CN106633195A - A nanometer cellulose/clay transparent nanometer composite material and a preparing method thereof - Google Patents
A nanometer cellulose/clay transparent nanometer composite material and a preparing method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
- C08L1/04—Oxycellulose; Hydrocellulose, e.g. microcrystalline cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
A nanometer cellulose/clay transparent nanometer composite material and a preparing method thereof are disclosed. The composite material includes nanometer cellulose, clay, an auxiliary agent and water. The method includes stripping the clay with the nanometer cellulose A, mixing and stirring an obtained clay stripping solution and nanometer cellulose B, and performing drying treatment to obtain the composite material. The prepared polymer transparent nanometer composite material has excellent flame retardance, high strength, high modulus and high gas liquid barrier properties and also has characteristics of a light weight, environment protection, a high light transmittance, and the like. Through testing, the thickness of the composite material is 77-83 [mu]m, and the light transmittance of the composite material under 750 nm wavelength is 80% or above. The composite material is expected to replace some traditional transparent materials and used for product packaging, aviation and spaceflight, the automobile industry, military industry products, electron and electronic apparatus, and other fields.
Description
Technical field
The invention belongs to polymeric transparent material field, and in particular to a kind of nano-cellulose/clay transparent nano is combined
Material and preparation method thereof.
Background technology
Nano composite polymer/laminated silicate material has excellent physical and mechanical property, heat resistance and gas liquid
Barrier property, anisotropy etc., the quality light compared to conventional polymer composite and it is with low cost the advantages of so as to
With extremely wide application prospect.But in the research of nano composite polymer/laminated silicate material at this stage, due to technique
It is immature with condition, its transparence can not be made in the case where its good characteristic is kept, it is strongly limit in transparent material
The application in material field.
China Patent Publication No. CN 1569953A discloses good, the inhibited from yellowing polymerization of a kind of heat resistance height, transparency
Thing/Nano composite material of montmorillonite and preparation method thereof, by intercalation twice, is obtained novel active organo montmorillonite, then with it is poly-
Methyl methacrylate is mixed with montmorillonite content in composite, but this kind of composite and there was only 0.2-0.8%, and resin contains
Amount is too high, because resin is not easily decomposed, pollutes environment, and does not meet the theory of current environmental protection.
The extent of exfoliation of clay is higher in polymer/clay composite, and dispersiveness is better, more advantageously forms network,
So as to further enhance its glossiness and transparency.Akira Isogai et al. are prepared for a kind of superpower, high-gas resistance nanometer
Cellulose/china clay laminar composite, is prepared, although preparation process is carried out to china clay by the blending of china clay, nano-cellulose
Mechanical treatment is crossed, but due to the restriction of handling process, does not obtain the china clay lamellar structure being completely exfoliated, china clay still remains
The skeleton structure of stratiform, therefore the transparency of prepared composite is restricted.（CN Wu, T Saito, S
Fujisawa, H Fukuzumi, A Isogai, et all. Ultrastrong and High Gas-Barrier
Nanocellulose/Clay-Layered Composites, 《Biomacromolecules》, 2012, 13(6):1927-
32)。
Therefore, a kind of nano-cellulose/clay transparent nanocomposite and preparation method thereof is developed, it is existing for solving
In having technology, polymer/clay composite technology of preparing scheme, exist raw material not environmentally, production operation is loaded down with trivial details, clay stripping
From the defect such as low degree, Composite material transparent degree be low and integrated cost is high, become that those skilled in the art are urgently to be resolved hurrily to be asked
Topic.
The content of the invention
In view of this, the invention provides a kind of nano-cellulose/clay transparent nanocomposite and preparation method thereof,
For overcoming the shortcomings of that prior art is present, prepare a kind of green, nontoxic, cheap, renewable, degradable polymeric transparent and receive
Nano composite material.
In order to achieve the above object, present invention employs following technical scheme.
A kind of preparation method of nano-cellulose/clay transparent nanocomposite, comprises the following steps that：
Step one：By the mixing of clay, nano-cellulose A and water, mechanical treatment, centrifugal treating after stirring, clay stripping is obtained
Chaotropic；
Step 2：Clay stripper is mixed with nano-cellulose B, auxiliary agent, after mechanical agitation, drying process obtains described
Nano-cellulose/clay transparent nanocomposite.
Further optimize, clay described in step one is one or more in kaolin, montmorillonite and illite.
Further optimize, nano-cellulose A described in step one is fento cellulose, crystallite cellulose and bacterium
One kind in cellulose.
Further optimize, in step one, in terms of parts by weight, the clay is 90-95 parts, and nano-cellulose A is 5-
10 parts；The mixed liquid concentration of the clay, nano-cellulose A and water is 1-10mg/mL.
Further optimize, mechanical treatment described in step one includes ultrasonic cell disruptor process, high pressure homogenizer
Process or be uniformly dispersed at a high speed machine process, and the mechanical treatment degree is：The yield of monolithic layer clay accounts for clay total amount after process
20-50%.
Further optimize, in step one, the speed of the centrifugal treating is 4000-6000r/min, during centrifugal treating
Between be 20-40min；The concentration of the clay stripper is 0.2-5mg/mL.
Further optimize, nano-cellulose B described in step 2 is fento cellulose, crystallite cellulose and bacterium
One kind in cellulose.
Further optimize, auxiliary agent described in step 2 is one or more in resin, even paint and surfactant.
Further optimize, in step 2, in terms of parts by weight, the nano-cellulose B is 50-95 parts, and clay is peeled off
Liquid 5-50 parts, auxiliary agent 0-10 parts, the mixed liquid concentration of the clay stripper, nano-cellulose B and auxiliary agent is 5-10mg/mL.
Further optimize, the speed stirred described in step 2 is 2000-20000r/min, and the time of stirring is 30-
60min。
Further optimize, it is constant temperature and humidity drying to be dried described in step 2, dry temperature is 30-70 DEG C, humidity
For 30-70%RH.
Nano-cellulose obtained in the preparation method by described in any of the above-described/clay transparent nanocomposite.
In sum, the invention provides a kind of nano-cellulose/clay transparent nanocomposite and preparation method thereof.
The nano-cellulose/clay transparent nanocomposite includes following component：Nano-cellulose, clay, auxiliary agent and water.It is described
Preparation method is to peel off clay using nano-cellulose A, and the clay stripper for obtaining and nano-cellulose are mixed, and is dried
After obtain the nano-cellulose/clay transparent nanocomposite.The nano combined material of polymeric transparent prepared by the present invention
Material also imparts light weight, environmental protection, light transmittance while with excellent flame retardancy, high intensity, high-modulus, high gas-liquid barrier
High characteristic.Jing is tested, and prepared transparent nanocomposite thickness is 77 ~ 83 m, and light transmittance reaches under 750nm wavelength
More than 80%, it is expected to replace parts of traditional transparent material, solve prior art raw material not environmental protection, production operation numerous
The defect such as trivial, clay extent of exfoliation is low, Composite material transparent degree is low and integrated cost is high.
Technical solution of the present invention uses abundance, the Nanowire that biodegradable, mechanical performance is excellent, heat endurance is high
Dimension element, using its amphiphilic nature, peels off under mechanical action clay, using 1-dimention nano cellulose and two-dimensional sheet nano clay
Unique physicochemical characteristics, prepares a kind of green, nontoxic, cheap, renewable, degradable transparent nanocomposite,
Research system is potential applied widely, can be suitably used for its with similar nano cellulose material design feature or physicochemical characteristic
Allogene sill, with huge development potentiality and application prospect, is expected to replace parts of traditional transparent material, is applied to product
The fields such as packaging, Aero-Space, auto industry, war products, electronic apparatus.
Description of the drawings
Fig. 1 is the structural representation that nano-cellulose of the present invention peels off two-dimentional clay.
Specific embodiment
It is saturating to a kind of nano-cellulose/clay that the present invention is provided with reference to example in order to the present invention is described in more detail
Bright nano composite material and preparation method thereof, is specifically described.
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described enforcement
Example is only a part of embodiment of the invention, rather than the embodiment of whole.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model of present invention protection
Enclose.
The invention provides a kind of nano-cellulose/clay transparent nanocomposite and preparation method thereof, for solving
In prior art, the product that polymer/clay composite material and preparation method thereof is obtained has raw material not environmental protection, production exercise
Make the defects such as loaded down with trivial details, clay extent of exfoliation is low, Composite material transparent degree is low and integrated cost is high.
The preparation method comprises the steps：
Step one：By the mixing of clay 90-95 parts, nano-cellulose A 5-10 parts and water, the mixing that concentration is 1-10mg/mL is obtained
Liquid, carries out mechanical treatment after stirring, the yield of monolithic layer clay accounts for the 20-50% of clay total amount after process, 4000-
Centrifugal treating 20-40min under 6000r/min rotating speeds, obtains the clay stripper that concentration is 0.2-5mg/mL；
Step 2：By nano-cellulose B 50-95 parts, clay stripper 5-50 parts and the mixing of auxiliary agent 0-10 parts, obtaining concentration is
The mixed liquor of 5-10mg/mL, stir process 30-60min under 2000-20000r/min is 30-70 DEG C in temperature, and humidity is
Drying is processed and obtains nano-cellulose/clay transparent nanocomposite under 30-70%RH environment.
Nano-cellulose A of the present invention peels off the structural representation after two-dimentional clay as shown in figure 1, untreated as shown in Figure 1
Front clay is layer structure, and after lift-off processing, clay is stripped as single chip architecture, adds nano-cellulose as dispersant, profit
With the unique physical chemistry speciality of nano-cellulose so that monolithic clay keeps released state.
Embodiment 1
Fento cellulose/montmorillonite transparent nanocomposite
Step one：By the mixing of 90 parts of montmorillonite, 10 parts of fento cellulose A and water, the mixing that concentration is 5.5mg/mL is obtained
Liquid, after stirring, through ultrasonic cell disruptor process, the yield of monolithic layer montmorillonite is 40% after process, in 5000r/
Centrifugal treating 30min under min rotating speeds, obtains the montmorillonite stripper that concentration is 2.2mg/mL；
Step 2：By 90 parts of fento cellulose, the 10 parts of mixing of montmorillonite stripper, the mixing that concentration is 7.5mg/mL is obtained
Liquid, stir process 45min under 10000r/min is 45 DEG C in temperature, and humidity is that drying process obtains micro- under 45%RH environment
Fibrillated fibers element/montmorillonite transparent nanocomposite.
Fento cellulose obtained by the present invention/montmorillonite transparent nanocomposite average thickness is 80 m, and
The light transmittance measured under 750nm wavelength is 93%.
Embodiment 2
Bacteria cellulose/kaolin transparent nanocomposite
Step one：By the mixing of 92 parts of kaolin, 8 parts of fento cellulose and water, the mixed liquor that concentration is 1.0mg/mL is obtained, stirred
After mixing uniformly, through ultrasonic cell disruptor process, the kaolinic yield of monolithic layer is 50% after process, is turned in 6000r/min
Lower centrifugal treating 20min of speed, obtains the kaolin stripper that concentration is 0.5mg/mL；
Step 2：By 60 parts of bacteria cellulose, 35 parts of kaolin stripper, 5 parts of mixing of glycerine, concentration is obtained for 10mg/mL's
Mixed liquor, stir process 30min under 20000r/min is 70 DEG C in temperature, and humidity is that drying is processed under 70%RH environment
To bacteria cellulose/kaolin transparent nanocomposite.
Bacteria cellulose obtained by the present invention/kaolin transparent nanocomposite average thickness is 83 m, and
The light transmittance measured under 750nm wavelength is 85%.
Embodiment 3
Fento cellulose/kaolin/illite transparent nanocomposite
Step one：By 45 parts of kaolin, 45 parts of illite, 10 parts of crystallite cellulose and water mixing, concentration is obtained for 10mg/mL
Mixed liquor, after stirring, through high pressure homogenizer process, after process monolithic layer kaolin, illitic yield be 30%,
Centrifugal treating 30min under 5000r/min rotating speeds, obtains kaolin/illite stripper that concentration is 3 mg/mL；
Step 2：It it is 50 parts by fento cellulose, kaolin/50 parts of illite stripper mixing obtains concentration for 8mg/mL
Mixed liquor, stir process 60min under 2000r/min, temperature be 40 DEG C, humidity be 60%RH environment under drying process
After obtain fento cellulose/kaolin/illite transparent nanocomposite.
Fento cellulose/kaolin/illite transparent nanocomposite average thickness obtained by the present invention is 82
M, and the light transmittance measured under 750nm wavelength is 80%.
Embodiment 4
Crystallite cellulose/montmorillonite transparent nanocomposite
Step one：By the mixing of 95 parts of montmorillonite, 5 parts of bacteria cellulose and water, the mixed liquor that concentration is 10mg/mL, stirring are obtained
After uniform, through being uniformly dispersed at a high speed, machine is processed, and the yield of monolithic layer montmorillonite is 20% after process, under 4000r/min rotating speeds
Centrifugal treating 40min, obtains the montmorillonite stripper that concentration is 4.9mg/mL；
Step 2：It it is 95 parts by crystallite cellulose, the 5 parts of mixing of montmorillonite stripper obtain the mixing that concentration is 10mg/mL
Liquid, stir process 60min under 20000r/min is 30 DEG C in temperature, and humidity is that drying process obtains micro- under 70%RH environment
Crystallization cellulose/montmorillonite transparent nanocomposite.
Crystallite cellulose obtained by the present invention/montmorillonite transparent nanocomposite average thickness is 78 m, and
The light transmittance measured under 750nm wavelength is 91%.
Embodiment 5
Crystallite cellulose/kaolin/montmorillonite transparent nanocomposite
Step one：By 60 parts of kaolin, 33 parts of montmorillonite, 7 parts of crystallite cellulose and water mixing, concentration is obtained for 7.5mg/mL
Mixed liquor, after stirring, through high pressure homogenizer process, monolithic layer kaolin after process, the yield of montmorillonite are 40%,
Centrifugal treating 30min under 5000r/min rotating speeds, obtains kaolin/montmorillonite stripper that concentration is 3.0mg/mL；
Step 2：80 parts of crystallite cellulose, kaolinite/10 parts of montmorillonite stripper, 3 parts of ammoniacal liquor, 7 parts of polyvinyl alcohol are mixed
Close, obtain the mixed liquor that concentration is 5mg/mL, stir process 50min under 10000r/min is 55 DEG C in temperature, and humidity is
Drying obtains crystallite cellulose/kaolin/montmorillonite transparent nanocomposite after processing under 30%RH environment.
Crystallite cellulose/kaolin/montmorillonite transparent nanocomposite average thickness obtained by the present invention is 77
M, and the light transmittance measured under 750nm wavelength is 90%.
In sum, the invention provides a kind of nano-cellulose/clay transparent nanocomposite and preparation method thereof,
The polymeric transparent nano composite material includes following component：Nano-cellulose, clay, auxiliary agent and water, the preparation method
Clay is peeled off under the conditions of liquid phase mechanical treatment using nano-cellulose, Jing after centrifugation fully dispersed, uniform and stable list is obtained
Piece clay stripper, then stir with nano-cellulose mixing machinery, drying obtains nano-cellulose/clay transparent nano and is combined
Material.Polymeric transparent nano composite material prepared by the present invention with excellent flame retardancy, high intensity, high-modulus,
While high gas-liquid barrier, the characteristics such as its light weight, environmental protection, light transmittance height are imparted.Jing is tested, and prepared transparent nano is answered
In 77 ~ 83 m thickness, light transmittance reaches more than 80% to condensation material under 750nm wavelength, is expected to replace parts of traditional transparent material, solution
Determined raw material not environmental protection, production operation is loaded down with trivial details, clay extent of exfoliation is low, Composite material transparent degree is low and integrated cost is high
Etc. defect.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these modified and retouchings also should
It is considered as protection scope of the present invention.
Claims (10)
1. the preparation method of a kind of nano-cellulose/clay transparent nanocomposite, it is characterised in that comprise the steps：
Step one：By the mixing of clay, nano-cellulose A and water, mechanical treatment, centrifugal treating after stirring, clay stripping is obtained
Chaotropic；
Step 2：Clay stripper is mixed with nano-cellulose B, auxiliary agent, after mechanical agitation, drying process obtains described
Nano-cellulose/clay transparent nanocomposite.
2. the preparation method of a kind of nano-cellulose/clay transparent nanocomposite according to claim 1, its feature
It is that clay described in step one is one or more in kaolin, montmorillonite and illite.
3. the preparation method of a kind of nano-cellulose/clay transparent nanocomposite according to claim 1, its feature
It is that nano-cellulose A described in step one is the one kind in fento cellulose, crystallite cellulose and bacteria cellulose.
4. the preparation method of a kind of nano-cellulose/clay transparent nanocomposite according to claim 1, its feature
It is that in step one, in terms of parts by weight, the clay is 90-95 parts, and nano-cellulose A is 5-10 parts；The clay, receive
The mixed liquid concentration of rice cellulose A and water is 1-10mg/mL.
5. the preparation method of a kind of nano-cellulose/clay transparent nanocomposite according to claim 1, its feature
It is that in step one, the mechanical treatment includes that ultrasonic cell disruptor is processed, high pressure homogenizer process or high speed disperse equal
Even machine is processed, and the mechanical treatment degree is：The yield of monolithic layer clay accounts for the 20-50% of clay total amount after process.
6. the preparation method of a kind of nano-cellulose/clay transparent nanocomposite according to claim 1, its feature
It is that in step one, the speed of the centrifugal treating is 4000-6000r/min, and the centrifugal treating time is 20-40min；It is described
The concentration of clay stripper is 0.2-5mg/mL.
7. the preparation method of a kind of nano-cellulose/clay transparent nanocomposite according to claim 1, its feature
It is that in step 2, the nano-cellulose B is the one kind in fento cellulose, crystallite cellulose and bacteria cellulose；
The auxiliary agent is one or more in resin, even paint and surfactant.
8. the preparation method of a kind of nano-cellulose/clay transparent nanocomposite according to claim 1, its feature
Be, in step 2, in terms of parts by weight, the nano-cellulose B be 50-95 parts, clay stripper 5-50 parts, auxiliary agent 0-10
Part；The clay stripper, nano-cellulose B, the mixed liquid concentration of auxiliary agent are 5-10mg/mL.
9. the preparation method of a kind of nano-cellulose/clay transparent nanocomposite according to claim 1, its feature
It is that in step 2, the speed of the stirring is 2000-20000r/min, and the time of stirring is 30-60min；The drying is
Constant temperature and humidity drying, dry temperature is 30-70 DEG C, and humidity is 30-70%RH.
10. a kind of nano-cellulose/clay transparent nano is combined obtained in the preparation method by described in any one of claim 1-9
Material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107216488A (en) * | 2017-06-29 | 2017-09-29 | 南京理工大学 | A kind of bacteria cellulose/bar-shaped clay composite membrane and preparation method thereof |
| CN107416854A (en) * | 2017-07-26 | 2017-12-01 | 华南理工大学 | A kind of monolithic layer clay stripper and preparation method thereof |
| CN107459045A (en) * | 2017-07-26 | 2017-12-12 | 华南理工大学 | A kind of clay film and preparation method thereof |
| WO2019002680A1 (en) * | 2017-06-26 | 2019-01-03 | Teknologian Tutkimuskeskus Vtt Oy | Fire-retardant composition and coating |
| CN112912424A (en) * | 2018-10-12 | 2021-06-04 | 株式会社庆东元 | Method for preparing thermosetting foam having excellent flame retardancy and thermosetting foam prepared using the same |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019002680A1 (en) * | 2017-06-26 | 2019-01-03 | Teknologian Tutkimuskeskus Vtt Oy | Fire-retardant composition and coating |
| US11608443B2 (en) | 2017-06-26 | 2023-03-21 | Teknologian Tutkimuskeskus Vtt Oy | Fire-retardant composition and coating |
| CN107216488A (en) * | 2017-06-29 | 2017-09-29 | 南京理工大学 | A kind of bacteria cellulose/bar-shaped clay composite membrane and preparation method thereof |
| CN107416854A (en) * | 2017-07-26 | 2017-12-01 | 华南理工大学 | A kind of monolithic layer clay stripper and preparation method thereof |
| CN107459045A (en) * | 2017-07-26 | 2017-12-12 | 华南理工大学 | A kind of clay film and preparation method thereof |
| CN112912424A (en) * | 2018-10-12 | 2021-06-04 | 株式会社庆东元 | Method for preparing thermosetting foam having excellent flame retardancy and thermosetting foam prepared using the same |
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| CN106633195B (en) | 2020-09-22 |
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