CN109053907A - A method of preparing nano micro crystal cellulose - Google Patents
A method of preparing nano micro crystal cellulose Download PDFInfo
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- CN109053907A CN109053907A CN201810717325.XA CN201810717325A CN109053907A CN 109053907 A CN109053907 A CN 109053907A CN 201810717325 A CN201810717325 A CN 201810717325A CN 109053907 A CN109053907 A CN 109053907A
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- micro crystal
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
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Abstract
The invention discloses a kind of preparation methods for preparing nano micro crystal cellulose, it is characterized in that method and step is as follows: cellulosic material is dispersed in advance dissolved in the water of cellulase activators, and adjusting system pH value is 4-8, the cellulase dissolved in advance through water is added, it is hydrolyzed 2-20 hours at 40-60 DEG C, obtains the slurry containing microcrystalline cellulose；By the slurry containing microcrystalline cellulose through ultrasonic grind, then through washing purification, obtain nano micro crystal cellulose filter cake；It is nano micro crystal cellulose filter cake is broken, dry, obtain nano micro crystal cellulose semi-finished product；Nano micro crystal cellulose semi-finished product obtain nano micro crystal cellulose after crushed.Beneficial effects of the present invention: using purified cotton, wood pulp cellulose or bamboo pulp fiber element as raw material, production cost is effectively reduced；Using cellulase as hydrolysing agent, the requirement to equipment is effectively reduced；One of cellulase subacidity cellulase, neutral cellulase, alkali cellulose enzyme；Reaction condition is mild, low energy consumption.
Description
Technical field
The invention belongs to technical field of polymer chemistry, are related to a kind of preparation method for preparing nano micro crystal cellulose.
Background technique
Native cellulose is the most abundant biomass resource on the earth, and the annual yield in the whole world is about 7.5 × 1010t。
It is present in various biologies, as plant, animal and some bacteriums are medium.Cellulose is by β-D- pyrans formula grape
The linear natural polymer that glycosyl is formed by connecting each other with Isosorbide-5-Nitrae-β-glycosidic bond, mainly by crystal region and noncrystalline domain two
It is grouped as.Currently, cellulose is widely used to biological medicine, packaging, automobile and other industries.
Nano-cellulose (Nanocelluloe, NC) is using fibrous material as raw material, at chemistry, physics or biology
The cellulosic material with 1-dimention nano size of the approach preparation of reason, it is with the basic structure of cellulose, performance and receives
The typical characteristics of rice grain, such as: density is low, derives from renewable raw materials, biodegradable, elasticity modulus is up to 140GPa, has
It is modified etc. conducive to surface is carried out to it.
Huge specific surface area, higher Young's modulus, superpower adsorption capacity and high reactivity, make nanofiber
Element has some distinctive optical properties, rheological property and mechanical performance.These characteristics make it have wide application value, can
Using as the reinforcing material in nanocomposite, and for medicine, packaging, papermaking, food additives, paint,
The fields such as plate, building materials.
The technology that nano micro crystal cellulose is prepared in Vehicles Collected from Market has: mineral acid hydrolysis method, mixed-acid hydrolysis method, mixed acid
Auxiliary ultrasonic Hydrolyze method, radiation exposure edman degradation Edman, mechanical degradation method: including mechanical milling method, high pressure homogenization method etc., biology
Method.
Method advantage of the invention is: microcrystalline cellulose is prepared using enzyme hydrolysis method, it is micro- using ultrasonic grind to make
Crystalline cellulose, which is further degraded, to be reached nanoscale and obtains nano micro crystal cellulose.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of preparation method for preparing nano micro crystal cellulose,
It uses purified cotton, wood pulp cellulose or bamboo pulp fiber element for raw material in the method, using cellulase as hydrolysing agent, passes through
The processes such as hydrolysis, Ultrasonic Pulverization, purification, drying, crushing obtain microcrystalline cellulose product.
To achieve the purpose of the present invention, it provides the following technical solutions: a kind of preparation method preparing nano micro crystal cellulose,
It is characterized in that method and step is as follows:
(1) cellulosic material is dispersed in advance dissolved in the water of 0.05-0.5 (w/w) % cellulase activators, and adjusted
Whole system pH value is 4-8, and the cellulase dissolved in advance through water is added, hydrolyzes 2-20 hours, is obtained containing micro- at 40-60 DEG C
The slurry of crystalline cellulose；
(2) by the slurry containing microcrystalline cellulose through ultrasonic grind, then through washing purification, nano micro crystal cellulose is obtained
Filter cake；
(3) nano micro crystal cellulose filter cake is broken, dry, obtain nano micro crystal cellulose semi-finished product；
(4) nano micro crystal cellulose semi-finished product obtain nano micro crystal cellulose after crushed.
Middle China Forestry Science Research Institute Zhuo Zhifei of the present invention et al. is prepared using cellulose hydrolyzation bamboo pulp fiber
During nano micro crystal cellulose, after carrying out grinding pretreatment to bamboo pulp fiber using PFI mill first, cellulase is recycled
It hydrolyzes 2-4 days and nano micro crystal cellulose is made through ultrasonic disperse.In the present invention, cellulosic raw material is through simple crushing, nothing
It the pretreatment such as need to grind, reduce the difficulty of process implementing；In the reaction system by the way that suitable cellulase activators are added,
Improve enzymolysis efficiency, highly shortened the process time, wherein zymoexciter be one of sodium chloride, potassium chloride or its
Compound, additional amount are 0.05-0.5 (w/w) %.
Beneficial effects of the present invention:
1) fine with purified cotton, wood pulp in the method the present invention provides a kind of preparation method of nano micro crystal cellulose
Dimension element or bamboo pulp fiber element are raw material, effectively reduce production cost；
It 2) with cellulase is hydrolysis in the method the present invention provides a kind of preparation method of nano micro crystal cellulose
Reagent effectively reduces the requirement to equipment；
3) the present invention provides a kind of preparation method of nano micro crystal cellulose, the method cellulase subacidity is fine
Tie up one of plain enzyme, neutral cellulase, alkali cellulose enzyme；
4) the present invention provides a kind of preparation method of nano micro crystal cellulose, reaction condition is mild in the method, energy
Source consumption is low；
5) the present invention provides a kind of preparation method of nano micro crystal cellulose, the method stable technical process, operations
Simplicity, microcrystalline cellulose obtained, appearance are white powder, and uniformity is good.
Specific embodiment
The present invention is described in detail combined with specific embodiments below, but not limited to this.
Wood pulp of the present invention be Chile produce " silver-colored star " board wood pulp, bamboo pulp be domestic bamboo pulp, degree of polymerization 1300-1500,
Purified cotton is the M15 type product of Hebei purified cotton company production.
Embodiment 1
In the reactor with stirring, 1kg is dispersed in by broken wood pulp cellulose/bamboo pulp/purified cotton raw materials
It is in advance 4.0 dissolved with the pH value in the water of 0.05% cellulase activators, adjusting reaction system, is added and is dissolved with 500ml water
Cellulase, stir evenly, system temperature risen to 59-60 DEG C, is reacted 20 hours.After reaction, gained slurry is turned
Enter and is handled in ultrasonic reaction kettle, expelling water in vacuumfilter, and washing purification is carried out with 10L moisture 4 times, obtain nano microcrystalline fibre
Plain filter cake is tieed up, through being dried to obtain nano microcrystalline cellulose product.
Embodiment 2
In the reactor with stirring, by 1kg by broken bamboo pulp fiber element stock dispersion in advance dissolved with 0.1%
In the water of cellulase activators, the pH value for adjusting reaction system is 4.5, and the cellulase dissolved with 500ml water, stirring is added
Uniformly, system temperature is risen to 54-55 DEG C, reacted 10 hours.After reaction, gained slurry is transferred in ultrasonic reaction kettle
Reason is filtered by vacuum expelling water, and carries out washing purification with 10L moisture 4 times, obtains nano micro crystal cellulose filter cake, then through dry
To nano microcrystalline cellulose product.
Embodiment 3
In the reactor with stirring, by 1kg by broken bamboo pulp fiber element stock dispersion in advance dissolved with
In the water of 0.15% cellulase activators, the pH value for adjusting reaction system is 5.0, and the cellulose dissolved with 500ml water is added
Enzyme stirs evenly, and system temperature is risen to 54-55 DEG C, is reacted 5 hours.After reaction, gained slurry is transferred to ultrasonic reaction
It is handled in kettle, expelling water is filtered by vacuum, and carry out washing purification with 5000ml moisture 4 times, obtains nano micro crystal cellulose filter cake；Again
Through being dried to obtain nano microcrystalline cellulose product.
Embodiment 4
In the reactor with stirring, by 1kg by broken wood pulp cellulose stock dispersion in advance dissolved with 0.3%
In the water of cellulase activators, the pH value for adjusting reaction system is 6.5, and the cellulase dissolved with 500ml water, stirring is added
Uniformly, system temperature is risen to 54-55 DEG C, reacted 3 hours.After reaction, gained slurry is transferred in ultrasonic reaction kettle
Reason is filtered by vacuum expelling water, and carries out washing purification with 10L moisture 4 times, obtains nano micro crystal cellulose filter cake；Filter cake is through drying
And obtain nano microcrystalline cellulose product.
Embodiment 5
In the reactor with stirring, by 1kg by broken wood pulp cellulose stock dispersion in advance dissolved with 0.5%
In the water of cellulase activators, the pH value for adjusting reaction system is 8.0, and the cellulase dissolved with 500ml water, stirring is added
Uniformly, system temperature is risen to 50-55 DEG C, reacted 18 hours.After reaction, gained slurry is transferred in ultrasonic reaction kettle
Reason is filtered by vacuum expelling water, and carries out washing purification with 10L moisture 4 times, obtains nano micro crystal cellulose filter cake；Filter cake is through drying
Obtain nano microcrystalline cellulose product.
Claims (3)
1. a kind of preparation method for preparing nano micro crystal cellulose, it is characterised in that method and step is as follows:
(1) cellulosic material is dispersed in advance dissolved in the water of 0.05-0.5 (w/w) % cellulase activators, and adjusts and is
System pH value is 4-8, and the cellulase dissolved in advance through water is added, hydrolyzes 2-20 hours at 40-60 DEG C, is obtained containing crystallite fibre
Tie up the slurry of element；
(2) by the slurry containing microcrystalline cellulose through ultrasonic grind, then through washing purification, nano micro crystal cellulose filter is obtained
Cake；
(3) nano micro crystal cellulose filter cake is broken, dry, obtain nano micro crystal cellulose semi-finished product；
(4) nano micro crystal cellulose semi-finished product obtain nano micro crystal cellulose after crushed.
2. a kind of preparation method for preparing nano micro crystal cellulose according to claim 1, it is characterised in that: cellulose is former
Material is purified cotton, wood pulp cellulose or bamboo pulp fiber element.
3. a kind of preparation method for preparing nano micro crystal cellulose according to claim 1, it is characterised in that: cellulase
For hydrolysing agent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810717325.XA CN109053907A (en) | 2018-07-03 | 2018-07-03 | A method of preparing nano micro crystal cellulose |
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| CN201810717325.XA CN109053907A (en) | 2018-07-03 | 2018-07-03 | A method of preparing nano micro crystal cellulose |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110590963A (en) * | 2019-10-24 | 2019-12-20 | 福州大学 | Kelp cellulose nanocrystal and preparation method thereof |
| WO2022229510A1 (en) * | 2021-04-30 | 2022-11-03 | Andritz Oy | System and method for producing microcrystalline cellulose |
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| CN103726379A (en) * | 2014-01-09 | 2014-04-16 | 齐鲁工业大学 | Application of modified nano-microcrystalline cellulose serving as papermaking strengthening agent |
| CN103726380A (en) * | 2014-01-09 | 2014-04-16 | 齐鲁工业大学 | Application of modified nano-microcrystalline cellulose serving as retention and drainage aid for papermaking |
| CN104293858A (en) * | 2013-07-19 | 2015-01-21 | 天津科技大学 | Preparation method for nano-microcrystalline cellulose |
| FI20145299A (en) * | 2014-03-31 | 2015-10-01 | Upm Kymmene Corp | A process for preparing fibrillated cellulose |
| CN105603020A (en) * | 2016-01-21 | 2016-05-25 | 青岛农业大学 | Nanocrystalline cellulose preparation method |
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2018
- 2018-07-03 CN CN201810717325.XA patent/CN109053907A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104293858A (en) * | 2013-07-19 | 2015-01-21 | 天津科技大学 | Preparation method for nano-microcrystalline cellulose |
| CN103726379A (en) * | 2014-01-09 | 2014-04-16 | 齐鲁工业大学 | Application of modified nano-microcrystalline cellulose serving as papermaking strengthening agent |
| CN103726380A (en) * | 2014-01-09 | 2014-04-16 | 齐鲁工业大学 | Application of modified nano-microcrystalline cellulose serving as retention and drainage aid for papermaking |
| FI20145299A (en) * | 2014-03-31 | 2015-10-01 | Upm Kymmene Corp | A process for preparing fibrillated cellulose |
| CN105603020A (en) * | 2016-01-21 | 2016-05-25 | 青岛农业大学 | Nanocrystalline cellulose preparation method |
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| 蒋玲玲等: ""纤维素酶制备纳米纤维素晶体的研究"", 《化学与生物工程》 * |
| 高雪丽主编: "《食品添加剂》", 31 January 2013, 中国科学技术出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110590963A (en) * | 2019-10-24 | 2019-12-20 | 福州大学 | Kelp cellulose nanocrystal and preparation method thereof |
| WO2022229510A1 (en) * | 2021-04-30 | 2022-11-03 | Andritz Oy | System and method for producing microcrystalline cellulose |
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