopic picture that embodiment 1 extracts isolated natural high-crystallinity plant cellulose.
Specific implementation mode
The present invention is described in further detail by the following examples, and embodiments of the present invention are not limited thereto.
Embodiment 1
The green alga for being derived from freshwater lake is cleaned, impurity, natural air drying are removed, machinery is ground, and obtains green alga powder.According to solid
Liquor ratio is 1:5（w/w）, sodium hypochlorite dosage is 10 % of green alga powder（w/w）, by green alga powder（5.0 g）, sodium hypochlorite
（0.5 g）It is placed in the NaAc_HAc buffer solution that pH is 4.0,40 DEG C of temperature is persistently stirred to react 3 h.Reaction terminates,
Green alga powder becomes milky from green, and washing to neutrality is separated by solid-liquid separation.Separating obtained solid residue is further arranged in hydrogen-oxygen
Change deproteination matter in sodium solution, solid-to-liquid ratio 1:8（w/w）, sodium hydroxide concentration is 10 % of solid residue（w/w）, temperature
50 DEG C, persistently it is stirred to react 4 h.Reaction solution is washed to neutrality after reaction, is separated by solid-liquid separation.Elemental analyser detects albumen
Nitrogen element content before and after matter elimination reaction, the removal efficiency that protein is calculated are 96.1%.Dilute hydrochloric acid hydrolysis removing egg is used again
The mineral components such as calcareous after white matter in separating obtained solid residue, are further purified.A concentration of 3 wt% of dilute hydrochloric acid, Gu
Liquor ratio is 1:3（w/w）, it is lasting to stir, it is heated to boiling, keeps 1 min of boiling, remove heat source, stand 12 h at room temperature.
Reaction solution is washed to neutrality after reaction, is separated by solid-liquid separation, drying solid obtains natural high-crystallinity plant cellulose.It adopts
With 575 DEG C of natural high-crystallinity plant celluloses of calcining of Muffle furnace, ash content is 0.8 %.X-ray diffraction analysis detaches cellulose
Crystallinity shows to obtain natural high-crystallinity plant cellulose, and crystallinity is 92.0 %.
The present embodiment extract the scanning electron microscopic picture of isolated natural high-crystallinity plant cellulose as shown in Figure 1,
Show that this cellulose has the microstructure being interweaved, is suitable for renewable porous material.Fiber obtained by other embodiments
The scanning electron microscopic picture of element is similar with Fig. 1, all has the microstructure being interweaved.
Embodiment 2
The green alga raw material for being derived from river is cleaned, impurity, natural air drying are removed, machinery is ground, and obtains green alga powder.According to solid
Liquor ratio is 1:10（w/w）, sodium hypochlorite dosage is 20 % of green alga powder（w/w）, by green alga powder（4.0 g）, sodium hypochlorite
（0.8 g）It is placed in the NaAc_HAc buffer solution that pH is 4.5,55 DEG C of temperature is persistently stirred to react 4.5 h.Reaction knot
Beam, green alga powder become milky from green, and washing to neutrality is separated by solid-liquid separation.Separating obtained solid residue is further arranged in
Deproteination matter in sodium hydroxide solution, solid-to-liquid ratio 1:10（w/w）, sodium hydroxide concentration is 25 % of solid residue（w/w）,
Temperature 70 C is persistently stirred to react 6 h.Reaction solution is washed to neutrality after reaction, is separated by solid-liquid separation.Elemental analyser detects
The front and back nitrogen element content of removal of protein reaction, the removal efficiency that protein is calculated are 98.2 %.Dilute hydrochloric acid is used to hydrolyze again
The mineral components such as calcareous after deproteination matter in separating obtained solid residue, are further purified.Dilute hydrochloric acid a concentration of 6
Wt%, solid-to-liquid ratio 1:5（w/w）, it is lasting to stir, it is heated to boiling, keeps 5 min of boiling, remove heat source, it is quiet at room temperature
Set 24 h.Reaction solution is washed to neutrality after reaction, is separated by solid-liquid separation, drying solid, it is fine to obtain natural high-crystallinity plant
Dimension element.The natural high-crystallinity plant cellulose produced is calcined for 575 DEG C using Muffle furnace, ash content is 0.4 %.X-ray diffraction point
The crystallinity of analysis separation cellulose shows to obtain natural high-crystallinity plant cellulose, and crystallinity is 96.0 %.
Embodiment 3
The green alga raw material for being derived from the shallow water along the coast is cleaned, impurity, natural air drying are removed, machinery is ground, and obtains green alga powder.It presses
It is 1 according to solid-to-liquid ratio:20（w/w）, sodium hypochlorite dosage is 40 % of green alga powder（w/w）, by green alga powder（5.0 g）, secondary chlorine
Sour sodium（2.0 g）It is placed in the NaAc_HAc buffer solution that pH is 5.0, temperature 70 C is persistently stirred to react 6 h.Reaction knot
Beam, green alga powder become milky from yellow green, and washing to neutrality is separated by solid-liquid separation.Separating obtained solid residue is further set
The deproteination matter in sodium hydroxide solution, solid-to-liquid ratio 1:12（w/w）, sodium hydroxide concentration is 15 % of solid residue（w/
w）, temperature 60 C is persistently stirred to react 5 h.Reaction solution is washed to neutrality after reaction, is separated by solid-liquid separation.Elemental analyser
The front and back nitrogen element content of removal of protein reaction is detected, the removal efficiency that protein is calculated is 97.0 %.Dilute hydrochloric acid is used again
The mineral components such as calcareous in separating obtained solid residue are hydrolyzed after deproteination matter, are further purified.Dilute hydrochloric acid a concentration of 4
Wt%, solid-to-liquid ratio 1:4（w/w）, it is lasting to stir, it is heated to boiling, keeps 3 min of boiling, remove heat source, it is quiet at room temperature
Set 12 h.Reaction solution is washed to neutrality after reaction, is separated by solid-liquid separation, drying solid, it is fine to obtain natural high-crystallinity plant
Dimension element.The natural high-crystallinity plant cellulose produced is calcined for 575 DEG C using Muffle furnace, ash content is 0.65 %.X-ray diffraction point
The crystallinity of analysis separation cellulose shows to obtain natural high-crystallinity plant cellulose, and crystallinity is 93.5 %.
Embodiment 4
The green alga raw material for being derived from freshwater lake is cleaned, impurity, natural air drying are removed, machinery is ground, and obtains green alga powder.It presses
It is 1 according to solid-to-liquid ratio:15（w/w）, sodium hypochlorite dosage is 30 % of green alga powder（w/w）, by green alga powder（5.0 g）, secondary chlorine
Sour sodium（1.5 g）It is placed in the NaAc_HAc buffer solution that pH is 4.8, temperature 50 C is persistently stirred to react 4 h.Reaction knot
Beam, green alga powder become milky from yellow green, and washing to neutrality is separated by solid-liquid separation.Separating obtained solid residue is further set
The deproteination matter in sodium hydroxide solution, solid-to-liquid ratio 1:12（w/w）, sodium hydroxide concentration is 20 % of solid residue（w/
w）, temperature 60 C is persistently stirred to react 4 h.Reaction solution is washed to neutrality after reaction, is separated by solid-liquid separation.Elemental analyser
The front and back nitrogen element content of removal of protein reaction is detected, the removal efficiency that protein is calculated is 97.5 %.Dilute hydrochloric acid is used again
The mineral components such as calcareous in separating obtained solid residue are hydrolyzed after deproteination matter, are further purified.Dilute hydrochloric acid a concentration of 4
Wt%, solid-to-liquid ratio 1:4（w/w）, it is lasting to stir, it is heated to boiling, keeps 3 min of boiling, remove heat source, it is quiet at room temperature
Set 24 h.Reaction solution is washed to neutrality after reaction, is separated by solid-liquid separation, drying solid, it is fine to obtain natural high-crystallinity plant
Dimension element.The natural high-crystallinity plant cellulose produced is calcined for 575 DEG C using Muffle furnace, ash content is 0.6 %.X-ray diffraction point
The crystallinity for analysing cellulose shows to obtain natural high-crystallinity plant cellulose, and crystallinity is 95.0%.
Embodiment 5
The green alga raw material for being derived from river is cleaned, impurity, natural air drying are removed, machinery is ground, and obtains green alga powder.According to solid
Liquor ratio is 1:15（w/w）, sodium hypochlorite dosage is 30 % of green alga powder（w/w）, by green alga powder（4.5 g）, sodium hypochlorite
（1.35 g）It is placed in the NaAc_HAc buffer solution that pH is 4.8, temperature 60 C is persistently stirred to react 6 h.Reaction terminates,
Green alga powder becomes milky from green, and washing to neutrality is separated by solid-liquid separation.Separating obtained solid residue is further arranged in hydrogen-oxygen
Change deproteination matter in sodium solution, solid-to-liquid ratio 1:10（w/w）, sodium hydroxide concentration is 15 % of solid residue（w/w）, temperature
60 DEG C, persistently it is stirred to react 6 h.Reaction solution is washed to neutrality after reaction, is separated by solid-liquid separation.Elemental analyser detects albumen
Nitrogen element content before and after matter elimination reaction, the removal efficiency that protein is calculated are 97.3 %.Dilute hydrochloric acid hydrolysis removing is used again
The mineral components such as calcareous after protein in separating obtained solid residue, are further purified.A concentration of 5 wt% of dilute hydrochloric acid, Gu
Liquor ratio is 1:5（w/w）, it is lasting to stir, it is heated to boiling, keeps 4 min of boiling, remove heat source, stand 18 h at room temperature.
Reaction solution is washed to neutrality after reaction, is separated by solid-liquid separation, drying solid obtains natural high-crystallinity plant cellulose.It adopts
The natural high-crystallinity plant cellulose produced is calcined with Muffle furnace for 575 DEG C, and ash content is 0.55 %.X-ray diffraction analysis fiber
The crystallinity of element shows to obtain natural high-crystallinity plant cellulose, and crystallinity is 92.5 %.
Listed above is only specific embodiments of the present invention.Present invention is not limited to the above embodiments, can also there are many
Deformation.All deformations that those skilled in the art directly can export or associate from present disclosure, should all
It is considered protection scope of the present invention.
Claims (9)
1. a kind of preparation method of natural high-crystallinity plant cellulose, which is characterized in that include the following steps：
（1）Green alga is washed, impurity is removed, natural air drying is ground, and obtains green alga powder；The green alga is Cladophora, water silk floss
One or more of category, Scenedesmus and Chlorella；
（2）In acid condition, the pigment in green alga powder is removed using hypochlorite oxidation, after reaction washes reaction solution
To neutrality, then it is separated by solid-liquid separation；
（3）By step（2）Separating obtained solid residue is placed in sodium hydroxide solution, and isolating protein is removed in reaction, after reaction
Reaction solution is washed till neutrality, then is separated by solid-liquid separation；
（4）Using dilute hydrochloric acid solution acidic hydrolysis step（3）Inorganic salts in obtained solid residue, by hydrolyzate after hydrolysis
It is washed till neutrality, is separated by solid-liquid separation, it is dry, obtain natural high-crystallinity plant cellulose.
2. a kind of preparation method of natural high-crystallinity plant cellulose according to claim 1, which is characterized in that step
（1）The green alga comes from freshet, lake or the shallow water along the coast.
3. a kind of preparation method of natural high-crystallinity plant cellulose according to claim 1, which is characterized in that step
（2）The step of hypochlorite oxidation is：At 40 ~ 70 DEG C, by green alga powder, sodium hypochlorite, the vinegar that pH is 4.0 ~ 5.0
Acid-sodium acetate buffer is with solid-to-liquid ratio for 1:5~1:20 are mixed evenly, and react 3 ~ 6 h, and the sodium hypochlorite is green alga
10 ~ 40 wt% of powder.
4. a kind of preparation method of natural high-crystallinity plant cellulose according to claim 1, which is characterized in that step
（2）The color of raw material is bleached by green or yellow green to white or milky during the sodium chlorate oxidation.
5. a kind of preparation method of natural high-crystallinity plant cellulose according to claim 1, which is characterized in that step
（3）In, the solid-to-liquid ratio of solid residue and sodium hydroxide solution is 1:8~1:15, the sodium hydroxide in the sodium hydroxide solution is
The temperature of 10 ~ 25 wt% of solid residue quality, reaction are 50 ~ 70 DEG C, and the time of reaction is 3 ~ 6 h.
6. a kind of preparation method of natural high-crystallinity plant cellulose according to claim 1, which is characterized in that step
（3）The removal degree of protein is obtained by the content calculation of elemental analyser detection nitrogen in the solid residue, is removed
Rate is more than 96 %.
7. a kind of preparation method of natural high-crystallinity plant cellulose according to claim 1, which is characterized in that step
（4）The step of acidic hydrolysis is：Into solid residue with solid-to-liquid ratio for 1:3~1:5 are added the hydrochloric acid of a concentration of 3 ~ 6 wt%
Solution, stirring, is heated to boiling, and keeps 1 ~ 5 min of boiling, removes heat source, stands 12 ~ 24 h at room temperature.
8. a kind of natural high-crystallinity plant cellulose made from claim 1-7 any one of them preparation methods.
9. a kind of natural high-crystallinity plant cellulose according to claim 8, which is characterized in that the natural high-crystallinity
There is plant cellulose network intertexture appearance structure, crystallinity to be more than 92.0 %, and ash value is less than 4.0 %.
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| DE102019001184B4 (en) | 2019-02-18 | 2023-06-22 | Soumeya Nadir | Process for the production of paper based on cellulose isolated by means of a gentle extraction process from aquatic macrophytes, in particular waterweed (Elodea), and paper produced by this process |
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| CN103255662A (en) * | 2013-05-06 | 2013-08-21 | 青岛大学 | Preparation method of nanometer fibril enteromorpha cellulose |
| CN103980530A (en) * | 2014-05-27 | 2014-08-13 | 哈尔滨工业大学 | Method for preparing seaweed cellulose aerogel oil absorption material |
| CN105189857A (en) * | 2013-01-25 | 2015-12-23 | 文迪克斯环境股份有限公司 | Process for isolating cellulose from cellulosic biomass, isolated cellulose of type i and composite materials comprising same |
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| CN105189857A (en) * | 2013-01-25 | 2015-12-23 | 文迪克斯环境股份有限公司 | Process for isolating cellulose from cellulosic biomass, isolated cellulose of type i and composite materials comprising same |
| CN103255662A (en) * | 2013-05-06 | 2013-08-21 | 青岛大学 | Preparation method of nanometer fibril enteromorpha cellulose |
| CN103980530A (en) * | 2014-05-27 | 2014-08-13 | 哈尔滨工业大学 | Method for preparing seaweed cellulose aerogel oil absorption material |
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