CN109679115A - The preparation method of fibrillation cellulose suspension - Google Patents
The preparation method of fibrillation cellulose suspension Download PDFInfo
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- CN109679115A CN109679115A CN201811530718.6A CN201811530718A CN109679115A CN 109679115 A CN109679115 A CN 109679115A CN 201811530718 A CN201811530718 A CN 201811530718A CN 109679115 A CN109679115 A CN 109679115A
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- cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/04—Oxycellulose; Hydrocellulose
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Abstract
The present invention discloses a kind of preparation method of fibrillation cellulose suspension, comprising the following steps: (1) prepares pretreatment fluid: sodium hydroxide, urea, deionized water being mixed, stirring obtains pretreatment fluid；(2) pretreatment of microcrystalline cellulose: microcrystalline cellulose is added in pretreatment fluid, then stirring is heated, is ultrasonically treated after cooled to room temperature, is then centrifuged for, and is filtered, is washed with deionized, what is filtered is precipitated as pretreated microcrystalline cellulose；(3) preparation of fento cellulose: the product of step (2) is configured to the suspension that mass concentration is 0.5-1.5% with deionized water, then homogenizes, obtains fibrillation cellulose suspension.Method provided by the invention, the fento cellulose of preparation are cellulose Ⅰ type, and the crystallinity of fento cellulose is 60.4%, and yield is up to 80% or so, and thermal stability is good.
Description
Technical field
The invention belongs to cellulose technology fields, and in particular to a kind of preparation method of fibrillation cellulose suspension.
Background technique
Nano-cellulose is broadly defined as cellulose of at least one dimension scale within the scope of 1-100 nm, Ke Yi
Stable colloid is dispersed into water, it is non-toxic and tasteless, it is both not soluble in water under room temperature, also it is not dissolved in common organic solvents.It is usually
Referred to as nanofibrils cellulose (Nanofibrillatedcellulose, NFC), fento cellulose
(Microfibrillatedcellulose, MFC), Cellulose nanocrystal (Cellulosenanocrystals, CNCs), nanometer
Microcrystalline cellulose (Nanocrystallinecellulose, NCC), Cellulose nanocrystal must (Cellulosenanowhisker,
CNW), cellulose nano particle (Cellulosenanoparticle, CNP) etc..According to nano-cellulose pattern, particle size
And the difference of raw material, nano-cellulose are generally divided into 3 classes.Compared with cellulose and microcrystalline cellulose, nano-cellulose in addition to
Except reproducibility and biodegradable, also with the excellent performance of many nanoparticles, such as higher chemical reaction
Activity, large specific surface area, high-crystallinity, high thermal stability, high Young's modulus, high intensity, hyperfine structure and high transparency
Deng.Excellent performance leads nano-cellulose in functional composite materials such as medicine, reinforcing material, transparent membrane barrier materials
Domain is with a wide range of applications.
Currently, the method for preparing nano-cellulose mainly has chemical method, Mechanical Method, bioanalysis.Wherein, chemical method is to pass through
The NCC for obtaining that there is high-crystallinity to remove amorphous region is chemically treated to fiber.It is hydrolyzed using 64% concentrated sulfuric acid fine
Dimension element can prepare the NCC of corynebacterium, uniform particle diameter, but yield is low, and the concentrated sulfuric acid has strong corruption in preparation process
Corrosion, the high requirements on the equipment, final product purification process time-consuming water consumption, reagent recycling is difficult, has certain destruction to make environment
With.Mechanical Method is directly to carry out mechanical treatment to fiber, such as mill, homogeneous, ultrasound or microjet processing obtain MFC.It is powerful
Physical shear conquassation effect can make fiber wire-dividing broom purification, tiny microfibril is removed from fiber finer cell wall, and gradually forming has
The cellulose of nanoscale.Though greatly reducing the use of reagent using these high speed grinding equipment, energy consumption is high, production cost
It is high.Bioanalysis, which prepares nano-cellulose, to be synthesized using bacterium, and bacteria cellulose elasticity modulus is big, good mechanical stability, compares table
Area is big, and has good biocompatibility and degradability；But its long preparation period, low efficiency, and bacterium is for synthesis
The requirement of environment is very high, is generally also not easy largely to be prepared.So the preparation of nano-cellulose often combines chemistry pre-
Processing and mechanical treatment, to reduce energy consumption.For the preparation of nano-cellulose, urgent need develops environmentally protective, inexpensive system
Preparation Method.
Summary of the invention
In view of the drawbacks of the prior art, the present invention provides a kind of preparation method of fibrillation cellulose suspension.
The preparation method of fibrillation cellulose suspension, comprising the following steps:
(1) pretreatment fluid is prepared: by sodium hydroxide, urea, deionized water according to mass ratio (5-10): (15-20): (80-90)
Mixing, stirs 20-30min under the revolving speed of 500rpm, obtains pretreatment fluid；
(2) pretreatment of microcrystalline cellulose: microcrystalline cellulose is added in pretreatment fluid, stirs 30- under the revolving speed of 1000rpm
40min is then heated to 40-50 DEG C of holding 30-45min, is ultrasonically treated 10-15min after cooled to room temperature, then from
The heart is filtered, is washed with deionized 5-10 times, what is filtered is precipitated as pretreated microcrystalline cellulose；
(3) preparation of fento cellulose: it is 0.5-1.5%'s that the product of step (2), which is configured to mass concentration, with deionized water
Then suspension homogenizes, obtain fibrillation cellulose suspension.
Preferably, step (2) microcrystalline cellulose is corncob microcrystalline cellulose.
Preferably, the mass ratio of step (2) microcrystalline cellulose and pretreatment fluid is (1-6): 50.
Preferably, the condition of step (2) described ultrasonic treatment are as follows: ultrasonic power 400-500W, supersonic frequency 45KHz.
Preferably, the condition of step (2) described centrifugation are as follows: revolving speed 3000rpm, centrifugation time 30-40min.
Preferably, the number to homogenize is 3 times, wherein the pressure to homogenize for the first time is 80MPa, and second
The pressure of matter is 90MPa, and the pressure to homogenize for the third time is 110MPa.
Corncob microcrystalline cellulose of the present invention is purchased from Shengquan Group Co. Ltd., Jinan.
Advantages of the present invention:
The fento cellulose of method provided by the invention, preparation is cellulose Ⅰ type, and the crystallinity of fento cellulose is
60.4%, yield is up to 80% or so, and thermal stability is good, and thermal degradation temperature is up to 240 DEG C, and diameter is in 5-20nm.
Specific embodiment
Embodiment 1
The preparation method of fibrillation cellulose suspension, comprising the following steps:
(1) it prepares pretreatment fluid: sodium hydroxide, urea, deionized water being mixed according to mass ratio 5: 15: 80,500rpm's
20min is stirred under revolving speed, obtains pretreatment fluid；
(2) pretreatment of microcrystalline cellulose: the microcrystalline cellulose used is corncob microcrystalline cellulose；According to the microcrystalline cellulose
The mass ratio of element and pretreatment fluid is 1:50, and microcrystalline cellulose is added in pretreatment fluid, is stirred under the revolving speed of 1000rpm
30min, is then heated to 40 DEG C of holding 45min, after cooled to room temperature, in ultrasonic power 400W, supersonic frequency 45KHz
Under the conditions of be ultrasonically treated 10min, be then centrifuged 30min under conditions of revolving speed 3000rpm, filter, be washed with deionized 5
Secondary, what is filtered is precipitated as pretreated microcrystalline cellulose；
(3) product of step (2) preparation of fento cellulose: is configured to the suspension that mass concentration is 0.5% with deionized water
Then liquid homogenizes 3 times, the number to homogenize is 3 times, wherein the pressure to homogenize for the first time is 80MPa, for the second time
The pressure to homogenize is 90MPa, and the pressure to homogenize for the third time is 110MPa, obtains fibrillation cellulose suspension.
Embodiment 2
The preparation method of fibrillation cellulose suspension, comprising the following steps:
(1) it prepares pretreatment fluid: sodium hydroxide, urea, deionized water being mixed according to mass ratio 10: 20: 90,500rpm's
30min is stirred under revolving speed, obtains pretreatment fluid；
(2) pretreatment of microcrystalline cellulose: the microcrystalline cellulose used is corncob microcrystalline cellulose；According to the microcrystalline cellulose
The mass ratio of element and pretreatment fluid is 6:50, and microcrystalline cellulose is added in pretreatment fluid, is stirred under the revolving speed of 1000rpm
40min, is then heated to 50 DEG C of holding 30min, after cooled to room temperature, in ultrasonic power 500W, supersonic frequency 45KHz
Under the conditions of be ultrasonically treated 10min, be then centrifuged 40min under conditions of revolving speed 3000rpm, filter, be washed with deionized 10
Secondary, what is filtered is precipitated as pretreated microcrystalline cellulose；
(3) product of step (2) preparation of fento cellulose: is configured to the suspension that mass concentration is 1.5% with deionized water
Then liquid homogenizes 3 times, the number to homogenize is 3 times, wherein the pressure to homogenize for the first time is 80MPa, for the second time
The pressure to homogenize is 90MPa, and the pressure to homogenize for the third time is 110MPa, obtains fibrillation cellulose suspension.
Embodiment 3
The preparation method of fibrillation cellulose suspension, comprising the following steps:
(1) it prepares pretreatment fluid: sodium hydroxide, urea, deionized water being mixed according to mass ratio 8: 18: 85,500rpm's
25min is stirred under revolving speed, obtains pretreatment fluid；
(2) pretreatment of microcrystalline cellulose: the microcrystalline cellulose used is corncob microcrystalline cellulose；According to the microcrystalline cellulose
The mass ratio of element and pretreatment fluid is 3:50, and microcrystalline cellulose is added in pretreatment fluid, is stirred under the revolving speed of 1000rpm
35min, is then heated to 45 DEG C of holding 40min, after cooled to room temperature, in ultrasonic power 450W, supersonic frequency 45KHz
Under the conditions of be ultrasonically treated 12min, be then centrifuged 35min under conditions of revolving speed 3000rpm, filter, be washed with deionized 8
Secondary, what is filtered is precipitated as pretreated microcrystalline cellulose；
(3) product of step (2) preparation of fento cellulose: is configured to the suspension that mass concentration is 1% with deionized water
Then liquid homogenizes 3 times, the number to homogenize is 3 times, wherein the pressure to homogenize for the first time is 80MPa, for the second time
The pressure to homogenize is 90MPa, and the pressure to homogenize for the third time is 110MPa, obtains fibrillation cellulose suspension.
Claims (6)
1. the preparation method of fibrillation cellulose suspension, it is characterised in that: the following steps are included:
(1) pretreatment fluid is prepared: by sodium hydroxide, urea, deionized water according to mass ratio (5-10): (15-20): (80-90)
Mixing, stirs 20-30min under the revolving speed of 500rpm, obtains pretreatment fluid；
(2) pretreatment of microcrystalline cellulose: microcrystalline cellulose is added in pretreatment fluid, stirs 30- under the revolving speed of 1000rpm
40min is then heated to 40-50 DEG C of holding 30-45min, is ultrasonically treated 10-15min after cooled to room temperature, then from
The heart is filtered, is washed with deionized 5-10 times, what is filtered is precipitated as pretreated microcrystalline cellulose；
(3) preparation of fento cellulose: it is 0.5-1.5%'s that the product of step (2), which is configured to mass concentration, with deionized water
Then suspension homogenizes, obtain fibrillation cellulose suspension.
2. the preparation method of fibrillation cellulose suspension according to claim 1, it is characterised in that: step (2) is described micro-
Crystalline cellulose is corncob microcrystalline cellulose.
3. the preparation method of fibrillation cellulose suspension according to claim 1, it is characterised in that: step (2) is described micro-
The mass ratio of crystalline cellulose and pretreatment fluid is (1-6): 50.
4. the preparation method of fibrillation cellulose suspension according to claim 1, it is characterised in that: step (2) is described super
The condition of sonication are as follows: ultrasonic power 400-500W, supersonic frequency 45KHz.
5. the preparation method of fibrillation cellulose suspension according to claim 1, it is characterised in that: step (2) it is described from
The condition of the heart are as follows: revolving speed 3000rpm, centrifugation time 30-40min.
6. the preparation method of fibrillation cellulose suspension according to claim 1, it is characterised in that: time to homogenize
Number is 3 times, wherein the pressure to homogenize for the first time is 80MPa, and the pressure to homogenize for the second time is 90MPa, is homogenized for the third time
Pressure be 110MPa.
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| CN201811530718.6A CN109679115A (en) | 2018-12-14 | 2018-12-14 | The preparation method of fibrillation cellulose suspension |
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| CN201811530718.6A CN109679115A (en) | 2018-12-14 | 2018-12-14 | The preparation method of fibrillation cellulose suspension |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117328287A (en) * | 2023-11-13 | 2024-01-02 | 华邦特西诺采新材料股份有限公司 | Nanocellulose composite material and paper with nanocellulose composite material |
-
2018
- 2018-12-14 CN CN201811530718.6A patent/CN109679115A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117328287A (en) * | 2023-11-13 | 2024-01-02 | 华邦特西诺采新材料股份有限公司 | Nanocellulose composite material and paper with nanocellulose composite material |
| CN117328287B (en) * | 2023-11-13 | 2024-05-10 | 华邦特西诺采新材料股份有限公司 | Nanocellulose composite material and paper with nanocellulose composite material |
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