CN105968404A - Non-solution synthesis method of extrusion-resistant, fire-prevention and super-hydrophobic polymer material - Google Patents
Non-solution synthesis method of extrusion-resistant, fire-prevention and super-hydrophobic polymer material Download PDFInfo
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- CN105968404A CN105968404A CN201610322813.1A CN201610322813A CN105968404A CN 105968404 A CN105968404 A CN 105968404A CN 201610322813 A CN201610322813 A CN 201610322813A CN 105968404 A CN105968404 A CN 105968404A
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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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
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- C09K3/00—Materials not provided for elsewhere
- C09K3/32—Materials not provided for elsewhere for absorbing liquids to remove pollution, e.g. oil, gasoline, fat
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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
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08J2361/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08J2361/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
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Abstract
The invention relates to a non-solution synthesis method of an extrusion-resistant, fire-prevention and super-hydrophobic polymer material, belongs to the field of polymer material preparation, and aims at solving the technical problems that the existing synthesis method of the material for absorbing petroleum in water produces a great deal of pollutants such as waste water and waste liquid, so that the treatment process is complicated, the manufacturing cost is high, and true large-scale application is hard to realize. The non-solution synthesis method comprises the following step: by adopting silicone oil, modifying the surface of a polymer material in a polymerization manner by means of a gas-phase oligomeric silane chain when the temperature is higher than 50 DEG C or above to obtain the extrusion-resistant, fire-prevention and super-hydrophobic polymer material. After the non-solution method is adopted, the polymer material is modified; the non-solution synthesis method is a simple and green synthesis method, and does not produce any waste liquid and waste gas. The raw materials adopted by the method are low in price and easy to obtain, and the synthesis method is simple.
Description
Technical field
The present invention relates to macromolecule material preparation area, be specifically related to the non-solution synthesis method of a kind of anti-extrusion, fire prevention and super-hydrophobic macromolecular material.
Background technology
Marine ecosystems and littoral environment are brought huge destruction by oil, the leakage accident of water-fast hydrocarbons frequently.On the other hand, crude oil and hydrocarbons have inflammable and explosive character, and it is revealed and the most easily causes on fire and blast, brings huge loss to life and property.The heavy oil that current commercial oil skimmer processes viscosity bigger is highly effective.But for the oil that viscosity is less, due to features such as its diffusion area are big, oil reservoir is thin, it is difficult with traditional oil collection mode that encloses and clears up.Use the means such as dispersant, microorganism eutrophication and burning ecological environment not only brings secondary destroy or pollutes, and waste the energy oil product of worsening shortages.Therefore, develop new material further, efficiently clear up and reclaim water surface low viscosity oil slick and water-fast hydrocarbons has been extremely urgent.In order to obtain efficient adsorbent, the modification carrying out necessity on the three-dimensional porous material of organic (generally biopolymer and synthetic macromolecule) is a kind of effective approach.Although the newest three-dimensional porous material is used for adsorbing the oil in water; but its method for modifying and synthesizing is carried out often in the solution; this not only results in the pollutant such as substantial amounts of waste water, waste liquid; also make its complex disposal process, manufacturing cost high simultaneously, be difficulty with real large-scale application.
Summary of the invention
The invention solves the problems that being currently used for adsorbing the synthetic method of the material of oil in water can produce the pollutant such as substantial amounts of waste water, waste liquid; make its complex disposal process, manufacturing cost high; it is difficulty with the technical problem of real large-scale application, it is provided that the non-solution synthesis method of a kind of anti-extrusion, fire prevention and super-hydrophobic macromolecular material.
In order to solve above-mentioned technical problem, technical scheme is specific as follows:
The non-solution synthesis method of a kind of anti-extrusion, fire prevention and super-hydrophobic macromolecular material, comprises the following steps:
Use silicone oil, in temperature more than more than 50 DEG C, modified in polymer surface polymerization by the oligomerization silane chain of gas phase, prepare anti-extrusion, fire prevention and super-hydrophobic macromolecular material.
In technique scheme, the duct of described macromolecular material is the duct of opening, and voidage is 99.8%-10%.
In technique scheme, described macromolecular material is melmac sponge, aromatic ring polymer family macromolecule material, heterocycle polymer family macromolecule material, ladder polymer family macromolecule material or elemento-organic polymer family macromolecule material.
In technique scheme, described silicone oil is the fatty acid chain containing alkyl, the fatty acid chain containing fluorine or the silicone oil containing aromatic group.
In technique scheme, specific experiment step and the experiment condition of described non-solution synthesis method are as follows:
Being placed in by macromolecular material in the container filling silicone oil, heating-up temperature is 50-400 DEG C, and the response time is 10 minutes-48 hours, then reaction system is cooled to room temperature, prepares anti-extrusion, fire prevention and super-hydrophobic macromolecular material.
The invention has the beneficial effects as follows:
(1) present invention uses non-solution methods to realize the modification to macromolecular material, is a kind of simple, green synthetic method, does not produce any waste liquid and waste gas.The low in raw material price used is easy to get, and synthetic method is simple.
(2) method of modifying that the present invention provides is simple and gentle, from Fig. 1 a Yu 1b it can be seen that do not destroy its original structure before and after Xiu Shiing.Shown in Fig. 1 c, pass through elementary analysis, it was demonstrated that can effectively modify target substance.Considering from superhydrophobic property, the material prepared by the method has good superhydrophobic property.As shown in Figure 1 d, original melmac sponge is hydrophilic (Fig. 1 a, Fig. 1 c), once touches water, quickly water is sucked in sponge (Fig. 1 d), puts it in water, quickly submerged (under Fig. 1 f).And on the contrary, the water contact angle of material prepared by us has reached 160.4 °, illustrate that it has good superhydrophobic property (Fig. 1 e, 1f), water droplet can not be adsorbed to material internal, form the drop of intimate ball-type (Fig. 1 e g), and can swim on the water surface (on Fig. 1 f) well on its surface.
(3) consider from engineering properties, anti-extrusion, fire prevention and the super-hydrophobic sponge prepared by this method have extraordinary engineering properties, as shown in Figure 2 a, this sponge can arbitrarily compress the volume of 10-80%, it can return to original volume effectively；And after we process 1000 times by compression 50% this mode further, it still can return to original volume (Fig. 2 b) effectively, its pattern does not still have the biggest change (Fig. 2 c), above description of test is by us this gentleness, green construction method, the engineering properties of original melmac sponge can be kept to greatest extent, so that final anti-extrusion, fire prevention and super-hydrophobic sponge have extraordinary engineering properties.Utilize the character of this anti-extrusion, effectively can reclaim, by pressing method simply, the organic solvent adsorbed.
(4) considering from fire prevention angle, we use commercial commonly used polypropylene non-woven fabric as reference, by combustion experiment, find that anti-extrusion, fire prevention and the super-hydrophobic sponge prepared by this method have flameproof effect well.(700 DEG C), polypropylene non-woven fabric vigorous combustion as shown in Figure 3 a by the way of microwave heating, and discharge substantial amounts of heat energy (Fig. 3 c) and flue dust (Fig. 3 d), burning the most completely (as Fig. 3 a is right).On the contrary, anti-extrusion, fire prevention and the super-hydrophobic sponge prepared by this method are in the case of microwave heating, as shown in Figure 3 b, in 4 seconds on fire, but extinguished in 3 seconds, only discharge little heat energy (Fig. 3 c, d) and flue dust (Fig. 3 d), and finally still leave substantial amounts of residuals (as Fig. 3 b is right).Anti-extrusion, fire prevention and the super-hydrophobic sponge that this explanation is prepared by this method inherently has the ability of flame resistant.
(5) considering from reality application angle, anti-extrusion, fire prevention and the super-hydrophobic sponge prepared by this method can adsorb crude oil effectively, can reclaim, and can be easy to large-scale production by the way of extruding.Adopt the adsorbing material produced in this way, can not only effectively remove the oil (Fig. 4 a-d) on the water surface, and because building-up process environmental protection will not bring any harmful effect to environment, when actual treatment Oil spills, can not only effectively remove the crude oil on the water surface, and the restoration of the ecosystem (Fig. 4 e-h) on contaminated ground can be effectively realized.
Accompanying drawing explanation
With detailed description of the invention, the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 is to modify the scanning electron microscope of forward and backward melmac sponge, Elemental redistribution and water absorption test figure；Wherein: a) for the scanning electron microscope diagram of melmac sponge before modifying；B) scanning electron microscope diagram of melmac sponge after the modification of embodiment 1 preparation；C) distribution diagram of element of melmac sponge after the modification of embodiment 1 preparation；D) add water the front melmac sponge of modification, and water is quickly drawn into the picture within sponge；Melmac sponge after the modification of the embodiment that e) adds water 1 preparation, water will not be adsorbed onto inside sponge, but pool the picture of the water droplet of almost spherical on its surface；F) before modifying, melmac sponge sinks under water because of water suction, and the melmac sponge after modification floats on the picture on the water surface.
Fig. 2 be modify after the measuring mechanical property figure of melmac sponge；Wherein: a) the measuring mechanical property figure of melmac sponge after the modification of embodiment 1 preparation, compression ratio is from 10-80%；B) after modifying, melmac sponge is repeated 1000 times with the degree of compression ratio 50%；C) compress 50% test process and compress the photo after 1000 times.
Fig. 3 is polypropylene non-woven fabric and the combustion testing figure of melmac sponge after modifying；Wherein: a) picture of the oil absorption material polypropylene non-woven fabric combustion testing that business uses；B) picture of the combustion testing of melmac sponge after the modification of embodiment 1 preparation；C) polypropylene non-woven fabric with modify after melmac sponge burning Heat liberation unit figure；D) polypropylene non-woven fabric with modify after melmac sponge burning smoke release figure.
Fig. 4 is that the melmac sponge after modifying removes greasy dirt figure；Wherein: a) picture in the pond polluted by Oil spills；B) the melmac sponge after the modification of embodiment 1 preparation is used to carry out the picture of oil removal；C) picture of the melmac sponge of absorption greasy dirt；C) picture in the pond after oil removal；E) after one week, the picture of the overall picture in pond after oil removal；F) pond occur the picture of water plant；G) pond occur the picture of aquatic animal；H) pond occur the picture of Rana ovum.
Detailed description of the invention
The invention thought of the present invention is: the invention solves the problems that being currently used for adsorbing the synthetic method of the material of oil in water can produce the pollutant such as substantial amounts of waste water, waste liquid; make its complex disposal process, manufacturing cost high, be difficulty with the technical problem of real large-scale application.Silane chain based on oligomerization can form this phenomenon of relatively firm silane polymer effectively in surface of solids polymerization, our reported first, use cheap silicone oil as raw material, at relatively low temperature, by adding the oligomerization silane chain being thermally generated gas phase, just can realize macromolecular material carries out modification effectively, and by simply changing the group of silicone oil, the groups such as different groups such as methyl, ethyl, perfluorocarbon can be modified.We are further with such a characteristic, in fireproof tripolycyanamide porous three-dimensional structure, successfully modify the groups such as upper perfluorocarbon, we have found that this modification can not only effectively change the hydrophilic of tripolycyanamide and enable it to effectively adsorb Organic substance, but also remain its mechanical performance and fire protecting performance well.The more important thing is that the method can be extended to other high temperature-resistant polymer material such as polyimide material, aromatic polyamide fibres etc..This method of modifying, can not only avoid completely complexity, produce a large amount of waste water, the molten liquid-phase operation of refuse, and simply efficient, be that one has promising method very much.
Embodiment 1
Being placed in the container filling methyl-silicone oil by melmac sponge, heating-up temperature is 230 DEG C, and the response time is 5 hours.Then reaction system is cooled to room temperature, and prepared material is referred to as material 1.
Embodiment 2
Being placed in the container filling ethyl silicon oil by melmac sponge, heating-up temperature is 230 DEG C, and the response time is 5 hours.Then reaction system is cooled to room temperature, and prepared material is referred to as material 2.
Embodiment 3
Being placed in the container filling phenyl silicone oil by melmac sponge, heating-up temperature is 230 DEG C, and the response time is 5 hours.Then reaction system is cooled to room temperature, and prepared material is referred to as material 3.
Embodiment 4
By melmac sponge in the container filling fluorine containing silicone oil, heating-up temperature is 230 DEG C, and the response time is 5 hours.Then reaction system is cooled to room temperature, and prepared material is referred to as material 4.
Embodiment 5
Being placed in the container filling methyl-silicone oil by melmac sponge, heating-up temperature is 180 DEG C, and the response time is 48 hours.Then reaction system is cooled to room temperature, and prepared material is referred to as material 5.
Embodiment 6
Being placed in the container filling methyl-silicone oil by melmac sponge, heating-up temperature is 200 DEG C, and the response time is 24 hours.Then reaction system is cooled to room temperature, and prepared material is referred to as material 6.
Embodiment 7
Being placed in the container filling methyl-silicone oil by melmac sponge, heating-up temperature is 210 DEG C, and the response time is 10 hours.Then reaction system is cooled to room temperature, and prepared material is referred to as material 7.
Embodiment 8
Being placed in the container filling methyl-silicone oil by melmac sponge, heating-up temperature is 220 DEG C, and the response time is 8 hours.Then reaction system is cooled to room temperature, and prepared material is referred to as material 8.
Embodiment 9
Being placed in the container filling methyl-silicone oil by melmac sponge, heating-up temperature is 230 DEG C, and the response time is 6 hours.Then reaction system is cooled to room temperature, and prepared material is referred to as material 9.
Embodiment 10
Being placed in the container filling methyl-silicone oil by melmac sponge, heating-up temperature is 240 DEG C, and the response time is 4 hours.Then reaction system is cooled to room temperature, and prepared material is referred to as material 10.
Embodiment 11
Being placed in the container filling methyl-silicone oil by melmac sponge, heating-up temperature is 250 DEG C, and the response time is 2 hours.Then reaction system is cooled to room temperature, and prepared material is referred to as material 11.
Embodiment 12
Being placed in the container filling methyl-silicone oil by poly-sub-benzene macromolecular material, heating-up temperature is 400 DEG C, and the response time is 10 minutes.Then reaction system is cooled to room temperature, and prepared material is referred to as material 12.Described macromolecular material can also be Parylene, polyarylether, polyarylate or aromatic polyamide.
Embodiment 13
Being placed in the container filling methyl-silicone oil by polyimides macromolecular material, heating-up temperature is 50 DEG C, and the response time is 2 hours.Then reaction system is cooled to room temperature, and prepared material is referred to as material 13.Described macromolecular material can also be polybenzimidazoles or poly quinoline.
Embodiment 14
Being placed in the container filling methyl-silicone oil by polypyrrole ladder polymer macromolecular material, heating-up temperature is 250 DEG C, and the response time is 2 hours.Then reaction system is cooled to room temperature, and prepared material is referred to as material 14.Described macromolecular material can also be graphite mould ladder polymer, phenanthroline class ladder polymer or quinolines ladder polymer.
Embodiment 15
Being placed in the container filling methyl-silicone oil by organic polymer macromolecular material siliceous for main chain, heating-up temperature is 250 DEG C, and the response time is 2 hours.Then reaction system is cooled to room temperature, and prepared material is referred to as material 15.Described macromolecular material can also be that main chain is phosphorous or the organic polymer of boron or other organometallic polymers.
Embodiment 16
The anti-extrusion of embodiment 1-15, fire prevention and super-hydrophobic macromolecular material are carried out the contact angle test of water, to determine its super-hydrophobic character.As shown in table 1: within the scope of different silane groups and bigger temperature, all to realize the superhydrophobic property of prepared material.
| The kind of material | The contact angle of water |
| Material 1 | 163.4° |
| Material 2 | 162.5° |
| Material 3 | 163.1° |
| Material 4 | 160.3° |
| Material 5 | 157.4° |
| Material 6 | 155.7° |
| Material 7 | 155.7° |
| Material 8 | 162.5° |
| Material 9 | 162.5° |
| Material 10 | 152.4° |
| Material 11 | 162.5° |
| Material 12 | 160.1° |
| Material 13 | 159.2° |
| Material 14 | 155.6° |
| Material 15 | 158.3° |
The contact angle test of prepared material within the scope of silane group that table 1 is different and bigger temperature
Obviously, above-described embodiment is only for clearly demonstrating example, and not restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also cannot all of embodiment be given exhaustive.And the obvious change thus extended out or variation still in the protection domain of the invention among.
Claims (5)
1. an anti-extrusion, fire prevention and the non-solution synthesis method of super-hydrophobic macromolecular material, it is characterised in that
Comprise the following steps:
Use silicone oil, in temperature more than more than 50 DEG C, by the oligomerization silane chain of gas phase at macromolecular material table
Face polymerization is modified, and prepares anti-extrusion, fire prevention and super-hydrophobic macromolecular material.
The non-solution synthesis of anti-extrusion the most according to claim 1, fire prevention and super-hydrophobic macromolecular material
Method, it is characterised in that the duct of described macromolecular material is the duct of opening, and voidage is
99.8%-10%.
The non-solution synthesis of anti-extrusion the most according to claim 1, fire prevention and super-hydrophobic macromolecular material
Method, it is characterised in that described macromolecular material is melmac sponge, aromatic ring polymerization species high score
Sub-material, heterocycle polymer family macromolecule material, ladder polymer family macromolecule material or element organic polymer
Species macromolecular material.
The non-solution synthesis of anti-extrusion the most according to claim 1, fire prevention and super-hydrophobic macromolecular material
Method, it is characterised in that described silicone oil is the fatty acid chain containing alkyl, fatty acid chain containing fluorine or contain
There is the silicone oil of aromatic group.
5. non-according to the anti-extrusion described in claim 1-4 any one, fire prevention and super-hydrophobic macromolecular material
Solution synthesis method, it is characterised in that the specific experiment step of described non-solution synthesis method and experiment condition
As follows:
Being placed in by macromolecular material in the container filling silicone oil, heating-up temperature is 50-400 DEG C, and the response time is 10
Minutes-48 hours, then reaction system is cooled to room temperature, prepares anti-extrusion, fire prevention and super-hydrophobic height
Molecular material.
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Citations (5)
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|---|---|---|---|---|
| CN102665894A (en) * | 2009-11-23 | 2012-09-12 | 3M创新有限公司 | Methods of surface treating porous particles |
| CN103276707A (en) * | 2013-05-14 | 2013-09-04 | 中国科学技术大学 | Floating oil collecting device, manufacturing method thereof and applications thereof |
| CN103951843A (en) * | 2014-03-11 | 2014-07-30 | 中国科学院长春应用化学研究所 | Preparation method of extrusion resistant, fire preventing and super hydrophobic sponge |
| CN104140553A (en) * | 2014-07-18 | 2014-11-12 | 天津大学 | Hydrophobic chitosan-silicon dioxide composite aerogel and preparation method and oil absorption application thereof |
| CN104945656A (en) * | 2015-06-25 | 2015-09-30 | 华南理工大学 | High-performance cellulose base oil absorption material and preparing method thereof |
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2016
- 2016-05-16 CN CN201610322813.1A patent/CN105968404A/en active Pending
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|---|---|---|---|---|
| CN102665894A (en) * | 2009-11-23 | 2012-09-12 | 3M创新有限公司 | Methods of surface treating porous particles |
| CN103276707A (en) * | 2013-05-14 | 2013-09-04 | 中国科学技术大学 | Floating oil collecting device, manufacturing method thereof and applications thereof |
| CN103951843A (en) * | 2014-03-11 | 2014-07-30 | 中国科学院长春应用化学研究所 | Preparation method of extrusion resistant, fire preventing and super hydrophobic sponge |
| CN104140553A (en) * | 2014-07-18 | 2014-11-12 | 天津大学 | Hydrophobic chitosan-silicon dioxide composite aerogel and preparation method and oil absorption application thereof |
| CN104945656A (en) * | 2015-06-25 | 2015-09-30 | 华南理工大学 | High-performance cellulose base oil absorption material and preparing method thereof |
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Application publication date: 20160928 |