CN108624033A - A kind of preparation method of Cellulose nanocrystal modified aqueous polyurethane composite material - Google Patents
A kind of preparation method of Cellulose nanocrystal modified aqueous polyurethane composite material Download PDFInfo
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- CN108624033A CN108624033A CN201810489294.7A CN201810489294A CN108624033A CN 108624033 A CN108624033 A CN 108624033A CN 201810489294 A CN201810489294 A CN 201810489294A CN 108624033 A CN108624033 A CN 108624033A
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
-
- 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
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
- C08J2401/04—Oxycellulose; Hydrocellulose
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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
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/5398—Phosphorus bound to sulfur
Abstract
A kind of preparation method of Cellulose nanocrystal modified aqueous polyurethane composite material, belongs to Waterborne PU Composite technical field.Preparation process is as follows：Microcrystalline cellulose, chitosan and sulfuric acid solution is taken to mix under magnetic stirring, and heating water bath；Deionized water is added in mixture after to water-bath, and dialysis treatment is done after centrifugation, and then freeze-drying obtains Cellulose nanocrystal；Then aqueous polyurethane, Cellulose nanocrystal, deionized water and dipropyl disulfide are mixed for potassium phosphate；After ultrasonic disperse on polyfluortetraethylene plate film, toasted after drying.Cellulose nanocrystal modified aqueous polyurethane composite material of the present invention, Cellulose nanocrystal and aqueous polyurethane is compound, chitosan and dipropyl disulfide is added for potassium phosphate by the proportioning of science, can improve the addition in the prior art with Cellulose nanocrystal can lead to problems such as the thermal stability decline of WPU/CNs and elongation at break decline.
Description
Technical field
The invention belongs to Waterborne PU Composite technical fields, and in particular to a kind of Cellulose nanocrystal modified water-soluble
The preparation method of compound polyurethane material.
Background technology
Polyurethane is the multifunctional polymer of amido-containing acid ester structure on molecule chain.By polyurethane resin dissolving or
It is aqueous polyurethane (WPU) to be dispersed in water the binary colloid system to be formed.Due to hard, soft segment the structure of aqueous polyurethane
It is flexibly adjustable with ratio, at the same also have the characteristics that nontoxic, VOC content it is low with it is non-ignitable, in answering for the fields such as coating, adhesive
With more and more extensive.But aqueous polyurethane strand is linear structure mostly, it is difficult to obtain the high glued membrane of crosslink density, simultaneously
Hydrophilic radical is introduced in segmented structure, causes mechanical property, thermal stability and the water resistance of its film poor.Therefore, it is necessary to
Aqueous polyurethane is modified, to improve its comprehensive performance.
Nano material has the effects such as unique small-size effect, photoelectric effect, surface interface, is combined to aqueous poly-
Composite material conductive can be assigned in urethane material, inhales the characteristics such as wave, heat-insulated, wear-resisting, improve mechanical property, the hot property of material
With resistance to ag(e)ing.Cellulose is the biological material that content is most abundant in nature, the cellulose nanometer obtained from cellulose
Brilliant (CNs) is the highly crystalline substance for having bar-shaped nanostructure, has the characteristics that cheap and easy to get, renewable, easy modification,
Young's modulus is close to 150GPa.Cellulose nanocrystal and aqueous polyurethane is mutually compound, can effectively improve the heat resistance of WPU with
Mechanical property.But the thermal stability of WPU/CNs can be caused to decline with the addition of Cellulose nanocrystal.
Invention content
The technical issues of solution：In view of the above technical problems, it is poly- to provide a kind of Cellulose nanocrystal modified water-soluble by the present invention
The preparation method of urethane composite material has the advantages that preparation process is simple, prepares material thermal resistance and thermal stability are high.
Technical solution：A kind of preparation method of Cellulose nanocrystal modified aqueous polyurethane composite material, the preparation side
Method includes the following steps：
Step 1 weighs 2~5 mass parts microcrystalline celluloses, 0.1~0.5 mass parts chitosan is added to 80~100 mass
In part 64wt.% sulfuric acid solutions, after magnetic agitation, 1~2h is reacted under 30~40 DEG C of water bath conditions；
The dilution of 900~1000 mass parts deionizations is added into the mixture after water-bath by step 2, then to suspending
Liquid is centrifuged, and carries out dialysis treatment to the dispersion liquid after centrifugation with dialysis membrane, is then freeze-dried；
Step 3 take 40~50 mass parts solid contents be 30wt.% aqueous polyurethanes in flask, be added 1.5~3 mass
Cellulose nanocrystal, 10~20 mass parts deionized waters and 0.6~1.2 mass parts dipropyl disulfide of part step 2 freeze-drying
For potassium phosphate；
Flask is placed in ultrasonator by step 4, under 300~400W power conditions, ultrasonic disperse 30~
45min；
Finely dispersed dispersion liquid is poured into film on polyfluortetraethylene plate by step 5, after room temperature is dried, 68~75 DEG C of bakings
The film that thickness is 0.25~0.32mm is made in roasting 4~6h.
Preferably, weighing 3 mass parts microcrystalline celluloses in the step 1,0.4 mass parts chitosan is added to 95 matter
It measures in part 64wt.% sulfuric acid solutions, after magnetic agitation, reacts 1.5h under 35 DEG C of water bath conditions.
Preferably, the dilution of 950 mass parts deionizations is added in the step 2 into the mixture after water-bath.
Preferably, taken in the step 3 45 mass parts solid contents be 30wt.% aqueous polyurethanes in flask, be added
Cellulose nanocrystal, 15 mass parts deionized waters and the 0.8 mass parts dipropyl disulfide of 2 mass parts step 2 freeze-drying are for phosphorus
Sour potassium.
Preferably, flask is placed in ultrasonator in the step 4, under 350W power conditions, ultrasonic disperse
40min。
Preferably, after room temperature is dried in the step 5, the film that thickness is 0.3mm is made in 70 DEG C of baking 5h.
Advantageous effect：Cellulose nanocrystal modified aqueous polyurethane composite material of the present invention, by Cellulose nanocrystal
It is compound with aqueous polyurethane, chitosan and dipropyl disulfide are added for potassium phosphate by the proportioning of science, existing skill can be improved
As the addition of Cellulose nanocrystal can cause thermal stability decline and the elongation at break decline etc. of WPU/CNs to be asked in art
Topic.Composite property prepared by the present invention is excellent, glass transition temperature TgIt is -4.58~-2.89 DEG C, specific heat variable Δ Cp
For 0.546~0.637Jg-1℃-1, tensile strength be 21.32~24.54MPa, elongation at break be 1432.23~
1502.23%.
Specific implementation mode
Embodiment 1
A kind of preparation method of Cellulose nanocrystal modified aqueous polyurethane composite material, the preparation method includes following
Step：
Step 1 weighs 2 mass parts microcrystalline celluloses, 0.1 mass parts chitosan is added to 80 mass parts 64wt.% sulfuric acid
In solution, after magnetic agitation, 1h is reacted under 30 DEG C of water bath conditions；
The dilution of 900 mass parts deionizations is added into the mixture after water-bath by step 2, is then carried out to suspension
It centrifuges, dialysis treatment is carried out to the dispersion liquid after centrifugation with dialysis membrane, is then freeze-dried；
Step 3 take 40 mass parts solid contents be 30wt.% aqueous polyurethanes in flask, be added 1.5 mass parts steps
Cellulose nanocrystal, 10 mass parts deionized waters and the 0.6 mass parts dipropyl disulfide of two freeze-dryings are for potassium phosphate；
Flask is placed in ultrasonator by step 4, under 300W power conditions, ultrasonic disperse 30min；
Finely dispersed dispersion liquid is poured into film on polyfluortetraethylene plate by step 5, after room temperature is dried, 68 DEG C of bakings
The film that thickness is 0.25mm is made in 4h.
Embodiment 2
A kind of preparation method of Cellulose nanocrystal modified aqueous polyurethane composite material, the preparation method includes following
Step：
Step 1 weighs 5 mass parts microcrystalline celluloses, 0.5 mass parts chitosan is added to 100 mass parts 64wt.% sulphur
In acid solution, after magnetic agitation, 2h is reacted under 40 DEG C of water bath conditions；
Step 2 be added into the mixture after water-bath 1000 mass parts deionizations dilution, then to suspension into
Row centrifuges, and carries out dialysis treatment to the dispersion liquid after centrifugation with dialysis membrane, is then freeze-dried；
Step 3 take 50 mass parts solid contents be 30wt.% aqueous polyurethanes in flask, be added 3 mass parts step 2
The Cellulose nanocrystal of freeze-drying, 20 mass parts deionized waters and 1.2 mass parts dipropyl disulfides are for potassium phosphate；
Flask is placed in ultrasonator by step 4, under 400W power conditions, ultrasonic disperse 45min；
Finely dispersed dispersion liquid is poured into film on polyfluortetraethylene plate by step 5, after room temperature is dried, 75 DEG C of bakings
The film that thickness is 0.32mm is made in 6h.
Embodiment 3
A kind of preparation method of Cellulose nanocrystal modified aqueous polyurethane composite material, the preparation method includes following
Step：
Step 1 weighs 3 mass parts microcrystalline celluloses, 0.4 mass parts chitosan is added to 95 mass parts 64wt.% sulfuric acid
In solution, after magnetic agitation, 1.5h is reacted under 35 DEG C of water bath conditions；
The dilution of 950 mass parts deionizations is added into the mixture after water-bath by step 2, is then carried out to suspension
It centrifuges, dialysis treatment is carried out to the dispersion liquid after centrifugation with dialysis membrane, is then freeze-dried；
Step 3 take 45 mass parts solid contents be 30wt.% aqueous polyurethanes in flask, be added 2 mass parts step 2
The Cellulose nanocrystal of freeze-drying, 15 mass parts deionized waters and 0.8 mass parts dipropyl disulfide are for potassium phosphate；
Flask is placed in ultrasonator by step 4, under 350W power conditions, ultrasonic disperse 40min；
Finely dispersed dispersion liquid is poured into film on polyfluortetraethylene plate by step 5, after room temperature is dried, 70 DEG C of bakings
The film that thickness is 0.3mm is made in 5h.
Comparative example 1
With embodiment 3, difference lies in chitosan is not added, specific preparation process is as follows：
Step 1 weighs 3 mass parts microcrystalline celluloses and is added in 95 mass parts 64wt.% sulfuric acid solutions, magnetic agitation
Afterwards, 1.5h is reacted under 35 DEG C of water bath conditions；
The dilution of 950 mass parts deionizations is added into the mixture after water-bath by step 2, is then carried out to suspension
It centrifuges, dialysis treatment is carried out to the dispersion liquid after centrifugation with dialysis membrane, is then freeze-dried；
Step 3 take 45 mass parts solid contents be 30wt.% aqueous polyurethanes in flask, be added 2 mass parts step 2
The Cellulose nanocrystal of freeze-drying, 15 mass parts deionized waters and 0.8 mass parts dipropyl disulfide are for potassium phosphate；
Flask is placed in ultrasonator by step 4, under 350W power conditions, ultrasonic disperse 40min；
Finely dispersed dispersion liquid is poured into film on polyfluortetraethylene plate by step 5, after room temperature is dried, 70 DEG C of bakings
The film that thickness is 0.3mm is made in 5h.
Comparative example 2
With embodiment 3, difference lies in dipropyl disulfide is not added for potassium phosphate, specific preparation process is as follows：
Step 1 weighs 3 mass parts microcrystalline celluloses, 0.4 mass parts chitosan is added to 95 mass parts 64wt.% sulfuric acid
In solution, after magnetic agitation, 1.5h is reacted under 35 DEG C of water bath conditions；
The dilution of 950 mass parts deionizations is added into the mixture after water-bath by step 2, is then carried out to suspension
It centrifuges, dialysis treatment is carried out to the dispersion liquid after centrifugation with dialysis membrane, is then freeze-dried；
Step 3 take 45 mass parts solid contents be 30wt.% aqueous polyurethanes in flask, be added 2 mass parts step 2
The Cellulose nanocrystal of freeze-drying, 15 mass parts deionized waters；
Flask is placed in ultrasonator by step 4, under 350W power conditions, ultrasonic disperse 40min；
Finely dispersed dispersion liquid is poured into film on polyfluortetraethylene plate by step 5, after room temperature is dried, 70 DEG C of bakings
The film that thickness is 0.3mm is made in 5h.
Cellulose nanocrystal modified aqueous polyurethane composite wood prepared by Examples 1 to 3 and comparative example 1 and comparative example 2
Material carries out performance measurement.The film prepared to Examples 1 to 3 and comparative example 1 and comparative example 2 by differential scanning calorimeter carries out
Detection, obtains the glass transition temperature T of samplegWith specific heat variable Δ Cp.Then with ASTM standard, to Examples 1 to 3 and right
Composite material prepared by ratio 1 and comparative example 2 is tested.Test method be each sample according to ASTM standard, being cut into width is
6mm, gauge length are the dumbbell film of 25mm, and it is compound newly to think carefully that measurement technology Co., Ltd electronic universal tester is carried out using Shenzhen
The tensile property of object is tested.Final testing result takes the average value of 5 measurements.Test result is with reference to following table.
| Tg/℃ | ΔCp/J·g-1℃-1 | Tensile strength/MPa | Elongation at break/% | |
| Embodiment 1 | -4.58 | 0.546 | 21.32 | 1432.23 |
| Embodiment 2 | -3.97 | 0.589 | 22.37 | 1478.45 |
| Embodiment 3 | -2.89 | 0.637 | 24.54 | 1502.23 |
| Comparative example 1 | -8.22 | 0.194 | 15.62 | 865.34 |
| Comparative example 2 | -7.54 | 0.242 | 17.65 | 643.47 |
Claims (6)
1. a kind of preparation method of Cellulose nanocrystal modified aqueous polyurethane composite material, which is characterized in that the preparation side
Method includes the following steps：
Step 1 weighs 2 ~ 5 mass parts microcrystalline celluloses, 0.1 ~ 0.5 mass parts chitosan is added to 80 ~ 100 mass parts 64
In wt.% sulfuric acid solutions, after magnetic agitation, 1 ~ 2 h is reacted under 30 ~ 40 DEG C of water bath conditions；
Step 2 be added into the mixture after water-bath 900 ~ 1000 mass parts deionizations dilution, then to suspension into
Row centrifuges, and carries out dialysis treatment to the dispersion liquid after centrifugation with dialysis membrane, is then freeze-dried；
Step 3 take 40 ~ 50 mass parts solid contents be 30 wt.% aqueous polyurethanes in flask, be added 1.5 ~ 3 mass parts steps
Cellulose nanocrystal, 10 ~ 20 mass parts deionized waters and 0.6 ~ 1.2 mass parts dipropyl disulfide of two freeze-dryings are for phosphoric acid
Potassium；
Flask is placed in ultrasonator by step 4, under 300 ~ 400W power conditions, 30 ~ 45 min of ultrasonic disperse；
Finely dispersed dispersion liquid is poured into film on polyfluortetraethylene plate by step 5, after room temperature is dried, 68 ~ 75 DEG C of bakings 4 ~
The film that thickness is 0.25 ~ 0.32mm is made in 6h.
2. a kind of preparation method of Cellulose nanocrystal modified aqueous polyurethane composite material according to claim 1,
It is characterized in that, 3 mass parts microcrystalline celluloses is weighed in the step 1,0.4 mass parts chitosan is added to 95 mass parts 64
In wt.% sulfuric acid solutions, after magnetic agitation, 1.5 h are reacted under 35 DEG C of water bath conditions.
3. a kind of preparation method of Cellulose nanocrystal modified aqueous polyurethane composite material according to claim 1,
It is characterized in that, the dilution of 950 mass parts deionizations is added in the step 2 into the mixture after water-bath.
4. a kind of preparation method of Cellulose nanocrystal modified aqueous polyurethane composite material according to claim 1,
Be characterized in that, taken in the step 3 45 mass parts solid contents be 30 wt.% aqueous polyurethanes in flask, be added 2 mass parts
Cellulose nanocrystal, 15 mass parts deionized waters and the 0.8 mass parts dipropyl disulfide of step 2 freeze-drying are for potassium phosphate.
5. a kind of preparation method of Cellulose nanocrystal modified aqueous polyurethane composite material according to claim 1,
It is characterized in that, flask is placed in ultrasonator in the step 4, under 350W power conditions, 40 min of ultrasonic disperse.
6. a kind of preparation method of Cellulose nanocrystal modified aqueous polyurethane composite material according to claim 1,
It is characterized in that, after room temperature is dried in the step 5, the film that thickness is 0.3 mm is made in 70 DEG C of 5 h of baking.
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Cited By (4)
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| CN110041687A (en) * | 2019-04-15 | 2019-07-23 | 浙江梅盛实业股份有限公司 | A kind of preparation method of colour polyurethane and artificial leather |
| CN112175379A (en) * | 2020-09-30 | 2021-01-05 | 潘肖芬 | Biological membrane material |
| CN112281488A (en) * | 2020-10-13 | 2021-01-29 | 义乌市中力工贸有限公司 | Cotton fabric crease-resistant finishing agent composition |
| CN112480650A (en) * | 2020-12-09 | 2021-03-12 | 浙江理工大学 | Cellulose nanocrystal and cellulose nanofiber reinforced and toughened aqueous polyurethane composite material and preparation method thereof |
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| CN112175379A (en) * | 2020-09-30 | 2021-01-05 | 潘肖芬 | Biological membrane material |
| CN112281488A (en) * | 2020-10-13 | 2021-01-29 | 义乌市中力工贸有限公司 | Cotton fabric crease-resistant finishing agent composition |
| CN112480650A (en) * | 2020-12-09 | 2021-03-12 | 浙江理工大学 | Cellulose nanocrystal and cellulose nanofiber reinforced and toughened aqueous polyurethane composite material and preparation method thereof |
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