CN102532765A - Moisture adsorption membrane and preparation method thereof - Google Patents
Moisture adsorption membrane and preparation method thereof Download PDFInfo
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- CN102532765A CN102532765A CN2012100318975A CN201210031897A CN102532765A CN 102532765 A CN102532765 A CN 102532765A CN 2012100318975 A CN2012100318975 A CN 2012100318975A CN 201210031897 A CN201210031897 A CN 201210031897A CN 102532765 A CN102532765 A CN 102532765A
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- 238000002360 preparation method Methods 0.000 title claims description 21
- 238000001179 sorption measurement Methods 0.000 title abstract description 14
- 239000012528 membrane Substances 0.000 title abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 76
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 66
- 239000002253 acid Substances 0.000 claims abstract description 41
- 150000001336 alkenes Chemical class 0.000 claims abstract description 35
- 239000000178 monomer Substances 0.000 claims abstract description 35
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 34
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims description 63
- 239000000835 fiber Substances 0.000 claims description 44
- 229960001866 silicon dioxide Drugs 0.000 claims description 41
- 239000003365 glass fiber Substances 0.000 claims description 36
- 235000012239 silicon dioxide Nutrition 0.000 claims description 33
- 239000000017 hydrogel Substances 0.000 claims description 27
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 18
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 17
- 239000000499 gel Substances 0.000 claims description 16
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 239000003999 initiator Substances 0.000 claims description 13
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 6
- 229940047670 sodium acrylate Drugs 0.000 claims description 6
- SONHXMAHPHADTF-UHFFFAOYSA-M sodium;2-methylprop-2-enoate Chemical compound [Na+].CC(=C)C([O-])=O SONHXMAHPHADTF-UHFFFAOYSA-M 0.000 claims description 6
- 239000000463 material Substances 0.000 abstract description 36
- 229920000098 polyolefin Polymers 0.000 abstract description 5
- 239000003607 modifier Substances 0.000 abstract 6
- 239000012784 inorganic fiber Substances 0.000 abstract 4
- 229920000642 polymer Polymers 0.000 abstract 2
- 238000002474 experimental method Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 194
- 238000010521 absorption reaction Methods 0.000 description 60
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 33
- 239000007787 solid Substances 0.000 description 18
- 238000012360 testing method Methods 0.000 description 18
- 238000003756 stirring Methods 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 239000004160 Ammonium persulphate Substances 0.000 description 13
- 239000004159 Potassium persulphate Substances 0.000 description 13
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 13
- 235000019395 ammonium persulphate Nutrition 0.000 description 13
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 13
- 235000019394 potassium persulphate Nutrition 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 239000000741 silica gel Substances 0.000 description 8
- 229910002027 silica gel Inorganic materials 0.000 description 8
- 230000002269 spontaneous effect Effects 0.000 description 8
- 239000003463 adsorbent Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 239000012467 final product Substances 0.000 description 6
- 229920006395 saturated elastomer Polymers 0.000 description 6
- 229920005601 base polymer Polymers 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 230000007423 decrease Effects 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- 230000000274 adsorptive effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 229940048053 acrylate Drugs 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 201000004792 malaria Diseases 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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Abstract
The invention provides a moisture adsorption membrane. The membrane is prepared from an olefin acid polymeric monomer, an inorganic fiber membrane and an inorganic modifier through polymerization reaction, wherein the inorganic modifier is silica and/or alumina. The olefin acid polymeric monomer is subjected to polymerization reaction in the presence of the inorganic fiber membrane and the inorganic modifier, and the obtained polyolefin acid polymer has a certain moisture adsorption property; the inorganic modifier is coated in the polymer in the polymerization process, so that the inorganic modifier is uniformly distributed in the moisture adsorption membrane; the used inorganic modifier has high specific surface area and adsorption property, so that the moisture adsorption capacity of the obtained moisture adsorption membrane is improved; experiment results show that the moisture adsorption capacity of the moisture adsorption membrane can be 1.5 times the self weight of the moisture adsorption membrane; the inorganic fiber membrane is taken as a support framework of polymerization reaction, so that a membraneous moisture adsorption material is obtained; and the mechanical strength of the moisture adsorption membrane is improved by the inorganic fiber membrane.
Description
Technical field
The technical field that the present invention relates to dehumidify relates in particular to a kind of hygroscopic film and preparation method thereof.
Background technology
Atmospheric moisture is an important environmental parameters that life and the production with people has substantial connection, and humidity all has significant effects to the comfort level of human body, the production process of product, the quality of product and the preservation period of product.Live and work in the malaria environment for a long time, the people knows from experience and receives the invasion and attack of " wet ", causes the thermal equilibrium of human body to be destroyed, and this not only influences HUMAN HEALTH, and can influence normal live and work, the efficient of reduction work.In Industrial processes, in the production process like precision instrument, measuring instrument, electronic product and Chemicals etc., if humidity is not controlled, the quality of product can be had a strong impact on.In a humid environment, food can be because the erosion of mould and moldy metamorphism, and metal can get rusty, and accuracy of instrument can descend, insulation parameter can reduce etc., and these all can cause great loss to national economy etc.It is thus clear that no matter the control of humidity is to living environment and Working environment, still production process and article protect are all seemed very important.Along with the raising of scientific and technological level and the development of production, air dewetting has formed and has developed into a new technology.
Generally use at present to remove wet stock be inorganic hygroscopic material; What wherein be widely used mainly contains silica gel, gac and molecular sieve; These inorganic hygroscopic materials can be realized the function that dehumidifies; Yet their moisture absorption capacity is generally lower, less than 60% of own wt, is difficult to satisfy the dehumidifying requirement in high humidity environment.In order to improve moisture absorption capacity except that wet stock; It is organic hygroscopic material of representative that prior art has developed with the ZX-I base polymer; Like publication number is the preparation method that the Chinese patent document of CN 101003598A discloses a kind of hygroscopic material of organic macromolecule; This method neutralizes acrylate monomers solution with sodium hydroxide solution, to wherein adding linking agent and initiator, under bath temperature is 40 ℃～70 ℃ water bath with thermostatic control condition, carry out polyreaction then; React after 2 hours～5 hours, obtain reaction product; The reaction product that obtains is carried out granulation, oven dry and pulverizing, obtain hygroscopic material of organic macromolecule.This method has adopted the polyacrylate resins at home first organic polymer hygroscopic materials, the hygroscopic material of organic macromolecule that obtains has hygroscopic property preferably, but it only possesses granular characteristic, can not satisfy the requirement of special dehumidifying shape.
In order to satisfy the demand of special dehumidifying shape; Prior art discloses with the inorganic fibre film as the inorganic hygroscopic material of the reinforcing of base material; Membranaceous inorganic hygroscopic material like the production of U.S. Roche Co.,Ltd; This hygroscopic material can satisfy the requirement of particular surroundings to the hygroscopic material shape, yet the wettability power of this membranaceous inorganic hygroscopic material is lower, and especially the effect on moisture extraction in high humidity environment is not good.
Summary of the invention
The object of the present invention is to provide a kind of hygroscopic film and preparation method thereof, hygroscopic film provided by the invention has higher moisture absorption capacity, and wettability power is better.
The present invention provides a kind of hygroscopic film, is obtained through polyreaction by olefin(e) acid class polymerization single polymerization monomer, inorganic fibre film and inorganic modified dose;
Said inorganic modified dose is silicon-dioxide and/or aluminum oxide.
Preferably, said olefin(e) acid class polymerization single polymerization monomer is one or more in vinylformic acid, methylacrylic acid, sodium acrylate and the sodium methacrylate.
Preferably, said inorganic fibre film is inorganic glass fiber film or inorganic ceramic tunica fibrosa.
Preferably, said inorganic modified dose is silicon dioxide gel and/or alumina sol.
The present invention provides a kind of preparation method of hygroscopic film, may further comprise the steps:
Olefin(e) acid class polymerization single polymerization monomer and pH value regulator, linking agent, initiator and inorganic modified dose are mixed, obtain the pH value and be 3.0～7.0 mixing solutions;
The inorganic fibre film is infiltrated in the said mixing solutions, obtains hydrogel after the polyreaction;
Said hydrogel is dry, obtain hygroscopic film;
Said inorganic modified dose is silicon-dioxide and/or aluminum oxide.
Preferably, said olefin(e) acid class monomer is one or more in vinylformic acid, methylacrylic acid, sodium acrylate and the sodium methacrylate.
Preferably, said inorganic modified dose is silicon dioxide gel and/or alumina sol.
Preferably, said inorganic fibre film is inorganic glass fiber film or inorganic ceramic tunica fibrosa.
Preferably, the temperature of said polyreaction is 30 ℃～90 ℃.
Preferably, the time of said polyreaction is 1 hour～10 hours.
The present invention provides a kind of hygroscopic film, is obtained through polyreaction by olefin(e) acid class polymerization single polymerization monomer, inorganic fibre film and inorganic modified dose; Said inorganic modified dose is silicon-dioxide and/or aluminum oxide.The present invention is a raw material with olefin(e) acid class polymerization single polymerization monomer, inorganic fibre film and inorganic modified dose, and it is carried out obtaining hydrogel thin film after the polyreaction; With obtaining hygroscopic film after the said hydrogel thin film drying.In the present invention, said olefin(e) acid class polymerization monomer polymerization obtains the polyolefin acid base polymer, and the polymkeric substance that obtains has hygroscopic property; In polymerization process; Said inorganic modified dose be wrapped in said polyolefin acid base polymer in; It is evenly dispersed in the hygroscopic film that obtains, and said inorganic modified dose is silicon-dioxide and/or aluminum oxide, and it has bigger specific surface area and stronger adsorptive power; Make hygroscopic film provided by the invention have higher moisture absorption capacity, wettability power is better; And said polyreaction carries out on the support frame that the inorganic fibre film provides, and makes hygroscopic film provided by the invention have higher physical strength.Experimental result shows; The moisture absorption capacity of hygroscopic film provided by the invention is up to 1.5 times of himself weight; And inorganic modified dose of moisture absorption dew point that can also improve said hygroscopic film; Along with the increase of inorganic modified agent content, the moisture absorption dew point of said hygroscopic film decreases, and the moisture absorption dew point of hygroscopic film provided by the invention can be low to moderate-27 ℃.
In addition, the preparation method of hygroscopic film provided by the invention is the skeleton of polyreaction with the inorganic fibre film, helps the formation of membranous absorbent material, and the hygroscopic film that obtains can satisfy the demand of special dehumidifying shape.
Description of drawings
The moisture absorption capacity of the hygroscopic material that Fig. 1 provides for the embodiment of the invention 1 and comparative example and the relation curve of relative humidity;
Wherein, the moisture absorption capacity of the hygroscopic material that provides for embodiment 1 of curve 1 and the relation curve of relative humidity; The moisture absorption capacity of the hygroscopic material that curve 2 provides for comparative example 1 and the relation curve of relative humidity; The moisture absorption capacity of the hygroscopic material that curve 3 provides for comparative example 2 and the relation curve of relative humidity.
Embodiment
The invention provides a kind of hygroscopic film, obtain through polyreaction by olefin(e) acid class polymerization single polymerization monomer, inorganic fibre film and inorganic modified dose;
Said inorganic modified dose is silicon-dioxide and/aluminum oxide.
Hygroscopic film provided by the invention is one of raw material with olefin(e) acid class polymerization single polymerization monomer, and it is carried out obtaining hygroscopic film after the polyreaction.Said olefin(e) acid class polymerization single polymerization monomer is preferably one or more in vinylformic acid, methylacrylic acid, sodium acrylate and the sodium methacrylate, and more preferably vinylformic acid and/or methylacrylic acid most preferably are vinylformic acid and methylacrylic acid; The present invention does not have particular restriction to the condition of said polyreaction, adopts the technical scheme of the monomeric polyreaction of olefin(e) acid class polymerization well known to those skilled in the art to get final product.
Hygroscopic film provided by the invention is one of raw material with the inorganic fibre film; The inorganic fibre film is to be the man-made fiber film that raw material is processed with the mineral substance; It has combined the weaved processing characteristics of fiber and the excellent properties of mineral substance, has high temperature resistant, Heat stability is good, anti-oxidant, corrosion-resistant, characteristic such as heat-proof quality is good.In the present invention, said inorganic fibre film is preferably inorganic glass fiber film or inorganic ceramic tunica fibrosa, more preferably inorganic glass fiber film.
The present invention is a propping material with the inorganic fibre film; Make said olefin(e) acid class polymerization single polymerization monomer under the condition that said inorganic fibre film exists, carry out polyreaction; Obtain hygroscopic film; The membrane structure of the hygroscopic film that obtains can be crooked, has the characteristic of reprocessing typing, makes hygroscopic film provided by the invention can satisfy the requirement of specific dehumidifying shape; And the inorganic fibre film has reinforcement effect to the hygroscopic film that obtains, and makes the hygroscopic film that forms have higher physical strength.
Hygroscopic film provided by the invention is one of raw material with inorganic modified dose; Said inorganic modified dose is silicon-dioxide and/or aluminum oxide; Said inorganic modified dose with technique scheme in said olefin(e) acid class polymerization single polymerization monomer and said inorganic fibre film carry out polyreaction, obtain hygroscopic film, in the process that said polyreaction is carried out; In the said inorganic modified dose of polymkeric substance that is wrapped in formation, make said inorganic modified dose to be evenly dispersed in the hygroscopic film that obtains.Inorganic modified dose of the present invention's employing itself has a large amount of small spaces, can form a large amount of adsorption surfaces, thereby increase the adsorption area to moisture; And because effect capillaceous; Make the water surface be spill; The dividing potential drop of the intrinsic standoff ratio water in air steam of the water vapour of the spill water surface is much lower, therefore can from air, absorb moisture, and through physical attraction power moisture retained; Thereby make hygroscopic film provided by the invention have higher moisture absorption capacity, hygroscopic property is better.
In the present invention; Said inorganic modified dose is preferably silicon dioxide gel and/or alumina sol; More preferably silicon dioxide gel and alumina sol, when being silicon-dioxide and aluminum oxide for said inorganic modified dose, the mass ratio of said silicon-dioxide and said aluminum oxide is preferably (0.1～5): (0.0001～0.02); More preferably (0.5～4): (0.001～0.01) most preferably is (1～3): (0.005～0.008); The solid content of said silicon dioxide gel is preferably 10%～60%, and more preferably 20%～50%, most preferably be 25%～40%; The solid content of said alumina sol is preferably 1%～15%, and more preferably 3%～10%, most preferably be 5%～8%.
The present invention provides a kind of hygroscopic film, is obtained through polyreaction by olefin(e) acid class polymerization single polymerization monomer, inorganic fibre film and inorganic modified dose; Said inorganic modified dose is silicon-dioxide and/or aluminum oxide.The hygroscopic film that obtains is a support frame with the inorganic fibre film; The polyolefin acid base polymer that is obtained by olefin(e) acid class polymerization monomer polymerization forms on the skeleton of inorganic fibre film; Obtained having membranaceous hygroscopic material; Can satisfy the requirement of special dehumidifying shape, and said inorganic fibre film has reinforcement effect to hygroscopic film, improved the physical strength of hygroscopic film; In polymerization process; Said inorganic modified dose is wrapped in the polymkeric substance; Make said inorganic modified dose to be scattered in equably in the hygroscopic film, inorganic modified dose has bigger specific surface area and higher hygroscopic property, has strengthened hygroscopic film to absorption of water; Thereby make hygroscopic film provided by the invention have higher moisture absorption capacity, wettability power is better.
The invention provides a kind of preparation method of hygroscopic film, may further comprise the steps:
Olefin(e) acid class polymerization single polymerization monomer and pH value regulator, linking agent, initiator and inorganic modified dose are mixed, obtain the pH value and be 3.0～7.0 mixing solutions;
The inorganic fibre film is infiltrated in the said mixing solutions, obtains hydrogel after the polyreaction;
Said hydrogel is dry, obtain hygroscopic film;
Said inorganic modified dose is silicon-dioxide and/or aluminum oxide.
The present invention at first mixes olefin(e) acid class polymerization single polymerization monomer and pH value regulator, linking agent, initiator and inorganic modified dose, obtains the pH value and be 3.0～7.0 mixing solutions.
The present invention is preferred earlier with olefin(e) acid class polymerization single polymerization monomer and the mixing of pH value regulator, and then is 3.0～7.0 mixing solutions to wherein adding linking agent, initiator and inorganic modified dose, obtaining the pH value, preferably obtains pH and be 4.0～6.5 mixing solutions.In the present invention, said olefin(e) acid class polymerization single polymerization monomer is preferably one or more in vinylformic acid, methylacrylic acid, sodium acrylate and the sodium methacrylate, and more preferably vinylformic acid and/or methylacrylic acid most preferably are vinylformic acid and methylacrylic acid; Said pH value regulator is preferably sodium hydroxide, sodium hydroxide solution more preferably, and the mass concentration of said sodium hydroxide solution is preferably 10%～50%, and more preferably 15%～45%, most preferably be 20%～30%; The present invention does not have special limitation to the mass ratio of said olefin(e) acid class polymerization single polymerization monomer and said pH value regulator, makes that the pH value of last mixing solutions is 3.0～7.0 to get final product.
Said olefin(e) acid class polymerization single polymerization monomer is with after said pH value regulator mixes, and the present invention is 3.0～7.0 mixing solutions to wherein adding linking agent, initiator and inorganic modified dose, obtaining the pH value; Said inorganic modified dose is silicon-dioxide and/or aluminum oxide.The present invention does not have special limitation to the addition sequence of said linking agent, initiator and inorganic modified dose, adopts the addition sequence of each raw material in the polyreaction well known to those skilled in the art to get final product.Preferred linking agent and the initiator of at first in the mixing solutions of olefin(e) acid class polymerization single polymerization monomer and said pH value regulator, adding of the present invention; After stirring again to wherein adding inorganic modified dose; Then to wherein preferably adding deionized water; Make the monomeric mass concentration of the polymerization of olefin(e) acid class described in the mixing solutions that obtains be preferably 10%～50%, more preferably 20%～40%.The pH value that the present invention obtains is that the color of 3.0～7.0 mixing solutions is turned white slightly.
In the present invention, said linking agent is preferably N, the N-DMAA; Said initiator is preferably one or both in Potassium Persulphate and the ammonium persulphate, more preferably Potassium Persulphate and ammonium persulphate; Said inorganic modified dose is preferably silicon dioxide gel and/or alumina sol, and said alumina sol is preferably intends thin aluminium stone colloidal sol.
Said olefin(e) acid class monomer and said linking agent, said initiator, said inorganic modified dose mass ratio are preferably 1: (0.0005～0.006): (0.0001～0.003): (0.1～3), more preferably 1: (0.001～0.005): (0.0005～0.002): (0.02～1); When being silicon-dioxide and aluminum oxide for said inorganic modified dose, the mass ratio of said silicon-dioxide and said aluminum oxide is preferably (0.1～5): (0.0001～0.02); The solid content of silicon dioxide gel according to the invention is preferably 10%～60%; More preferably 20%～50%, most preferably be 25%～40%, the solid content degree of said alumina sol is preferably 1%～15%; More preferably 3%～10%, most preferably be 5%～8%; When said initiator is Potassium Persulphate and ammonium persulphate; The present invention does not have special limitation to the mass ratio of said Potassium Persulphate and ammonium persulphate; Adopt Potassium Persulphate and the mass ratio of ammonium persulphate as initiator well known to those skilled in the art to get final product; In the present invention, the mass ratio of said Potassium Persulphate and ammonium persulphate is preferably 1: 1.
After obtaining the pH value and be 3.0～7.0 mixing solutions, the present invention is infiltrated on the inorganic fibre film in the said mixing solutions, obtains hydrogel after the polyreaction.
The present invention is infiltrated on the inorganic fibre film in the said mixing solutions; Preferably leave standstill to said inorganic fibre film adsorb said mixing solutions saturated after; The inorganic fibre film that the absorption that obtains is saturated preferably places under the air tight condition, carry out polyreaction after, obtain hydrogel.The present invention preferably said inorganic fibre film adsorb said mixing solutions saturated after, mixing solutions spontaneous current unnecessary on the inorganic fibre film that said absorption is saturated does not have the mobile mixing solutions down to said inorganic fibre film surface.
In the present invention, said inorganic fibre film is preferably inorganic glass fiber film or inorganic ceramic tunica fibrosa, more preferably inorganic glass fiber film; The thickness of said inorganic fibre film is preferably 0.18mm～0.60mm, more preferably 0.30mm～0.50mm; The surface-area of said inorganic fibre film is preferably 5.0cm
2～9cm
2, 6.0cm more preferably
2～8cm
2Olefin(e) acid class polymerization single polymerization monomer in the volume of said inorganic fibre film and the said mixing solutions, inorganic modified dose mass ratio are preferably (18～60) mm
3: (0.1～5) g: (0.01～0.5) g, more preferably (25～50) mm
3: (0.5～4) g: (0.05～0.1) g; The said time of leaving standstill is preferably 1 minute～and 20 minutes, more preferably 2 minutes～15 minutes, most preferably be 3 minutes～10 minutes; The present invention does not have particular restriction to said air tight condition, adopts air tight condition well known to those skilled in the art to get final product; The temperature of said polyreaction is preferably 35 ℃～70 ℃, more preferably 40 ℃～65 ℃, most preferably is 45 ℃～60 ℃; The time of said polyreaction is preferably 3 hours～and 10 hours, more preferably 4 hours～8 hours, most preferably be 5 hours～7 hours.
Obtain after the hydrogel, the present invention is preferably dry with said hydrogel, obtains hygroscopic film.The present invention does not have particular restriction to said exsiccant technical scheme, adopts exsiccant technical scheme well known to those skilled in the art to get final product.The present invention preferably places said hydrogel in the baking oven and dries, and the temperature of said oven dry is preferably 50 ℃～200 ℃, more preferably 55 ℃～180 ℃, most preferably is 60 ℃～160 ℃.
After obtaining hygroscopic film, the present invention tests the moisture absorption capacity of said hygroscopic film.The present invention is the initial mass of weighing hygroscopic film at first, is designated as m
0, load weighted hygroscopic film is placed in the fixed temperature and humidity test box, leave standstill and treat that the hygroscopic film suction is saturated, when promptly the quality of hygroscopic film was constant weight, the quality of weighing hygroscopic film was designated as m
1,, calculate the moisture absorption multiplying power of said hygroscopic film according to the formula shown in the formula (I).In the present invention, the temperature in the said test box is preferably 20 ℃～50 ℃, more preferably 25 ℃～40 ℃; Relative humidity in the said test box is preferably 30%RH～95%RH, more preferably 40%RH～90%RH; The said time of leaving standstill is preferably 0.5 hour～and 5 hours, more preferably 0.8 hour～3 hours.Experimental result shows that the moisture absorption capacity of hygroscopic film provided by the invention is 0.5 times～1.5 times of own wt.
In the formula (I), said N is the moisture absorption multiplying power of hygroscopic material;
Said m
0Initial mass for hygroscopic material;
Said m
1Be the hygroscopic material absorption quality after saturated.
The present invention also tests the moisture absorption dew point of the hygroscopic film that obtains; Test result shows; The moisture absorption dew point of hygroscopic film provided by the invention is only relevant with inorganic modified dose; Along with the increase of inorganic modified agent content, the moisture absorption dew point of hygroscopic film provided by the invention decreases, minimum reaching-27 ℃.
The present invention has carried out high temperature resistant test to said hygroscopic film, and test-results shows that the Heat stability is good of hygroscopic film provided by the invention can bear the high temperature up to 700 ℃; In addition, other performance tests that the hygroscopic film that obtains carries out are found also that hygroscopic film provided by the invention has the advantage that chemical property is stable, physical strength is high from the present invention.
The present invention provides a kind of hygroscopic film, is obtained through polyreaction by olefin(e) acid class polymerization single polymerization monomer, inorganic fibre film and inorganic modified dose; Said inorganic modified dose is silicon-dioxide and/or aluminum oxide.The present invention is a raw material with olefin(e) acid class polymerization single polymerization monomer, inorganic fibre film and inorganic modified dose, and said olefin(e) acid class polymerization single polymerization monomer carries out polyreaction under the condition of inorganic fibre film and inorganic modified dose of existence, obtain hygroscopic film.Wherein the polyolefin acid base polymer that obtains of olefin(e) acid class polymerization monomer polymerization has the certain moisture performance; Said inorganic modified dose of uniform distribution in hygroscopic film, it has bigger specific surface area and stronger absorption property, has further improved the moisture absorption capacity of hygroscopic film.Experimental result shows; The moisture absorption capacity of hygroscopic film provided by the invention is 0.5～1.5 times of own wt; And inorganic modified dose adding makes the moisture absorption dew point of hygroscopic film reduce, and along with the increase of inorganic modified agent content, the moisture absorption dew point of hygroscopic film decreases; The present invention makes the hygroscopic material that obtains have membranaceous characteristic with the support frame of inorganic fibre film as said polyreaction, can satisfy the requirement of special dehumidifying shape, and has improved the physical strength of hygroscopic film.In addition, hygroscopic film provided by the invention has resistance to elevated temperatures preferably.
In order to further specify the present invention, below in conjunction with embodiment hygroscopic film provided by the invention and preparation method thereof is described in detail, but can not they be interpreted as the restriction to protection domain of the present invention.
20.0g vinylformic acid and 10.0g methylacrylic acid are mixed; To wherein adding mass concentration is 10% sodium hydroxide solution; Its pH value is adjusted to 6.0, then to wherein adding 0.015g N, N-DMAA, 0.02g Potassium Persulphate and 0.02g ammonium persulphate; The back that stirs is that 30% silicon dioxide gel and 0.05g solid content are 6% alumina sol to wherein adding the 10g solid content; Stir the back to wherein adding deionized water, make its gross weight reach 100g, obtain the mixing solutions that color is turned white slightly.With thickness is that 0.4mm, surface-area are 7.5cm
2The inorganic glass fiber film be infiltrated in the said mixing solutions, after 5 minutes the inorganic glass fiber film is mentioned, make unnecessary mixing solutions spontaneous current not have the mobile mixing solutions down to inorganic glass fiber film surface.The inorganic glass fiber film that will soak full mixing solutions is positioned in the encloses container, then encloses container is positioned in the baking oven, under 55 ℃ constant temperature, carries out polyreaction, after 6 hours, obtains hydrogel.The hydrogel that obtains is placed in the baking oven, under 75 ℃ of the constant temperature it is dried to constant weight, obtain hygroscopic film.
The present invention carries out hygroscopic property with the hygroscopic film that obtains and measures; Measuring method is following: the hygroscopic film that obtains of 6 parts of quality of weighing present embodiment that is 10g respectively; It is placed respectively in the fixed temperature and humidity test box; The temperature of control in the test box is 35 ℃, and control relative humidity is respectively 90%RH, 80%RH, 70%RH, 60%RH, 50%RH and 40%RH, until the hygroscopic film moisture absorption to constant weight; Mensuration obtains the quality of the hygroscopic film after the moisture absorption, calculates the moisture absorption multiplying power of hygroscopic film according to formula (I).The result is as shown in Figure 1, the moisture absorption capacity of the hygroscopic material that Fig. 1 provides for the embodiment of the invention 1 and comparative example and the relation curve between the relative humidity.Can find out that by Fig. 1 when relative humidity was between 40%RH～70%RH, hygroscopic film that present embodiment obtains and spherical inorganic silica gel moisture adsorbent and membranaceous inorganic hygroscopic material had similar moisture absorption capacity; In relative humidity during greater than 70%RH; The moisture absorption capacity of the hygroscopic film of the embodiment of the invention 1 preparation is out and away greater than the moisture absorption capacity of spherical inorganic silica gel moisture adsorbent and membranaceous inorganic hygroscopic material; Reach as high as 140%, explain that hygroscopic film provided by the invention has excellent hygroscopic property.
The present invention detects the dew point of the hygroscopic film that obtains, and the result shows that the dew point of the hygroscopic film that present embodiment obtains is-25 ℃.
Comparative example 1
The spherical Kiselgel A produced of 6 parts of quality of weighing Qingdao Marine Chemical Co., Ltd. that is 10g respectively; It is placed respectively in the fixed temperature and humidity test box; Temperature in the control test box is 35 ℃; Control relative humidity is respectively 90%RH, 80%RH, 70%RH, 60%RH, 50%RH and 40%RH; To constant weight, mensuration obtains the quality of the spherical inorganic silica gel moisture adsorbent after the moisture absorption until the moisture absorption of spherical inorganic silica gel moisture adsorbent, calculates the moisture absorption capacity of spherical inorganic silica gel moisture adsorbent according to formula (I).
Test result is as shown in Figure 1, the moisture absorption capacity of the hygroscopic material that Fig. 1 provides for the embodiment of the invention 1 and comparative example and the relation curve between the relative humidity.Can find out that by Fig. 1 when relative humidity was between 40%RH～70%RH, the hygroscopic film that the spherical inorganic silica gel moisture adsorbent and the embodiment of the invention 1 obtain had similar moisture absorption capacity; When relative humidity during greater than 70%RH; The moisture absorption capacity of spherical inorganic silica gel moisture adsorbent is out and away less than the moisture absorption capacity of the hygroscopic film of the embodiment of the invention 1 preparation; The moisture absorption capacity of the hygroscopic film of the embodiment of the invention 1 preparation reaches as high as 140%, explains that hygroscopic film provided by the invention has excellent hygroscopic property.
Comparative example 2
The membranaceous inorganic hygroscopic material of honeycomb runner produced of 6 parts of quality of weighing U.S. Roche Co.,Ltd that is 10g respectively; It is placed respectively in the fixed temperature and humidity test box, and the temperature in the control test box is 35 ℃, and control relative humidity is respectively 90%RH, 80%RH, 70%RH, 60%RH, 50%RH and 40%RH; Until membranaceous inorganic hygroscopic material to constant weight; Test obtains the quality of the membranaceous inorganic hygroscopic material after the moisture absorption, according to formula (I), calculates the moisture absorption capacity of membranaceous inorganic hygroscopic material.
Test result is as shown in Figure 1, the moisture absorption capacity of the hygroscopic material that Fig. 1 provides for the embodiment of the invention 1 and comparative example and the relation curve between the relative humidity.Can find out that by Fig. 1 when relative humidity was between 40%RH～70%RH, the hygroscopic film that the membranaceous inorganic hygroscopic material and the embodiment of the invention 1 obtain had similar moisture absorption capacity; When relative humidity during greater than 70%RH; The moisture absorption capacity of membranaceous inorganic hygroscopic material is out and away less than the moisture absorption capacity of the hygroscopic film of the embodiment of the invention 1 preparation; The moisture absorption capacity of the hygroscopic film of the embodiment of the invention 1 preparation is the highest to be carved into 140%, explains that hygroscopic film provided by the invention has excellent hygroscopic property.
Embodiment 2
10.0g vinylformic acid and 6.5g vinylformic acid are mixed, and are 10% sodium hydroxide solution to wherein adding massfraction, and its pH value is adjusted to 4.0.To the pH value that obtains is to add 0.003g N in 4.0 the mixing solutions; N-DMAA, 0.005g Potassium Persulphate and 0.005g ammonium persulphate; The back that stirs is that 30% silicon dioxide gel and 0.05g solid content are 6% alumina sol to wherein adding the 3.3g solid content; Stir the back to wherein adding deionized water, make its gross weight reach 100g, obtain the mixing solutions that color is turned white slightly.With thickness is that 0.45mm, surface-area are 7.0cm
2The inorganic glass fiber film be infiltrated in the mixing solutions, after 5 minutes the inorganic glass fiber film is mentioned, make unnecessary mixing solutions spontaneous current not have the mobile mixing solutions down to inorganic glass fiber film surface.The inorganic glass fiber film that will soak full mixing solutions is positioned in the encloses container, then encloses container is positioned in the baking oven, under 65 ℃ constant temperature, carries out polyreaction, after 5 hours, obtains hydrogel.The hydrogel that obtains is placed in the baking oven, under 55 ℃ of the constant temperature it is dried to constant weight, obtain hygroscopic film.
The present invention carries out the hygroscopic property test with the hygroscopic film that obtains, and test result shows that the moisture absorption multiplying power of the hygroscopic film that present embodiment obtains is 0.9; The present invention detects the dew point of the hygroscopic film that obtains, and the result shows that the dew point of the hygroscopic film that present embodiment obtains is-17 ℃.
15.0g vinylformic acid and 20.0g methylacrylic acid are mixed, and are 10% sodium hydroxide solution to wherein adding massfraction, and its pH value is adjusted to 6.0.To the pH value that obtains is to add 0.021g N in 6.0 the mixing solutions; N-DMAA, 0.03g Potassium Persulphate and 0.03g ammonium persulphate; The back that stirs is that 30% silicon dioxide gel and 0.08g solid content are 6% alumina sol to wherein adding the 6g solid content; Stir the back to wherein adding deionized water, make its gross weight reach 100g, obtain the mixing solutions that color is turned white slightly.With thickness is that 0.38mm, surface-area are 8.0cm
2The inorganic glass fiber film be infiltrated in the mixing solutions, after 8 minutes the inorganic glass fiber film is mentioned, make unnecessary mixing solutions spontaneous current not have the mobile mixing solutions down to inorganic glass fiber film surface.The inorganic glass fiber film that will soak full mixing solutions is positioned in the encloses container, then encloses container is positioned in the baking oven, under 65 ℃ constant temperature, carries out polyreaction, after 6.5 hours, obtains hydrogel.The hydrogel that obtains is placed in the baking oven, under 120 ℃ of the constant temperature it is dried to constant weight, obtain hygroscopic film.
The present invention carries out hygroscopic property with the hygroscopic film that obtains and measures, and measures the result and shows that the moisture absorption multiplying power of the hygroscopic film that present embodiment obtains is 0.75; The present invention detects the dew point of the hygroscopic film that obtains, and the result shows that the dew point of the hygroscopic film that present embodiment obtains is-20 ℃.
Embodiment 4
8.0g vinylformic acid and 17.0g methylacrylic acid are mixed, and are 10% sodium hydroxide solution to wherein adding massfraction, and its pH value is adjusted to 4.0.To the pH value that obtains is to add 0.025g N in 4.0 the mixing solutions; N-DMAA, 0.010g Potassium Persulphate and 0.010g ammonium persulphate; The back that stirs is that 30% silicon dioxide gel and 0.15g solid content are 6% alumina sol to wherein adding the 15g solid content; Stir the back to wherein adding deionized water, make its gross weight reach 100g, obtain the mixing solutions that color is turned white slightly.With thickness is that 0.55mm, surface-area are 6.8cm
2The inorganic glass fiber film be infiltrated in the mixing solutions, after 10 minutes the inorganic glass fiber film is mentioned, make unnecessary mixing solutions spontaneous current not have the mobile mixing solutions down to inorganic glass fiber film surface.The inorganic glass fiber film that will soak full mixing solutions is positioned in the encloses container, then encloses container is positioned in the baking oven, under 65 ℃ constant temperature, carries out polyreaction, after 3.5 hours, obtains hydrogel.The hydrogel that obtains is placed in the baking oven, under 120 ℃ of the constant temperature it is dried to constant weight, obtain hygroscopic film.
The present invention carries out hygroscopic property with the hygroscopic film that obtains and measures, and measures the result and shows that the moisture absorption multiplying power of the hygroscopic film that present embodiment obtains is 0.7; The present invention detects the dew point of the hygroscopic film that obtains, and the result shows that the dew point of the hygroscopic film that present embodiment obtains is-27 ℃.
Embodiment 5
The adding massfraction is 10% sodium hydroxide solution in 35.0g vinylformic acid; Its pH value is adjusted to 5.5, then to wherein adding 0.025g N, N-DMAA, 0.020g Potassium Persulphate and 0.020g ammonium persulphate; The back that stirs is that 30% silicon dioxide gel and 0.30g solid content are 6% alumina sol to wherein adding the 15g solid content; Stir the back to wherein adding deionized water, make gross weight reach 100g, obtain the mixing solutions that color is turned white slightly.With thickness is that 0.55mm, surface-area are 6.0cm
2The inorganic glass fiber film be infiltrated in the mixing solutions, after 7 minutes the inorganic glass fiber film is mentioned, make unnecessary mixing solutions spontaneous current not have the mobile mixing solutions down to inorganic glass fiber film surface.The inorganic glass fiber film that will soak full mixing solutions is positioned in the encloses container, then encloses container is positioned in the baking oven, under 65 ℃ constant temperature, carries out polyreaction, after 7.5 hours, obtains hydrogel.The hydrogel that obtains is placed in the baking oven, under 100 ℃ of the constant temperature it is dried to constant weight, obtain hygroscopic film.
The present invention carries out hygroscopic property with the hygroscopic film that obtains and measures, and measures the result and shows that the moisture absorption multiplying power of the hygroscopic film that present embodiment obtains is 0.5; The present invention detects the dew point of the hygroscopic film that obtains, and the result shows that the dew point of the hygroscopic film that present embodiment obtains is-27 ℃.
Embodiment 6
5.0g vinylformic acid and 5.0g methylacrylic acid are mixed, and are 10% sodium hydroxide solution to wherein adding massfraction, and its pH value is adjusted to 5.5.To the pH value that obtains is to add 0.060g N in 5.5 the mixing solutions; N-DMAA, 0.030g Potassium Persulphate and 0.030g ammonium persulphate; The back that stirs is that 30% silicon dioxide gel and 0.02g solid content are 6% alumina sol to wherein adding the 1g solid content; Stir the back to wherein adding deionized water, make gross weight reach 100g, obtain the mixing solutions that color is turned white slightly.With thickness is that 0.28mm, surface-area are 10cm
2The inorganic glass fiber film be infiltrated in the mixing solutions, after 9 minutes the inorganic glass fiber film is mentioned, make unnecessary mixing solutions spontaneous current not have the mobile mixing solutions down to inorganic glass fiber film surface.The inorganic glass fiber film that will soak full mixing solutions is positioned in the encloses container, then encloses container is positioned in the baking oven, under 65 ℃ constant temperature, carries out polyreaction, after 7.5 hours, obtains hydrogel.The hydrogel that obtains is placed in the baking oven, under 85 ℃ of the constant temperature it is dried to constant weight, obtain hygroscopic film.
The present invention carries out hygroscopic property with the hygroscopic film that obtains and measures, and measures the result and shows that the moisture absorption multiplying power of the hygroscopic film that present embodiment obtains is 1.1; The present invention detects the dew point of the hygroscopic film that obtains, and the result shows that the dew point of the hygroscopic film that present embodiment obtains is-17 ℃.
Embodiment 7
15.0g vinylformic acid and 5.0g methylacrylic acid are mixed, and are 10% sodium hydroxide solution to wherein adding massfraction, and its pH value is adjusted to 4.7.To the pH value that obtains is to add 0.001g N in 4.7 the mixing solutions; N-DMAA, 0.018g Potassium Persulphate and 0.018g ammonium persulphate; The back that stirs is that 30% silicon dioxide gel and 0.008g solid content are 6% alumina sol to wherein adding the 8g solid content; Stir the back to wherein adding deionized water, make gross weight reach 100g, obtain the mixing solutions that color is turned white slightly.With thickness is that 0.3mm, surface-area are 7.5cm
2The inorganic glass fiber film be infiltrated in the mixing solutions, after 10 minutes the inorganic glass fiber film is mentioned, make unnecessary mixing solutions spontaneous current not have the mobile mixing solutions down to inorganic glass fiber film surface.The inorganic glass fiber film that will soak full mixing solutions is positioned in the encloses container, then encloses container is positioned in the baking oven, under 65 ℃ constant temperature, carries out polyreaction, after 8 hours, obtains hydrogel.The hydrogel that obtains is placed in the baking oven, under 145 ℃ of the constant temperature it is dried to constant weight, obtain hygroscopic film.
The present invention carries out hygroscopic property with the hygroscopic film that obtains and measures, and measures the result and shows that the moisture absorption multiplying power of the hygroscopic film that present embodiment obtains is 0.77; The present invention detects the dew point of the hygroscopic film that obtains, and the result shows that the dew point of the hygroscopic film that present embodiment obtains is-22 ℃.
Can know that by above embodiment hygroscopic film provided by the invention is obtained through polyreaction by olefin(e) acid class polymerization single polymerization monomer, inorganic fibre film and inorganic modified dose.In the present invention; Said inorganic modified dose is preferably silicon-dioxide and/or aluminum oxide; Said inorganic modified dose has higher adsorptive power, thereby the hygroscopic film provided by the invention that makes has higher moisture absorption capacity, and hygroscopic property is better; Experimental result shows that the moisture uptake of hygroscopic film provided by the invention can be up to 1.5 times of own wt.In addition, hygroscopic film provided by the invention has lower moisture absorption dew point, higher mechanical properties and higher heat resistance.The preparation method of hygroscopic film provided by the invention is simple, and raw material is simple, and cost is low.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (10)
1. hygroscopic film is obtained through polyreaction by olefin(e) acid class polymerization single polymerization monomer, inorganic fibre film and inorganic modified dose;
Said inorganic modified dose is silicon-dioxide and/or aluminum oxide.
2. hygroscopic film according to claim 1 is characterized in that, said olefin(e) acid class polymerization single polymerization monomer is one or more in vinylformic acid, methylacrylic acid, sodium acrylate and the sodium methacrylate.
3. hygroscopic film according to claim 1 is characterized in that, said inorganic fibre film is inorganic glass fiber film or inorganic ceramic tunica fibrosa.
4. hygroscopic film according to claim 1 is characterized in that, said inorganic modified dose is silicon dioxide gel and/or alumina sol.
5. the preparation method of a hygroscopic film may further comprise the steps:
Olefin(e) acid class polymerization single polymerization monomer and pH value regulator, linking agent, initiator and inorganic modified dose are mixed, obtain the pH value and be 3.0～7.0 mixing solutions;
The inorganic fibre film is infiltrated in the said mixing solutions, obtains hydrogel after the polyreaction;
Said hydrogel is dry, obtain hygroscopic film;
Said inorganic modified dose is silicon-dioxide and/or aluminum oxide.
6. preparation method according to claim 5 is characterized in that, said olefin(e) acid class monomer is one or more in vinylformic acid, methylacrylic acid, sodium acrylate and the sodium methacrylate.
7. preparation method according to claim 5 is characterized in that, said inorganic modified dose is silicon dioxide gel and/or alumina sol.
8. preparation method according to claim 5 is characterized in that, said inorganic fibre film is inorganic glass fiber film or inorganic ceramic tunica fibrosa.
9. preparation method according to claim 5 is characterized in that, the temperature of said polyreaction is 30 ℃～90 ℃.
10. preparation method according to claim 5 is characterized in that, the time of said polyreaction is 1 hour～10 hours.
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