CN108795018A - A kind of preparation method of polyurethane/fibrination functional configurations memory high molecular material - Google Patents
A kind of preparation method of polyurethane/fibrination functional configurations memory high molecular material Download PDFInfo
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- CN108795018A CN108795018A CN201810649692.0A CN201810649692A CN108795018A CN 108795018 A CN108795018 A CN 108795018A CN 201810649692 A CN201810649692 A CN 201810649692A CN 108795018 A CN108795018 A CN 108795018A
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- polyurethane
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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
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
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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
- C08L2201/12—Shape memory
Abstract
The present invention relates to the preparation methods that a kind of polyurethane/fibrination functional configurations remember high molecular material, and the composite solution of clear is obtained using ultrasonic disperse after ion solvent, absolute ethyl alcohol and deionized water are mixed；Silane coupling agent is added into composite solution, and acetic acid is added dropwise and adjusts solution PH, agitating solution makes silane coupling agent that hydrolysis occur；Microcrystalline cellulose is added into solution, is filtered using Buchner funnel after being sufficiently stirred；Step takes filter residue, and filter residue, which is placed in freeze drier, to be freeze-dried to obtain the microcrystalline cellulose of functionalization；The microcrystalline cellulose of functionalization, rhodamine are added into the mixed solution of polyurethane and N-Methyl pyrrolidone and stirs for step 5.The present invention by after functionalization cellulose and polyurethane and rhodamine carry out solution cast and prepare composite material, the binary heterozygosis network based on cellulose primitive is constructed, the shape memory high molecule material for taking into account temperature-responsive and ultraviolet light response for having high intensity, high tenacity is prepared.
Description
Technical field
The present invention relates to a kind of preparation method of shape memory high molecule material more particularly to a kind of polyurethane/celluloses
The preparation method of multi-functional shape memory high molecule material.
Background technology
Polymer shape memory material is a kind of stimulation-responsive materials changed by shape.Cause shape memory effect
Stimulation can be temperature, electric current, magnetic field, pH value, humidity and illumination etc..This kind of material is big with deflection, mechanical property is big
The feature that range is adjustable, while there is cheap, light weight and the molding advantage of easy processing.In recent years, shape memory is poly-
Object is closed with its excellent property, huge application prospect, such as intelligence sensor, intelligence weaving are shown in intellectual material field
Material, biologic medical medicament slow release direction, aerospace field have huge application.Polyurethane（SMPU）It is one kind to have firmly
The shape-memory polymer that segment and soft chain segment are constituted, this kind of high molecular advantage is can be by the ratio of control soft and hard segments
Or other groups are introduced to adjust or change its shape memory function.SMPU has excellent mechanical property and good biology
Compatibility, memory temperature can scope of design be wide, deformation quantity is big, shape memory effect is good, processability is good, but due to soft and hard segments
Phase separation also makes it there are recovery of shape speed the shortcomings of slow, repetitive memory effect is poor, mechanical strength is low, response function is single,
Traditional shape memory polyurethane material can no longer meet its requirement in some fields such as aerospaces now.How to improve
Its mechanical strength, prepares the problems such as multiple response functional material at recovery of shape rate, to widen its application field, is always
Problem to be solved.
Cellulose is a kind of inexhaustible, nexhaustible renewable resource.It has high-modulus, large specific surface area etc. excellent
Different physicochemical property, and it is compared with synthesizing macromolecule, cellulose also have can it is degradable, nontoxic, pollution-free, be easy to change
The advantages such as property, good biocompatibility, renewable, it is considered to be the main raw material(s) of following world energy sources and chemical industry is expected to replace
For glass fibre and other synthetic fibers.Currently, numerous scientific researchers remove enhancing polyurethane material by using cellulose
Material, and a series of significant achievements are gone, since the three-dimensional hydrogen bond network that the introducing of cellulose forms rigidity makes poly- ammonia
The intensity and modulus of ester material is greatly enhanced.But so far, the overwhelming majority removes toughening polyurethane using cellulose
While, necessarily lead to the greatly decline of toughness of material, it is therefore, how good under the degree of control polyurethane phase separation
Keep its shape memory function and prepare have the polyurethane material that strength and toughness gets both to meet aerospace with
And the demand in intelligence sensor field is very harsh.
Rhodamine be it is a kind of possessing excellent optical property, of low cost and stability is good, is often used as phosphor
The ideal material of material and bioprobe.It shows huge application prospect in terms of biosensor and medicament slow release, but
Be almost without report as fluorescer while and as the structural component with high molecular material to go regulation and control material
The physical and chemical performance of material.
Invention content
Present invention aims to overcome that existing memory material can not accomplish the polyurethane material that high intensity gets both with high tenacity
Difficulty, provide a kind of polyurethane of high-strength and high ductility/fibrination functional configurations and remember high molecular preparation method.This method
（1）One cleaning ambient of development is friendly and variation route of simple and feasible cellulose homogeneous-phase functionalization, compared to traditional
Solvent reaction system, the grafting efficiency of cellulose greatly improved (2) by after functionalization cellulose and polyurethane with
And rhodamine carries out solution cast and prepares composite material, constructs the binary heterozygosis network based on cellulose primitive, prepares and have
The multi-functional shape memory high molecule material for taking into account temperature-responsive and ultraviolet light response of high intensity, high tenacity.Compared to pure
Polyurethane, the composite functional material tensile strength prepared increase 200%, and elongation at break increases 300%, and have and
Its quick temperature-responsive function and photoresponse function, shape memory response rate have reached 92%.
The technical solution used in the present invention is：A kind of polyurethane/fibrination functional configurations memory high molecular material
Preparation method includes the following steps
Step 1 using ultrasonic disperse obtains answering for clear after being mixed ion solvent, absolute ethyl alcohol and deionized water
Close solution；
Silane coupling agent is added into composite solution for step 2, and acetic acid is added dropwise and adjusts solution PH, and agitating solution makes silane coupled
Hydrolysis occurs for agent；
Microcrystalline cellulose is added into solution for step 3, is filtered using Buchner funnel after being sufficiently stirred；
Step 4 takes filter residue, and filter residue, which is placed in freeze drier, to be freeze-dried to obtain the microcrystalline cellulose of functionalization；
Microcrystalline cellulose and the stirring of functionalization are added into the mixed solution of polyurethane and N-Methyl pyrrolidone for step 5；
Rhodamine is added into solution and is reacted for step 6；
Step 7 will obtain dry polyurethane/fibrination functional configurations after the solvent volatilization in reaction solution and remember macromolecule material
Material.
Further, absolute ethyl alcohol and deionized water volume ratio are 2-3 ratios 1 in step 1.
Further, acetic acid is added dropwise in step 2 and adjusts PH=4-5.
Further, hydrolysis is carried out at 80 DEG C in step 2.
Further, polyurethane and N-Methyl pyrrolidone quality in polyurethane and N-Methyl pyrrolidone mixed solution
Than being 1:10.
Further, the additive amount of the microcrystalline cellulose of functionalization is the 5-10% of polyurethane quality
Further, the additive amount of rhodamine is the 5-20% of functional fiber quality amount
Further, the volatilization of solvent carries out at room temperature in step 7.
Advantageous effect caused by the present invention includes：The present invention be to microcrystalline cellulose carry out homogeneous reaction kinetic with
Regulate and control grafting efficiency, using cellulose after functionalization and the dual enhancing of rhodamine and polyurethane formation based on cellulose is added
The network of toughening is in particular in prepare multi-functional shape memory high molecule material
（1）The silanization grafting dicyandiamide solution for having invented a kind of clean microcrystalline cellulose of green, due to the presence of ion solvent,
The reaction that cellulose is homogeneously changed in the case of dissolving.Compared to the system of traditional second alcohol and water, more
Green and environment-friendly solvent it is recyclable, the pollution to environment can be reduced, meet the requirement of Green Sustainable, and grafting efficiency
It greatly improves.
（2）Pass through the shape memory high score prepared with polyurethane and rhodamine after the microcrystalline cellulose after silane-functionalized
The characteristics of sub- material is provided simultaneously with high intensity and high tenacity compared to pure polyurethane material, intensity are increased than pure polyurethane
200%, elongation at break increases 300%.Solve the contradiction of the strength of materials and toughness mutual exclusion, it is can coordinating and exist
Together.And the intellectual material with temperature and ultraviolet light double stimuli responsive is prepared, has been remembered by the shape of temperature manipulation
Recall function to be greatly improved, recovery of shape rate is up to 92%.The material can be applied to the temperature sensor strained greatly and
Aerospace field.
（3）The present invention has greatly widened the use scope of cellulose, the silanization degree shown by manipulating cellulose,
It is used as primitive by cellulose and forms dual-network structure so that cellulose can be as the dual of reinforcing agent and chemical cross-linking agent
Role develops an important function of cellulose, and opening one for the cellulose that industrially produces later new answers
Use direction.
Description of the drawings
Fig. 1 is the ultraviolet light response function and curve of polyurethane/cellulose composite material；
Fig. 2 is the scanning electron microscopic picture in the tension failure face of polyurethane/cellulose composite material.
Specific implementation mode
Further details of explanation is done to the present invention with reference to the accompanying drawings and detailed description, it should be appreciated that
Protection scope of the present invention is not restricted by specific implementation.
Example 1
（1）The homogeneous reaction kinetic of microcrystalline cellulose
A kind of double solvents that green is novel is configured first：Accurate weighing 19g 1- allyls, 3- methylimidazole villaumite class ions
Solvent, measures 10ml absolute ethyl alcohols and 5ml deionized waters are added in three-necked flask, clear using being obtained after ultrasonic disperse 10min
Clear bright composite solution.1g silane coupling agents are added, after acetic acid adjusting PH=4 are added dropwise, magnetic agitation 1h makes silane at 80 DEG C
Hydrolysis occurs for coupling agent.The microcrystalline cellulose for weighing 1g again is added in three-necked flask, after being persistently stirred to react 3 hours,
Washing being filtered using Buchner funnel after being cooled to room temperature and obtaining filter residue, so repeatedly washing is not reacted completely with removing
Silane coupling agent.Finally, functionalization is obtained after microcrystalline cellulose after reaction being carried out freeze-drying 48h using freeze drier
Microcrystalline cellulose.
（2）The preparation of high-intensity and high-tenacity polyurethane/fibrination functional configurations memory high molecular material
Polyurethane after taking 2g to dry is dissolved in 20g N-Methyl pyrrolidone solution, and room temperature magnetic agitation 6h obtains clear
Lysate after the microcrystalline cellulose of 0.1g functionalization is added after continue to stir 12h, be eventually adding after the rhodamine of 5mg using super
After sound dispensing machine disperses 30min, continue after 10h is stirred at room temperature, it, will be molten after reaction to prepare the membrane material of smooth rule
Liquid pours among the evaporating dish of polytetrafluoroethylene (PTFE), and room temperature obtains dry polyurethane/fibrination function after solvent volatilizees 1 week
Shape memory high molecule material
Example 2
（1）The homogeneous reaction kinetic of microcrystalline cellulose
The reaction kinetic of microcrystalline cellulose, accurate weighing 19g 1- allyls, 3- methylimidazole villaumite classes are carried out according to example 1
Ion solvent, measures 12.5ml absolute ethyl alcohols and 5ml deionized waters are added in three-necked flask, after ultrasonic disperse 10min
Obtain the composite solution of clear.1g silane coupling agents are added, after acetic acid adjusting PH=4.5 are added dropwise, the magnetic agitation at 80 DEG C
1h makes silane coupling agent that hydrolysis occur.The microcrystalline cellulose for weighing 1g again is added in three-necked flask, is persistently stirred to react 3
After hour, washing being filtered using Buchner funnel after being cooled to room temperature and obtaining filter residue, so repeatedly washing is not complete to remove
The silane coupling agent of full response.Finally, it is obtained after microcrystalline cellulose after reaction being carried out freeze-drying 48h using freeze drier
The microcrystalline cellulose of functionalization.
(2) preparation of high-intensity and high-tenacity polyurethane/fibrination functional configurations memory high molecular material
Polyurethane after taking 2g to dry is dissolved in 20g N-Methyl pyrrolidone solution, and room temperature magnetic agitation 6h obtains clear
Lysate after be added 0.15g functionalization microcrystalline cellulose after continue stir 12h, after being eventually adding the rhodamine of 18.75mg
After disperseing 30min using ultrasonic disperse machine, continues after 10h is stirred at room temperature, the solution after reaction is poured into polytetrafluoroethylene (PTFE)
Among evaporating dish, room temperature obtains dry polyurethane/fibrination functional configurations after solvent volatilizees 1 week and remembers macromolecule material
Material.
Example 3
（1）The homogeneous reaction kinetic of microcrystalline cellulose
The reaction kinetic of microcrystalline cellulose, accurate weighing 19g 1- allyls, 3- methylimidazole villaumite classes are carried out according to example 1
Ion solvent, measures 15ml absolute ethyl alcohols and 5ml deionized waters are added in three-necked flask, is obtained using after ultrasonic disperse 10min
To the composite solution of clear.1g silane coupling agents are added, after acetic acid adjusting PH=5 are added dropwise, magnetic agitation 1h makes at 80 DEG C
Hydrolysis occurs for silane coupling agent.The microcrystalline cellulose for weighing 1g again is added in three-necked flask, is persistently stirred to react 3 hours
Afterwards, washing being filtered using Buchner funnel after being cooled to room temperature and obtaining filter residue, so repeatedly washing is no completely anti-to remove
The silane coupling agent answered.Finally, function is obtained after microcrystalline cellulose after reaction being carried out freeze-drying 48h using freeze drier
The microcrystalline cellulose of change
（2）The preparation of high-intensity and high-tenacity polyurethane/fibrination functional configurations memory high molecular material
Polyurethane after taking 2g to dry is dissolved in 20g N-Methyl pyrrolidone solution, and room temperature magnetic agitation 6h obtains clear
Lysate after be added 0.2g functionalization microcrystalline cellulose after continue stir 12h, used after being eventually adding the rhodamine of 40mg
After ultrasonic disperse machine disperses 30min, continues after 10h is stirred at room temperature, the solution after reaction is poured into the evaporation of polytetrafluoroethylene (PTFE)
Among ware, room temperature obtains dry polyurethane/fibrination functional configurations after solvent volatilizees 1 week and remembers high molecular material.
The tensile property of polyurethane/cellulose composite material made from above-described embodiment is shown in Table 1, can obtain tensile strength and break
It splits rate elongation and obtains raising by a relatively large margin compared to memory high molecular material prepared by traditional polyurethane.
The tensile property of 1 polyurethane of table/cellulose composite material
| Sample | Tensile strength (MPa) | Elasticity modulus (MPa) | Elongation at break (%) |
| Pure polyurethane（Comparative sample） | 3.0±0.2 | 25.9±2.6 | 267.3±26.2 |
| Example 1 | 5.4±0.1 | 19.6±2.1 | 686.1±9.3 |
| Example 2 | 5.1±0.1 | 19.7±1.3 | 713.2±34.3 |
| Example 3 | 5.8±0.3 | 19.1±1.3 | 706.5±22.9 |
Fig. 1 is the ultraviolet light response function and curve of polyurethane/cellulose composite material；By Fig. 1, it can be seen that, for preparing is poly-
Urethane/cellulose has the function of excellent ultraviolet light response, and it is nothing that material dissolving, which is dispersed in N-Methyl pyrrolidone solution,
Color is transparent, is subsequently placed at after irradiating 30min under the ultraviolet light of 365nm, and solution becomes pink from transparent, and ultraviolet
Occurs the absorption peak of 530nm or so in absorption spectrum.It can be seen that as the irradiation time increases, absorption peak it is strong
Degree is remarkably reinforced.Color switchs to water white transparency by pink again after carrying out 80 DEG C of heating 10min to solution.Change solution can carry out it is more
Transformation of the water white transparency to pink colour again of color caused by ultraviolet irradiation-heating of secondary cycle.
Fig. 2 is the scanning electron microscopic picture in the tension failure face of polyurethane/cellulose composite material.As seen from the figure, Fig. 2 a are
The tension failure face of pure polyurethane material can clearly be observed that the irregular round abscess being interconnected by aperture
Structure, and be loose, soft surface.And the fracture of polyurethane/cellulose composite material is then to form three-dimensional friendship
Join dimensional network structure, and can see Fig. 2 b with the close interface cohesion formed between cellulose and matrix polyurethane.
The present invention builds reinforcement dual function of the cellulose as the crosslinking agent sum of dual network skeleton, the rhodamine of introducing
B serves not only as the switch of photosensitizer and is also a kind of structural motif of novel macromolecular toughening agent establishment dual-network structure
Distribution assigns the functional material of material high tenacity and high recovery rate and efficiency collection calorifics and optics multiple response, can be simultaneously
It realizes material high intensity and high tenacity and is effectively improved this of the recovery rate of composite material of shape memory and be difficult in the material
The contradiction coexisted, on the other hand also so that material has multiple response function.Not only overcome lacking for original shape memory function
Point, and substantially increase its physical and chemical performance is very big to have widened its application field, especially setting in big strain transducer
The resolving ideas of optimization is provided on meter, while also complying with the theory of contemporary green bio base sustainable development.
The preferred embodiment of the present invention is above are only, the present invention is not limited in the content of embodiment.For in this field
Technical staff for, can have various change and change within the scope of technical scheme of the present invention, made by it is any variation and
Change, within the scope of the present invention.
Claims (8)
1. a kind of preparation method of polyurethane/fibrination functional configurations memory high molecular material, it is characterised in that：Including following
Step
Step 1 using ultrasonic disperse obtains answering for clear after being mixed ion solvent, absolute ethyl alcohol and deionized water
Close solution；
Silane coupling agent is added into composite solution for step 2, and acetic acid is added dropwise and adjusts solution PH, and agitating solution makes silane coupled
Hydrolysis occurs for agent；
Microcrystalline cellulose is added into solution for step 3, is filtered using Buchner funnel after being sufficiently stirred；
Step 4 takes filter residue, and filter residue, which is placed in freeze drier, to be freeze-dried to obtain the microcrystalline cellulose of functionalization；
Microcrystalline cellulose and the stirring of functionalization are added into the mixed solution of polyurethane and N-Methyl pyrrolidone for step 5；
Rhodamine is added into solution and is reacted for step 6；
Step 7 will obtain dry polyurethane/fibrination functional configurations after the solvent volatilization in reaction solution and remember macromolecule material
Material.
2. the preparation method of polyurethane according to claim 1/fibrination functional configurations memory high molecular material, special
Sign is：Absolute ethyl alcohol and deionized water volume ratio are 2 to 1 in step 1.
3. the preparation method of polyurethane according to claim 1/fibrination functional configurations memory high molecular material, special
Sign is：Acetic acid is added dropwise in step 2 and adjusts PH=5.
4. the preparation method of polyurethane according to claim 1/fibrination functional configurations memory high molecular material, special
Sign is：Hydrolysis is carried out at 80 DEG C in step 2.
5. the preparation method of polyurethane according to claim 1/fibrination functional configurations memory high molecular material, special
Sign is：Polyurethane and N-Methyl pyrrolidone mass ratio are 1 in polyurethane and N-Methyl pyrrolidone mixed solution:10.
6. the preparation method of polyurethane according to claim 1/fibrination functional configurations memory high molecular material, special
Sign is：The additive amount of the microcrystalline cellulose of functionalization is the 5-10% of polyurethane quality.
7. the preparation method of polyurethane according to claim 1/fibrination functional configurations memory high molecular material, special
Sign is：The additive amount of rhodamine is the 5-20% of functional fiber quality amount.
8. the preparation method of polyurethane according to claim 1/fibrination functional configurations memory high molecular material, special
Sign is：The volatilization of solvent carries out at room temperature in step 7.
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| CN110204883A (en) * | 2019-05-22 | 2019-09-06 | 南京林业大学 | A kind of preparation method of the compound water-oil separating thermal insulation aeroge of polyurethane fiber element |
| CN112898636A (en) * | 2021-02-18 | 2021-06-04 | 陕西科技大学 | Preparation method of self-healing cellulose-based plastic |
| CN113061274A (en) * | 2021-03-17 | 2021-07-02 | 广东工业大学 | Multi-structure color-changing intelligent optical film driven by multi-shape memory and preparation method and application thereof |
| CN115785531A (en) * | 2022-09-20 | 2023-03-14 | 南京林业大学 | Functionalized microcrystalline cellulose-based double-network gel film and preparation method thereof |
| CN116284968A (en) * | 2023-03-24 | 2023-06-23 | 四川大学华西医院 | Solvent-free preparation of shape memory polyurethane/biomass fiber composite foam and method for regulating and controlling plantar pressure of shape memory polyurethane/biomass fiber composite foam |
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| CN110204883A (en) * | 2019-05-22 | 2019-09-06 | 南京林业大学 | A kind of preparation method of the compound water-oil separating thermal insulation aeroge of polyurethane fiber element |
| CN110204883B (en) * | 2019-05-22 | 2021-03-26 | 南京林业大学 | Preparation method of polyurethane cellulose composite oil-water separation thermal insulation aerogel |
| CN112898636A (en) * | 2021-02-18 | 2021-06-04 | 陕西科技大学 | Preparation method of self-healing cellulose-based plastic |
| CN112898636B (en) * | 2021-02-18 | 2022-02-18 | 陕西科技大学 | Preparation method of self-healing cellulose-based plastic |
| CN113061274A (en) * | 2021-03-17 | 2021-07-02 | 广东工业大学 | Multi-structure color-changing intelligent optical film driven by multi-shape memory and preparation method and application thereof |
| CN113061274B (en) * | 2021-03-17 | 2022-11-22 | 广东工业大学 | Multi-structure color-changing intelligent optical film driven by multi-shape memory and preparation method and application thereof |
| CN115785531A (en) * | 2022-09-20 | 2023-03-14 | 南京林业大学 | Functionalized microcrystalline cellulose-based double-network gel film and preparation method thereof |
| CN115785531B (en) * | 2022-09-20 | 2023-11-03 | 南京林业大学 | Functionalized microcrystalline cellulose-based double-network gel film and preparation method thereof |
| CN116284968A (en) * | 2023-03-24 | 2023-06-23 | 四川大学华西医院 | Solvent-free preparation of shape memory polyurethane/biomass fiber composite foam and method for regulating and controlling plantar pressure of shape memory polyurethane/biomass fiber composite foam |
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