CN110305483A - A kind of low density porous polymer material of flexibility, preparation method and its application as physical protection material - Google Patents
A kind of low density porous polymer material of flexibility, preparation method and its application as physical protection material Download PDFInfo
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Abstract
The invention discloses a kind of low density porous polymer material of flexibility, preparation method and its applications as physical protection material, belong to the technical field of porous polymer material.A kind of preparation method of the low density porous polymer material of flexibility, the following steps are included: 1) stabilizer is added in oil-based system, stirring forms mixed solution, the mixed solution is added in water phase, stirring forms the glutinous lotion for playing state, white, it is static to be microfluidic to lotion or partly flow shape, gel emulsion is made；2) gel emulsion is subjected to thermal polymerization, flexible low density porous polymer material is obtained after dry；The preparation method is environmentally protective, simple process, solves the problems, such as venomous injurant release in the prior art；The low density porous polymer material of flexibility of this method preparation has many advantages, such as lightweight, porous, flexible, hydrophobic, high temperature resistant, nontoxic, controllable, reusable without skin irritatin, cost；The polymer material is as physical protection material application, and excellent combination property, cost are controllable, competitiveness is strong.
Description
Technical field
The invention belongs to the technical fields of porous polymer material, and in particular to a kind of low density porous polymeric material of flexibility
Material, preparation method and its application as physical protection material.
Background technique
Environment is space for the survival of mankind, it not only includes natural environment and daily life, study, working environment,
It further include the science configuration and use of the modern life, workplace fixture.Lasting, stable, the good development of environment for human survival is people
The basis of class health, with the development of technology and the improvement of people ' s living standards, the numerous environmental problems occurred in life are to people
The influence of body health is also increasingly severe, contaminated air, the noise to sound in one's ear, particular job occasion generate dust,
The toxic and harmful gas etc. that adverse circumstances generate all is the formidable enemy of human health, develops a kind of flexible light weight, wearing comfort, without skin
Skin stimulation, reusable, environmental-friendly, multi-functional physical protection material is extremely important.
Physical protection material refer to make in life, production or the course of work personnel mitigate or from injury, accident and
Occupational hazards and a kind of complementary prevention & protection articles provided, such as: avoid particulate matter, dust, bacterium and pernicious gas
Intake, protects the mask of respiratory system；Prevent noise from causing hearing impaired earplug or earmuff；Defend poisonous and harmful chemicals,
Particulate matter and the spraying equal biochemical defence suit for damaging skin；Warm-up with particular job environment such as heat-insulated, heat preservation and water-proof function
Belong to physical protection material.Mask, high-elastic silica gel, bubble is made using smelting and spray macromolecule fiber in common physical protection material
Earplug is made in foam, polyester material etc., and bright and beautiful silk cloth+dual coating flame-proof PVC/coating butyl rubber/neoprene-coating is contour
Protective garment is made in molecular material, can have both multiple functions now on the market almost without a kind of material, is used for physical protection material
Material field.
Chinese patent literature CN105085787A discloses the compressible low density porous polymer material of one kind and its preparation
Method, but the raw material of its preparation process selection includes styrene, divinylbenzene, methyl methacrylate, acrylonitrile or methyl
The polymerisable monomers such as tert-butyl acrylate, these monomers can discharge poisonous and hazardous VOCs in production and use process, and most
Final polymerization object material may include a small amount of residual solvent, can also discharge poisonous and hazardous VOCs in use process, be not suitable for using
In physical protection Material Field；And core material dimethyl silicone polymer is expensive in the patent document, causes to prepare porous
The higher cost of polymer material, thus above-mentioned compressible low density porous polymer material physical protection field apply by
Limit；In addition, the gel emulsion formula enlarge-effect of the patent document is larger, compares and be difficult to realize extensive steady production, this is
Since polymerization system includes polymerisable monomer and crosslinking agent curing cross-linking reaction, two kinds of dimethyl silicone polymer two-component heat cure
Different reaction types, the polymerization temperature and rate of polymerization of both reactions are different, therefore temperature is not when being mass produced
The uncontrollability of uniformity and reaction rate makes gel emulsion the problems such as a small amount of split-phase, demulsification, water outlet easily occur.
Summary of the invention
It is an object of the invention to overcome the above-mentioned prior art, a kind of low density porous polymeric material of flexibility is provided
Material, preparation method and its application as physical protection material.
In order to achieve the above objectives, the present invention is achieved by the following scheme:
A kind of preparation method of the low density porous polymer material of flexibility, comprising the following steps:
1) gel emulsion is prepared
Stabilizer is added in oil-based system, stirring forms mixed solution, and the mixed solution is added in water phase, stirs shape
It is static to be microfluidic to lotion or partly flow shape at white emulsion, gel emulsion is made；
By percentage to the quality, it the ratio of each component is: 0.1%~0.5% stabilizer, 15%~45% oily phase,
60%~80% water phase；Wherein, oil mutually by 5%~15% silane coupling agent, 5%~20% toughener and 5%~
10% diluent mixes；
Stabilizer is
2) the flexible low density porous polymer material of preparation
By the gel emulsion in room temperature~50 DEG C, it polymerize 2~4h, temperature is risen to 50~90 DEG C, polymerize 4~12h, most
Temperature is warming up to 90~120 DEG C afterwards, polymerize 2~4h, is dried to obtain flexible low density porous polymer material later.
Further, the silane coupling agent in step 1) is methyltrimethoxysilane, methyltriethoxysilane, ethyl
One of trimethoxy silane, ethyl triethoxysilane, vinyltrimethoxysilane or vinyltriethoxysilane
Or it is a variety of.
Further, the toughener in step 1) is in nitrile rubber, acrylic rubber, polyurethane or polysiloxanes
It is one or more.
Further, the diluent in step 1) is one of n-hexane, hexamethylene, normal heptane, ethyl alcohol or isopropanol
Or it is a variety of.
A kind of preparation method using the above-mentioned low density porous polymer material of flexibility is prepared flexible low density porous
Polymer material.
Further, the density of the polymer material is 0.20~0.40g/cm3, pore size is 10~100 μm, minimum
200 DEG C of thermal decomposition temperature >, no skin irritation is reacted.
A kind of application of the low density porous polymer material of flexibility as physical protection material.
Compared with prior art, the invention has the following advantages:
The preparation method of the low density porous polymer material of flexibility of the invention, the stabilizer used are that laboratory synthesizes certainly
Small molecule gelling agent, different from the conventional stabilizers such as surfactant, solid micro-/ nano particle, small molecule gelling agent relies on
Itself weak interaction, associates to form three-dimensional net structure by supermolecule, which lose the solvent being contained therein
Mobility is gone, to achieve the effect that form gel emulsion, it is big, continuous to solve stabilizing agent dosage existing for conventional gel lotion
Mutually it is prone to phase reversal with dispersed phase, and is used for the problems such as aftertreatment technology is complicated, energy consumption is high when templated synthesis；The flexibility
The preparation method of low density porous polymer material uses " synthesis+assembling " theory, the small molecule gelling agent formulated with laboratory
, by simple physical agitation/concussion plastic, make continuous phase package point using Water-In-Oil (W/O) type lotion as template for stabilizer
Dephasing prepares the gel emulsion of milky, viscoelastic state, by ageing, hydrolysis, condensation, is crosslinked, is dried to obtain.With conventional gel cream
The liquid phase of liquid/liquid phase structure is different, and the gel emulsion based on small molecule gelling agent is gel/liquid phase or gel/gel rubber system, from
And limit gel emulsion dispersed phase volume fraction no longer by being greater than 74%, gel emulsion is realized from concept to content with this
Total innovation；On the other hand, poisonous and hazardous VOCs will not be discharged in preparation process, process is environmentally protective；Prepare raw material valence
Lattice are cheap, concise in technology, and production cost is low；Preparation step is simple, and reaction condition is mild, with short production cycle；Expanded scope production
Affected by environment smaller, large-scale production stability is ensured.
The low density porous polymer material of flexibility of the invention, have lightweight, it is porous, flexible, nontoxic, pierced without skin
Sharp, at low cost, the production advantages such as environmentally protective, reusable.
The application of the low density porous polymer material of flexibility of the invention as physical protection material, restoring force is good, is not easy
Fold is generated, can be repeatedly used；Density of material is low, dresses light；Material has hydrophobicity, can keep physical protection material
Drying；To no skin irritation, guarantee the safety of wearer；Cost is controllable, function admirable, the similar product in market
In have very strong competitiveness.
Detailed description of the invention
Fig. 1 is compound ii/oil phase/aqueous systems gel emulsion photo of different moisture content, wherein (a) is 60% aqueous
The gel emulsion photo of amount is (b) the gel emulsion photo of 70% water content, (c) is the gel emulsion photo of 80% water content；
Fig. 2 is the appearance photo of material after compound ii/oil phase/aqueous systems of different moisture content polymerize, wherein (d) is
Material photo after the gel emulsion polymerization of 60% water content is (e) material photo after the gel emulsion polymerization of 70% water content,
It (f) is material photo after the gel emulsion polymerization of 80% water content；
Fig. 3 is the low density porous polymer material SEM photograph of flexibility of different moisture content, wherein (a), (b), (c) are respectively
For the SEM photograph of 80%, 70%, 60% material of water content, (a '), (b '), (c ') are respectively that the amplification of (a), (b), (c) are shone
Piece；
Fig. 4 be the low density porous polymer material of flexibility of 80% water content compress-spring back photo, wherein (a) is compression
Photo is (b) rebound photo；
Load-deformation curve when Fig. 5 is the flexible low density porous polymer material compression of 80% water content；
Fig. 6 is the low density porous polymer material water contact angle test chart of flexibility of different moisture content, wherein should in (a)
Material moisture content is 60%, (b) in the material moisture content be 70%, (c) in the material moisture content be 80%；
Fig. 7 is the low density porous polymer material TGA curve of flexibility of 80% water content；
Fig. 8 is the low density porous polymer material organic volatile residual volume test result of flexibility of 80% water content；
Fig. 9 is the low density porous polymer material PARA FORMALDEHYDE PRILLS(91,95) of flexibility and banana oil absorption property curve of 80% water content.
Wherein, above-mentioned 60%, 70%, 80% is mass percent；Above-mentioned 60%, 70%, the flexibility of 80% water content
Low density porous polymer material is prepared by embodiment 6, embodiment 5 and embodiment 1 respectively.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, below in conjunction in the embodiment of the present invention
Attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is only this
The embodiment of a part is invented, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without making creative work, should fall within the scope of the present invention.
It should be noted that description and claims of this specification and term " first " in above-mentioned attached drawing, "
Two " etc. be to be used to distinguish similar objects, without being used to describe a particular order or precedence order.It should be understood that using in this way
Data be interchangeable under appropriate circumstances, so as to the embodiment of the present invention described herein can in addition to illustrating herein or
Sequence other than those of description is implemented.In addition, term " includes " and " having " and their any deformation, it is intended that cover
Cover it is non-exclusive include, for example, the process, method, system, product or equipment for containing a series of steps or units are not necessarily limited to
Step or unit those of is clearly listed, but may include be not clearly listed or for these process, methods, product
Or other step or units that equipment is intrinsic.
The invention will be described in further detail with reference to the accompanying drawing:
Embodiment 1
1) preparation of gel emulsion
By percentage to the quality, it the ratio of each component is: compound ii 0.1%, oily phase 19.9%, water phase 80%；Wherein,
Oil phase component are as follows: methyltrimethoxysilane 5%, nitrile rubber 9.9%, n-hexane 5%；
Under room temperature, oil-based system is stirred into 10~20min, the compound ii as stabilizer is dissolved in oily phase body
System, concussion/stirring form uniform mixed solution, water phase are rapidly joined, concussion/10~30min of stirring, formation milky,
The lotion of viscoelastic state, it is static to flow shape at microfluidic/half to system, gel emulsion is made；
2) the flexible low density porous polymer material of preparation
The gel emulsion prepared is aged 10~30min at room temperature, is put into oil bath and polymerize.Polymerizing condition are as follows: room
Temperature polymerization 4h, is warming up to 60 DEG C of polymerization 12h, then be warming up to 90 DEG C of polymerization 4h, after the completion of polymerization, system is down to room temperature naturally；Material
Material is dry in 50 DEG C of baking ovens after taking out, and obtains soft, lightweight low density porous material, density 0.20g/cm3, pore size
It is 10~100 μm.
In embodiment 1 compound ii the preparation method is as follows:
Synthesize chemical compounds I
0.1mol cholesterol and 0.1molBoc-D- phenylalanine are dissolved in 250mL methylene chloride, stirred under ice-water bath
It makes it dissolve, 0.1mol DCC and 0.01mol DMAP is then added, mixed solution ice-water bath reacts 2h, then reacts at room temperature
Gained mixture is filtered, obtains pale yellow filtrate by 16h；Filtrate is passed through dry HCl gas under agitation, until body
System stops ventilation, filters, vacuum drying obtains powdered compounds I, reaction equation is as follows there is no when white precipitate generation:
Synthesize compound ii
0.1mol chemical compounds I is dissolved in 200mL benzene, 0.1mol triethylamine is added, is heated to reflux 2h, is cooled to room temperature；
It will be instilled dissolved with the 100mL benzole soln of 0.1mol succinic anhydride by constant pressure funnel with the speed of (1~2) drop/sec above-mentioned
In mixed solution, it is heated to reflux stirring 10h after being added dropwise completely, filters, vacuum drying obtains white powder compound ii, instead
Answer formula as follows:
Embodiment 2
1) preparation of gel emulsion
By percentage to the quality, it the ratio of each component is: compound ii 0.1%, oily phase 19.9%, water phase 80%；Wherein,
Oil phase component are as follows: ethyl trimethoxy silane 8%, nitrile rubber 6.9%, n-hexane 5%；
Under room temperature, oil-based system is stirred into 10~20min, stabilizer compounds II is dissolved in oil-based system, shake/
Stirring forms uniform mixed solution, water phase is rapidly joined, concussion/10~30min of stirring, forms milky, viscoelastic state
Lotion, it is static to flow shape at microfluidic/half to system, gel emulsion is made；
2) the flexible low density porous polymer material of preparation
The gel emulsion prepared is aged 10~30min at room temperature, is put into oil bath and polymerize.Polymerizing condition are as follows: room
Temperature polymerization 4h, is warming up to 60 DEG C of polymerization 12h, then be warming up to 90 DEG C of polymerization 4h, after the completion of to be polymerized, system is down to room temperature naturally；
Material is dry in 50 DEG C of baking ovens after taking out, and obtains soft, lightweight low density porous material, density 0.20g/cm3, hole ruler
Very little is 10~100 μm.
In embodiment 2 compound ii the preparation method is as follows:
Synthesize chemical compounds I
0.1mol cholesterol and 0.1molBoc-D- phenylalanine are dissolved in 250mL methylene chloride, stirred under ice-water bath
It makes it dissolve, 0.1mol DCC and 0.01mol DMAP is then added, mixed solution ice-water bath reacts 2h, then reacts at room temperature
Gained mixture is filtered, obtains pale yellow filtrate by 16h；Filtrate is passed through dry HCl gas under agitation, until body
System stops ventilation, filters, vacuum drying obtains powdered compounds I there is no when white precipitate generation.
Synthesize compound ii
0.1mol chemical compounds I is dissolved in 200mL benzene, 0.1mol triethylamine is added, is heated to reflux 2h, is cooled to room temperature；
It will be instilled dissolved with the 100mL benzole soln of 0.1mol succinic anhydride by constant pressure funnel with the speed of (1~2) drop/sec above-mentioned
In mixed solution, it is heated to reflux stirring 10h after being added dropwise completely, filters, vacuum drying obtains white powder compound ii.
Embodiment 3
1) gel emulsion is prepared
By percentage to the quality, it the ratio of each component is: compound ii 0.1%, oily phase 19.9%, water phase 80%；Wherein,
Oil phase component are as follows: vinyltrimethoxysilane 7%, nitrile rubber 5%, n-hexane 7.9%；
Under room temperature, oil-based system is stirred into 10~20min, stabilizer compounds II is dissolved in oil-based system, shake/
Stirring forms uniform mixed solution, water phase is rapidly joined, concussion/10~30min of stirring, forms milky, viscoelastic state
Lotion, it is static to flow shape at microfluidic/half to system, gel emulsion is made.
2) the flexible low density porous polymer material of preparation
The gel emulsion prepared is aged 10~30min at room temperature, is put into oil bath and polymerize.Polymerizing condition are as follows: room
Temperature polymerization 4h, is warming up to 60 DEG C of polymerization 12h, then be warming up to 90 DEG C of polymerization 4h, after polymerization, system is down to room temperature naturally；It will
Material takes out the drying in 50 DEG C of baking ovens, obtains soft, lightweight low density porous material, density 0.20g/cm3, pore size
It is 10~100 μm.
The synthetic method of compound ii is as follows in embodiment 3:
Synthesize chemical compounds I
0.1mol cholesterol and 0.1molBoc-D- phenylalanine are dissolved in 250mL methylene chloride, stirred under ice-water bath
It makes it dissolve, 0.1mol DCC and 0.01mol DMAP is then added, mixed solution ice-water bath reacts 2h, then reacts at room temperature
Gained mixture is filtered, obtains pale yellow filtrate by 16h；Filtrate is passed through dry HCl gas under agitation, until body
System stops ventilation, filters, vacuum drying obtains powdered compounds I there is no when white precipitate generation.
Synthesize compound ii
0.1mol chemical compounds I is dissolved in 200mL benzene, 0.1mol triethylamine is added, is heated to reflux 2h, is cooled to room temperature；
It will be instilled dissolved with the 100mL benzole soln of 0.1mol succinic anhydride by constant pressure funnel with the speed of (1~2) drop/sec above-mentioned
In mixed solution, it is heated to reflux stirring 10h after being added dropwise completely, filters, vacuum drying obtains white powder compound ii.
Embodiment 4
1) gel emulsion is prepared
By percentage to the quality, it the ratio of each component is: compound ii 0.3%, oily phase 29.7%, water phase 70%；Wherein,
Oil phase component are as follows: ethyl trimethoxy silane 15%, acrylic rubber 6.7%, normal heptane 8%；
Under room temperature, oil-based system is stirred into 10~20min, stabilizer compounds II is dissolved in oil-based system, shake/
Stirring forms uniform mixed solution, water phase is rapidly joined, concussion/10~30min of stirring, forms milky, viscoelastic state cream
Liquid, it is static to flow shape at microfluidic/half to system, gel emulsion is made；
2) the flexible low density porous polymer material of preparation
The gel emulsion prepared is aged 10~30min at room temperature, is put into oil bath and polymerize.Polymerizing condition are as follows: rise
Temperature is warming up to 80 DEG C of polymerization 10h to 40 DEG C of polyase 13 h, then is warming up to 100 DEG C of polyase 13 h, and after completing polymerization, system is down to naturally
Room temperature；Material is dry in 50 DEG C of baking ovens after taking out, and obtains soft, lightweight low density porous material, density 0.30g/
cm3, pore size is 10~100 μm.
The synthetic method of compound ii is as follows in embodiment 4:
Synthesize chemical compounds I
0.1mol cholesterol and 0.2molBoc-D- phenylalanine are dissolved in 250mL methylene chloride, stirred under ice-water bath
It makes it dissolve, 0.2mol DCC and 0.04mol DMAP is then added, mixed solution ice-water bath reacts 4h, then reacts at room temperature
Gained mixture is filtered, obtains pale yellow filtrate by 20h；Filtrate is passed through dry HCl gas under agitation, until body
System stops ventilation, filters, vacuum drying obtains powdered compounds I there is no when white precipitate generation；
Synthesize compound ii
0.1mol chemical compounds I is dissolved in 200mL benzene, 0.2mol triethylamine is added, is heated to reflux 4h, is cooled to room temperature；
It will be instilled dissolved with the 100mL benzole soln of 0.2mol succinic anhydride by constant pressure funnel with the speed of (1~2) drop/sec above-mentioned
In mixed solution, it is heated to reflux stirring 15h after being added dropwise completely, filters, vacuum drying obtains white powder compound ii.
Embodiment 5
1) gel emulsion is prepared
By percentage to the quality, it the ratio of each component is: compound ii 0.3%, oily phase 29.7%, water phase 70%；Wherein,
Oil phase component are as follows: ethyl trimethoxy silane 15%, acrylic rubber 6.7%, normal heptane 8%；
Under room temperature, oil-based system is stirred into 10~20min, stabilizer compounds II is dissolved in oil-based system, shake/
Stirring forms uniform mixed solution, water phase is rapidly joined, concussion/10~30min of stirring, forms milky, viscoelastic state cream
Liquid, it is static to flow shape at microfluidic/half to system, gel emulsion is made.
2) the flexible low density porous polymer material of preparation
The gel emulsion prepared is aged 10~30min at room temperature, is put into oil bath and polymerize.Polymerizing condition are as follows: rise
Temperature is warming up to 80 DEG C of polymerization 10h to 40 DEG C of polyase 13 h, then is warming up to 100 DEG C of polyase 13 h, and after completing polymerization, system is down to naturally
Room temperature；Material is dry in 50 DEG C of baking ovens after taking out, and obtains soft, lightweight low density porous material, density 0.30g/
cm3, pore size is 10~100 μm.
The synthetic method of compound ii is as follows in embodiment 5:
Synthesize chemical compounds I
0.1mol cholesterol and 0.2molBoc-D- phenylalanine are dissolved in 250mL methylene chloride, stirred under ice-water bath
It makes it dissolve, 0.2mol DCC and 0.04mol DMAP is then added, mixed solution ice-water bath reacts 4h, then reacts at room temperature
Gained mixture is filtered, obtains pale yellow filtrate by 20h；Filtrate is passed through dry HCl gas under agitation, until body
System stops ventilation, filters, vacuum drying obtains powdered compounds I there is no when white precipitate generation.
Synthesize compound ii
0.1mol chemical compounds I is dissolved in 200mL benzene, 0.2mol triethylamine is added, is heated to reflux 4h, is cooled to room temperature；
It will be instilled dissolved with the 100mL benzole soln of 0.2mol succinic anhydride by constant pressure funnel with the speed of (1~2) drop/sec above-mentioned
In mixed solution, it is heated to reflux stirring 15h after being added dropwise completely, filters, vacuum drying obtains white powder compound ii.
Embodiment 6
1) gel emulsion is prepared
By percentage to the quality, it the ratio of each component is: compound ii 0.5%, oily phase 39.5%, water phase 60%；Wherein,
Oil phase component are as follows: vinyltrimethoxysilane 15%, polyurethane 14.5%, isopropanol 10%；
Under room temperature, oil-based system is stirred into 10~20min, stabilizer compounds II is dissolved in oil-based system, shake/
Stirring forms uniform mixed solution, water phase is rapidly joined, concussion/10~30min of stirring, forms milky, viscoelastic state
Lotion, it is static to flow shape at microfluidic/half to system, gel emulsion is made.
2) the flexible low density porous polymer material of preparation
The gel emulsion prepared is aged 10~30min at room temperature, is put into oil bath and polymerize.Polymerizing condition are as follows: rise
Temperature is warming up to 90 DEG C of polymerization 8h to 50 DEG C of polymerization 2h, then is warming up to 120 DEG C of polymerization 2h, and after completing polymerization, system is down to room naturally
Temperature；Material is dry in 50 DEG C of baking ovens after taking out, and obtains soft, lightweight low density porous material, density 0.40g/cm3,
Pore size is 10~100 μm.
The synthetic method of compound ii is as follows in embodiment 6:
Synthesize chemical compounds I
0.1mol cholesterol and 0.3molBoc-D- phenylalanine are dissolved in 250mL methylene chloride, stirred under ice-water bath
It makes it dissolve, 0.6mol DCC and 0.08mol DMAP is then added, mixed solution ice-water bath reacts 6h, then reacts at room temperature
For 24 hours, gained mixture is filtered, obtains pale yellow filtrate；Filtrate is passed through dry HCl gas under agitation, until body
System stops ventilation, filters, vacuum drying obtains powdered compounds I there is no when white precipitate generation.
Synthesize compound ii
0.1mol chemical compounds I is dissolved in 200mL benzene, 0.4mol triethylamine is added, is heated to reflux 6h, is cooled to room temperature；
It will be instilled dissolved with the 100mL benzole soln of 0.4mol succinic anhydride by constant pressure funnel with the speed of (1~2) drop/sec above-mentioned
In mixed solution, it is heated to reflux stirring 20h after being added dropwise completely, filters, vacuum drying obtains white powder compound ii.
Embodiment 7
1) gel emulsion is prepared
By percentage to the quality, it the ratio of each component is: compound ii 0.2%, oily phase 19.8%, water phase 80%, wherein
Oil phase component are as follows: methyltrimethoxysilane 2%, ethyl trimethoxy silane 3%, nitrile rubber 4.8%, acrylic rubber
5%, n-hexane 2% and hexamethylene 3%；
Under room temperature, oil-based system is stirred into 10~20min, stabilizer compounds II is dissolved in oil-based system, shake/
Stirring forms uniform mixed solution, water phase is rapidly joined, concussion/10~30min of stirring, forms milky, viscoelastic state
Lotion, it is static to flow shape at microfluidic/half to system, gel emulsion is made.
2) the flexible low density porous polymer material of preparation
The gel emulsion prepared is aged 10~30min at room temperature, is put into oil bath and polymerize.Polymerizing condition are as follows: room
Temperature polymerization 4h, is warming up to 60 DEG C of polymerization 12h, then be warming up to 90 DEG C of polymerization 4h, after the completion of to be polymerized, system is down to room temperature naturally；
Material is dry in 50 DEG C of baking ovens after taking out, and obtains soft, lightweight low density porous material, density 0.20g/cm3, hole ruler
Very little is 10~100 μm.
The synthetic method of compound ii is as follows in embodiment 7:
Synthesize chemical compounds I
0.1mol cholesterol and 0.5molBoc-D- phenylalanine are dissolved in 250mL methylene chloride, stirred under ice-water bath
It makes it dissolve, 0.8mol DCC and 0.1mol DMAP is then added, mixed solution ice-water bath reacts 8h, then reacts at room temperature
For 24 hours, gained mixture is filtered, obtains pale yellow filtrate；Filtrate is passed through dry HCl gas under agitation, until body
System stops ventilation, filters, vacuum drying obtains powdered compounds I there is no when white precipitate generation.
Synthesize compound ii
0.1mol chemical compounds I is dissolved in 200mL benzene, 0.5mol triethylamine is added, is heated to reflux 8h, is cooled to room temperature；
It will be instilled dissolved with the 100mL benzole soln of 0.5mol succinic anhydride by constant pressure funnel with the speed of (1~2) drop/sec above-mentioned
In mixed solution, it is heated to reflux stirring after being added dropwise completely for 24 hours, filters, vacuum drying obtains white powder compound ii.
Embodiment 8
1) gel emulsion is prepared
By percentage to the quality, it the ratio of each component is: compound ii 0.3%, oily phase 29.7%, water phase 70%；Wherein,
Oil phase component are as follows: methyltriethoxysilane 5%, ethyl triethoxysilane 10%, nitrile rubber 3.7%, polyurethane 3%,
Hexamethylene 3% and normal heptane 5%；
Under room temperature, oil-based system is stirred into 10~20min, stabilizer compounds II is dissolved in oil-based system, shake/
Stirring forms uniform mixed solution, water phase is rapidly joined, concussion/10~30min of stirring, forms milky, viscoelastic state cream
Liquid, it is static to flow shape at microfluidic/half to system, gel emulsion is made.
2) the flexible low density porous polymer material of preparation
The gel emulsion prepared is aged 10~30min at room temperature, is put into oil bath and polymerize.Polymerizing condition are as follows: rise
Temperature is warming up to 80 DEG C of polymerization 10h to 40 DEG C of polyase 13 h, then is warming up to 100 DEG C of polyase 13 h, after the completion of to be polymerized, by system nature
It is down to room temperature；Material is dry in 50 DEG C of baking ovens after taking out, and obtains soft, lightweight low density porous material, and density is
0.30g/cm3, pore size is 10~100 μm.
The synthetic method of compound ii is as follows in embodiment 8:
Synthesize chemical compounds I
0.1mol cholesterol and 0.2molBoc-D- phenylalanine are dissolved in 250mL methylene chloride, stirred under ice-water bath
It makes it dissolve, 0.2mol DCC and 0.04mol DMAP is then added, mixed solution ice-water bath reacts 4h, then reacts at room temperature
Gained mixture is filtered, obtains pale yellow filtrate by 20h；Filtrate is passed through dry HCl gas under agitation, until body
System stops ventilation, filters, vacuum drying obtains powdered compounds I there is no when white precipitate generation.
Synthesize compound ii
0.1mol chemical compounds I is dissolved in 200mL benzene, 0.2mol triethylamine is added, is heated to reflux 4h, is cooled to room temperature；
It will be instilled dissolved with the 100mL benzole soln of 0.2mol succinic anhydride by constant pressure funnel with the speed of (1~2) drop/sec above-mentioned
In mixed solution, it is heated to reflux stirring 15h after being added dropwise completely, filters, vacuum drying obtains white powder compound ii.
Embodiment 9
1) gel emulsion is prepared
By percentage to the quality, it the ratio of each component is: compound ii 0.5%, oily phase 39.5%, water phase 60%；Wherein,
Oil phase component are as follows: methyltriethoxysilane 4%, ethyl triethoxysilane 6%, vinyltriethoxysilane 5%, butyronitrile
Rubber 9%, polysiloxanes 5.5%, normal heptane 6% and isopropanol 4%；
Under room temperature, oil-based system is stirred into 10~20min, stabilizer compounds II is dissolved in oil-based system, shake/
Stirring forms uniform mixed solution, water phase is rapidly joined, concussion/10~30min of stirring, forms milky, viscoelastic state
Lotion, it is static to flow shape at microfluidic/half to system, gel emulsion is made；
2) the flexible low density porous polymer material of preparation
The gel emulsion prepared is aged 10~30min at room temperature, is put into oil bath and polymerize.Polymerizing condition are as follows: rise
Temperature is warming up to 90 DEG C of polymerization 8h to 50 DEG C of polymerization 2h, then is warming up to 120 DEG C of polymerization 2h, after completing polymerization, is down to naturally to system
Room temperature；It is dry in 50 DEG C of baking ovens after taking-up material, obtain soft, lightweight low density porous material, density 0.40g/
cm3, pore size is 10~100 μm.
The synthetic method of compound ii is as follows in embodiment 9:
Synthesize chemical compounds I
0.1mol cholesterol and 0.3molBoc-D- phenylalanine are dissolved in 250mL methylene chloride, stirred under ice-water bath
It makes it dissolve, 0.6mol DCC and 0.08mol DMAP is then added, mixed solution ice-water bath reacts 6h, then reacts at room temperature
Gained mixture is filtered, obtains pale yellow filtrate by 20h；Filtrate is passed through dry HCl gas under agitation, until body
System stops ventilation, filters, vacuum drying obtains powdered compounds I there is no when white precipitate generation.
Synthesize compound ii
0.1mol chemical compounds I is dissolved in 200mL benzene, 0.4mol triethylamine is added, is heated to reflux 6h, is cooled to room temperature；
It will be instilled dissolved with the 100mL benzole soln of 0.4mol succinic anhydride by constant pressure funnel with the speed of (1~2) drop/sec above-mentioned
In mixed solution, it is heated to reflux stirring 20h after being added dropwise completely, filters, vacuum drying obtains white powder compound ii.
Embodiment 10
1) gel emulsion is prepared
By percentage to the quality, it the ratio of each component is: compound ii 0.5%, oily phase 39.5%, water phase 60%, wherein
Oil phase component are as follows: methyltrimethoxysilane 5%, methyltriethoxysilane 7%, vinyltriethoxysilane 3%, poly- ammonia
Ester 8%, polysiloxanes 6.5%, normal heptane 5%, ethyl alcohol 5%；
Under room temperature, oil-based system is stirred into 10~20min, stabilizer compounds II is dissolved in oil-based system, shake/
Stirring forms uniform mixed solution, water phase is rapidly joined, concussion/10~30min of stirring, forms milky, viscoelastic state
Lotion, it is static to flow shape at microfluidic/half to system, gel emulsion is made.
2) the flexible low density porous polymer material of preparation
The gel emulsion prepared is aged 10~30min at room temperature, is put into oil bath and polymerize.Polymerizing condition are as follows: rise
Temperature is warming up to 90 DEG C of polymerization 8h to 50 DEG C of polymerization 2h, then is warming up to 120 DEG C of polymerization 2h, and after the completion of polymerization, system is down to room naturally
Temperature；Material is dry in 50 DEG C of baking ovens after taking out, and obtains soft, lightweight low density porous material, density 0.40g/cm3,
Pore size is 10~100 μm.
The synthetic method of compound ii is as follows in embodiment 10:
Synthesize chemical compounds I
0.1mol cholesterol and 0.3molBoc-D- phenylalanine are dissolved in 250mL methylene chloride, stirred under ice-water bath
It makes it dissolve, 0.6mol DCC and 0.08mol DMAP is then added, mixed solution ice-water bath reacts 6h, then reacts at room temperature
Gained mixture is filtered, obtains pale yellow filtrate by 20h；Filtrate is passed through dry HCl gas under agitation, until body
System stops ventilation, filters, vacuum drying obtains powdered compounds I there is no when white precipitate generation.
Synthesize compound ii
0.1mol chemical compounds I is dissolved in 200mL benzene, 0.4mol triethylamine is added, is heated to reflux 6h, is cooled to room temperature；
It will be instilled dissolved with the 100mL benzole soln of 0.4mol succinic anhydride by constant pressure funnel with the speed of (1~2) drop/sec above-mentioned
In mixed solution, it is heated to reflux stirring 20h after being added dropwise completely, filters, vacuum drying obtains white powder compound ii.
It is the gel emulsion photo of 60% water content referring to Fig. 1, (a), (b) is the gel emulsion photo of 70% water content,
It (c) is the gel emulsion photo of 80% water content, as seen from the figure, it is one that the gel emulsion inversion being prepared, which is not flowed,
Uniform and stable, the preferable white emulsion of viscoplasticity of kind, illustrates that 60%~80% water content can prepare the gel haveing excellent performance
Lotion.
Referring to fig. 2, (d) is the photo of material after the gel emulsion polymerization of 60% water content in Fig. 2, (e) is 70% aqueous
The photo of material after the gel emulsion polymerization of amount is (f) photo of material after the gel emulsion polymerization of 80% water content, You Tuke
, the porous polymer material of preparation is uniformly complete, excellent without fault of construction, overall performance, illustrate 60%~80% it is aqueous
Amount can prepare flexible low density porous polymer material.
Referring to Fig. 3, (a), (b), (c) in Fig. 3 are respectively that the flexibility of water content 80%, 70%, 60% is low density porous
The SEM photograph of polymer material, wherein (a ')~(c ') is respectively the corresponding enlarged photograph of (a)~(c).Using Quanta200
Scanning electron microscope carries out microstructure observing, and sample test front surface need to carry out metal spraying processing, and SEM test acceleration voltage is
20kV, emission current are 100 μ A.It can be obtained from the figure that: the flexible low-density polymeric materials of preparation have hierarchical porous structure abundant,
Pore size is 10~100 μm, and with the reduction of water content, the pore structure of polymer material is gradually become smaller, this is because this hair
It is bright using the small molecule gelling agent of preparation as stabilizer, using Water-In-Oil (W/O) type lotion as template, make continuous phase wrap up dispersed phase
(water) prepares gel emulsion, and water serves as pore-foaming agent in gel emulsion system, and the reduction of water content is so that the hole of material internal is tied
Structure gradually becomes smaller.
In order to verify its mechanical property, obtained test result is shown in Fig. 4 and Fig. 5, and the test object of Fig. 4 and Fig. 5 are reality
Apply the porous polymer material that example 1 is prepared；Fig. 4 is compression-rebound photo of 80% water content polymer material, and (a) is
Photo is compressed, is (b) rebound photo, can intuitively find out that the compression recovery performance of polymer material is very excellent, it is compressible
Property, it is flexible the features such as compensate for common hard material inconvenience existing for storage, transport and use process, meet simultaneously
The requirement of physical protection material requirements wearing comfort；Fig. 5 is the low density porous polymer material pressure of flexibility of 80% water content
Load-deformation curve when contracting, using WDW-100M microcomputer controlled electronic universal tester to flexible low density porous polymeric material
Material carry out compression performance test, when strain less than 50%, the load-deformation curve of polymer material substantially conform to recklessly can law,
The linear growth trend of curve；When strain is greater than 50%, the load-deformation curve of polymer material is exponentially increased, smaller
Stress sharply increases in the case where strain.
Referring to Fig. 6, (a), (b), (c) respectively correspond the flexible low density porous of 60%, 70%, 80% water content in Fig. 6
Polymer material water contact angle test chart, using DataphysicsOCA20 type video contact angle measuring instrument, by surfacing
Sample is placed on testboard, and drop volume is 2 μ L when test.It can be obtained from the figure that the water contact angle of polymer material is about~122 °,
With typical hydrophobic structure.
It is the low density porous polymer material TGA curve of flexibility of 80% water content referring to Fig. 7, Fig. 7, using U.S. TA public affairs
The thermogravimetric analyzer of department is tested, and selected sample carries out in air atmosphere, and 10 DEG C/min of heating rate, temperature range is room
Temperature is to 700 DEG C.It can be obtained from the figure that flexible low density porous polymer material has a small amount of thermal degradation before 200 DEG C, temperature reaches
It is sharply decomposed at 500 DEG C~600 DEG C, 700 DEG C reach degradation balance, and final residue rate is about 40%, show that polymer material has
There are excellent high temperature resistance and thermal structure stability, there is good thermal stability as physical protection material.
Referring to the low density porous polymeric material of flexibility that Fig. 8, Fig. 8 are using Headspace-Gas Chromatography Analysis to 80% water content
Material carries out organic volatile residual volume test result.Head space test condition are as follows: equilibration time is heated in 80 DEG C of equilibrium temperature of heating
10min, 120 DEG C of six-way valve temperature setting, 110 DEG C of transmission line temperature setting, pressure balance time 0.25min, sample injection time
1min；Gas-chromatography test condition are as follows: temperature program is 80 DEG C of holding 1min, rises to 200 DEG C with the heating rate of 25 DEG C/min,
5min is kept, it is 200 DEG C of injector temperature, 300 DEG C of detector temperature, column flow 1.0mL/min, hydrogen flowing quantity 30mL/min, empty
Throughput 300mL/min, input mode are split sampling, split ratio 10:1.It can be obtained by test result: polymer material and sky
White sample test curve essentially coincides, and shows that the porous polymer material finally prepared is remained without organic volatile, is a kind of peace
The material of human body environment is protected, be can be applied to loopful.
Referring to table 1, table 1 is Inspection and Quarantine Technic Center, Guangdong Entry-Exit Inspection and Qu to flexible low-density of the invention
Porous polymer material carries out skin irritatin test data, and test is according to national standard GB/T 21604-2008 " chemicals acute skin
Stimulation/corrosion test method " it carries out.Test result shows: each test time point does not observe the tester to family's rabbit skin
Erythema, oedema stimulate the reaction are caused, for 24 hours, respectively to observe time point highest point total mean value be 0 by 48h and 72h, according to skin irritatin intensity
Grade scale, the tested material are nonirritant reaction to rabbit skin irritation, can be used as a kind of and human contact protection material
Material.
1 Inspection and Quarantine Technic Center, Guangdong Entry-Exit Inspection and Qu of table is to the low density porous polymer of flexibility of the invention
The skin irritatin test data that material carries out
It is the low density porous polymer material PARA FORMALDEHYDE PRILLS(91,95) of flexibility and banana water absorption of 80% water content referring to Fig. 9, Fig. 9
Energy curve, the low density porous polymer material size of flexibility of selection are only the sample block of 2.1cm*1.8cm*1cm, are respectively placed in
In formaldehyde and banana oil sealed environment, flexible material reaches adsorption saturation after 20min, and PARA FORMALDEHYDE PRILLS(91,95) and the maximum of banana oil are inhaled
Attached amount is respectively 2.7mg/g and 22.6mg/g, shows effectively adsorb toxic and harmful gas present in environment.
The low density porous polymer material of flexibility of 80% water content can laboratory level amplification, size is up to 320 × 250
× 60mm, and still maintained under the size appearance uniform it is complete, without the characteristics such as fault of construction, overall performance be excellent.
In conclusion the low density porous polymer material of flexibility prepared by the present invention, can be used as physical protection material and is used for
Manufacture mask, earplug, earmuff and protective garment etc.；The polymer material mechanical recovery performance is good, when as physical protection material,
Deformation occurs when by external force, can reply after external force removal, be not likely to produce fold, can repeatedly use；Polymer material
Density is low, dresses light；Polymer material has hydrophobicity, can keep the drying of physical protection material；Polymer material has
Good absorption property when material as mask, gas mask or special occasions protective garment, can adsorb having in environment
Malicious nocuousness VOCs gas, is applied to particular job environment or hazardous chemical occasion, can effectively avoid human respiratory
Sucking or skin absorb；To no skin irritation, guarantee the safety of wearer.
The above content is merely illustrative of the invention's technical idea, and this does not limit the scope of protection of the present invention, all to press
According to technical idea proposed by the present invention, any changes made on the basis of the technical scheme each falls within claims of the present invention
Protection scope within.
Claims (7)
1. a kind of preparation method of the low density porous polymer material of flexibility, which comprises the following steps:
1) gel emulsion is prepared
Stabilizer is added in oil-based system, stirring forms mixed solution, the mixed solution is added in water phase, stirring forms white
Color lotion, it is static to be microfluidic to lotion or partly flow shape, gel emulsion is made；
By percentage to the quality, it the ratio of each component is: 0.1%~0.5% stabilizer, 15%~45% oily phase, 60%
~80% water phase；Wherein, oil is mutually by 5%~15% silane coupling agent, 5%~20% toughener and 5%~10%
Diluent mixes；
Stabilizer is
2) the flexible low density porous polymer material of preparation
By the gel emulsion in room temperature~50 DEG C, it polymerize 2~4h, temperature is risen to 50~90 DEG C, polymerize 4~12h, finally will
Temperature is warming up to 90~120 DEG C, polymerize 2~4h, is dried to obtain flexible low density porous polymer material later.
2. the preparation method of the low density porous polymer material of flexibility according to claim 1, which is characterized in that step 1)
In silane coupling agent be methyltrimethoxysilane, methyltriethoxysilane, ethyl trimethoxy silane, three ethoxy of ethyl
One of base silane, vinyltrimethoxysilane or vinyltriethoxysilane are a variety of.
3. the preparation method of the low density porous polymer material of flexibility according to claim 1, which is characterized in that step 1)
In toughener be one of nitrile rubber, acrylic rubber, polyurethane or polysiloxanes or a variety of.
4. the preparation method of the low density porous polymer material of flexibility according to claim 1, which is characterized in that step 1)
In diluent be one of n-hexane, hexamethylene, normal heptane, ethyl alcohol or isopropanol or a variety of.
5. a kind of preparation method of the low density porous polymer material of flexibility according to claim 1-4 is prepared into
To flexible low density porous polymer material.
6. the low density porous polymer material of flexibility according to claim 5, which is characterized in that the polymer material
Density is 0.20~0.40g/cm3, pore size is 10~100 μm, 200 DEG C of minimum thermal decomposition temperature >, to no skin irritation
Reaction.
7. a kind of application of low density porous polymer material of flexibility according to claim 5 as physical protection material.
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| CN105085787A (en) * | 2015-08-31 | 2015-11-25 | 陕西师范大学 | Compressible low-density porous polymer material and preparation method for same |
| CN108948252A (en) * | 2018-06-22 | 2018-12-07 | 南京亘闪生物科技有限公司 | A kind of preparation method of equal porous crosslinked polystyrene absorption resin |
| CN109825190A (en) * | 2018-11-02 | 2019-05-31 | 佛山市南海区里水镇经济促进局 | The preparation method of underwater environment manipulator shaft joint waterproof lubricant coating |
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| JP2004099418A (en) * | 2002-09-13 | 2004-04-02 | Naohiro Soga | Method for producing integrated porous material |
| CN105085787A (en) * | 2015-08-31 | 2015-11-25 | 陕西师范大学 | Compressible low-density porous polymer material and preparation method for same |
| CN108948252A (en) * | 2018-06-22 | 2018-12-07 | 南京亘闪生物科技有限公司 | A kind of preparation method of equal porous crosslinked polystyrene absorption resin |
| CN109825190A (en) * | 2018-11-02 | 2019-05-31 | 佛山市南海区里水镇经济促进局 | The preparation method of underwater environment manipulator shaft joint waterproof lubricant coating |
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