CN110042504A - Cyclodextrin composite ceramics presoma and preparation method with gel spinning function - Google Patents
Cyclodextrin composite ceramics presoma and preparation method with gel spinning function Download PDFInfo
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- CN110042504A CN110042504A CN201910192439.1A CN201910192439A CN110042504A CN 110042504 A CN110042504 A CN 110042504A CN 201910192439 A CN201910192439 A CN 201910192439A CN 110042504 A CN110042504 A CN 110042504A
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- cyclodextrin
- solution
- gel
- preparation
- inducing agents
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/10—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material by decomposition of organic substances
Abstract
Present disclose provides a kind of cyclodextrin composite ceramics presoma and preparation method thereof with gel spinning function.The cyclodextrin composite ceramics presoma with gel spinning function that the disclosure provides includes element polymer, cyclodextrin and gel inducing agents, or is prepared according to following methods: in a solvent by element polymer dissolution, being configured to element polymer solution；Gel inducing agents are added to element polymer solution, are configured to element polymer-gel inducing agents solution；In a solvent by cyclodextrin, it is configured to cyclodextrin solution；Cyclodextrin solution is added to element polymer-gel inducing agents solution, stirs evenly, forms cyclodextrin composite ceramics precursor sol；And heating cyclodextrin composite ceramics precursor sol forms cyclodextrin composite ceramics aqueous precursor gel so that gel inducing agents and cyclodextrin assemble.
Description
Technical field
This disclosure relates to a kind of cyclodextrin composite ceramics presoma and preparation method thereof with gel spinning function.
Background technique
Ceramic fibre is a kind of light weight, high temperature resistant, one kind that thermal stability is good, thermal conductivity is low, specific heat is small, intensity is high
Fibrous material.Due to having the above excellent comprehensive performance, ceramic fibre is in machinery, metallurgy, chemical industry, petroleum, electronics, aviation
The industries such as space flight, national defence are all widely used.From composition, ceramic fibre mainly include ceramic alumina fiber,
Zirconia ceramics fiber, silicon nitride ceramics fiber, silicon carbide ceramic fiber, boride ceramics fiber etc..The fiber of different components,
Its high temperature resistance, corrosion resistance, dielectric constant, radiation resistance, mechanical strength etc. are all not quite similar, therefore its each self-application
Advantage be also not quite similar.In addition, the ceramic fibre of identical type, preparation method, the presoma type of use and rear place
The different of reason process also have important influence to Properties of Ceramic Fiber.
By taking alumina fibre as an example, alumina fibre is the inorfil that a kind of main ingredient is aluminium oxide, crystal form packet
γ-, δ-, θ-, Alpha-alumina etc. are included, different crystal forms, high temperature resistance difference is greatly.It is a certain amount of by being introduced in presoma
Silica, can stablize the crystal phase of aluminium oxide, inhibit growing up for crystal grain under high temperature, principal crystalline phase is corundum and a small amount of mullite
Phase, using temperature up to 1400 DEG C or more.
Equally, using different spinning techniques, diameter, length, microscopic appearance of fiber etc. be not also identical.So far,
The spining technology of ceramic fibre mainly has melt spinning, high speed centrifugation to get rid of the techniques such as silk.Compared with macromolecule organic fiber, ceramics
The spinning process type of fiber is few, threshold is high, is also not easy to realize regulation to fiber morphology and microstructure.
Using solution wet spinning, it can be achieved that the continuous spinning of organic macromolecule high-volume, Dispersion relation, it can also be used to prepare
Superfine fibre (diameter is less than 1 micron), profiled filament, porous fibre, doughnut etc..For ceramic fibre, then it is difficult to realize
The various patterns of similar macromolecular fibre and form control, thus cause the promotion in performance cannot achieve.It is above-mentioned in order to realize
Purpose, critical issue be to synthesize a kind of ceramic forerunner for being suitable for solution-polymerized SBR, however so far before this ceramics
Driving body yet there are no report.
Summary of the invention
In order to solve at least one above-mentioned technical problem, present disclose provides a kind of cyclodextrin with gel spinning function
Composite ceramics presoma and preparation method thereof.
According to the disclosure in a first aspect, a kind of preparation of the cyclodextrin composite ceramics presoma with gel spinning function
Method comprising in a solvent by element polymer dissolution, be configured to element polymer solution；It is added to element polymer solution
Gel inducing agents are configured to element polymer-gel inducing agents solution；In a solvent by cyclodextrin, it is configured to cyclodextrin
Solution；Cyclodextrin solution is added to element polymer-gel inducing agents solution, stirs evenly, before forming cyclodextrin composite ceramics
Drive body colloidal sol；And heating cyclodextrin composite ceramics precursor sol forms ring paste so that gel inducing agents and cyclodextrin assemble
Smart composite ceramics aqueous precursor gel.
According at least one embodiment of the disclosure, element polymer includes poly- silicon-carbon alkane, poly- silicon borine, poly- silicon nitrogen
Alkane, PVDF hollow fiber membrane, the poly- silicon-carbon alkane containing metal any one, two or more any mixture.
According at least one embodiment of the disclosure, gel inducing agents include that line style of the average molecular weight greater than 1000 is poly-
Silicon-carbon alkane, poly- silicon borine, polysilazane, containing the poly- silicon-carbon alkane of metal and line style organic polymer polyethylene glycol, polypropylene glycol,
Polycaprolactone, polystyrene, polypropylene, polycarbonate, polyvinyl chloride any one, two or more any mixing
Object.
According at least one embodiment of the disclosure, solvent includes that alkane, alkene, aromatic series organic reagent, heterocycle have
Machine molecule, dimethylformamide (DMF) or dimethyl sulfoxide (DMSO).
According at least one embodiment of the disclosure, the mass concentration of element polymer is in element polymer solution
1%~30% and/or element polymer-gel inducing agents solution in gel inducing agents mass concentration be 0.5%~20%.
According at least one embodiment of the disclosure, cyclodextrin includes appointing for α-, β-, gamma-cyclodextrin and its derivative
It anticipates two or more a kind of, any mixture.
According at least one embodiment of the disclosure, cyclodextrin solution and element polymer-gel inducing agents solution
Volume ratio is 1:10~1:50.
According at least one embodiment of the disclosure, the speed of stirring is 500~3000rpm, the time of stirring is 1~
24 hours.
According at least one embodiment of the disclosure, heating includes baking oven heating, heating water bath or oil bath heating；With/
Or the target temperature of heating is 50~80 DEG C；And/or the heating rate of heating is 1 DEG C/min to 15 DEG C/min.
According to the second aspect of the disclosure, a kind of cyclodextrin composite ceramics presoma with gel spinning function, packet
Include element polymer, cyclodextrin and gel inducing agents；Or it is prepared according to above-mentioned any preparation method.
Detailed description of the invention
Attached drawing shows the illustrative embodiments of the disclosure, and it is bright together for explaining the principles of this disclosure,
Which includes these attached drawings to provide further understanding of the disclosure, and attached drawing is included in the description and constitutes this
Part of specification.
Fig. 1 is the preparation method route map according to the ceramic forerunner of the disclosure at least one embodiment.
Fig. 2 is molten according to the cyclodextrin composite ceramics presoma with gel spinning function of the acquisition of the embodiment of the present disclosure 1
The picture of glue.
Fig. 3 is coagulated according to the cyclodextrin composite ceramics presoma with gel spinning function that the embodiment of the present disclosure 1 obtains
The picture of glue.
Fig. 4 is the cyclodextrin composite ceramics presoma with gel spinning function obtained according to the embodiment of the present disclosure 3
Scanning electron microscope diagram.
Fig. 5 is molten according to the cyclodextrin composite ceramics presoma with gel spinning function of the acquisition of the embodiment of the present disclosure 4
The scanning electron microscope diagram of glue.
Fig. 6 is the cyclodextrin composite ceramics presoma with gel spinning function obtained according to the embodiment of the present disclosure 5
Scanning electron microscope diagram.
Fig. 7 is molten according to the cyclodextrin composite ceramics presoma with gel spinning function of the acquisition of the embodiment of the present disclosure 6
The scanning electron microscope diagram of glue.
Specific embodiment
The disclosure is described in further detail with embodiment with reference to the accompanying drawing.It is understood that this place
The specific embodiment of description is only used for explaining related content, rather than the restriction to the disclosure.It also should be noted that being
Convenient for description, part relevant to the disclosure is illustrated only in attached drawing.
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the disclosure can
To be combined with each other.The disclosure is described in detail below with reference to the accompanying drawings and in conjunction with embodiment.
In at least one embodiment of the disclosure, present disclose provides a kind of cyclodextrin with gel spinning function
Composite ceramics presoma and preparation method thereof.
According to the disclosure in a first aspect, a kind of preparation of the cyclodextrin composite ceramics presoma with gel spinning function
Method, as shown in Figure 1 comprising in a solvent by element polymer dissolution, be configured to element polymer solution；To element high score
Gel inducing agents are added in sub- solution, are configured to element polymer-gel inducing agents solution；In a solvent by cyclodextrin, match
Cyclodextrin solution is made；Cyclodextrin solution is added to element polymer-gel inducing agents solution, stirs evenly, forms cyclodextrin
Composite ceramics precursor sol；And heating cyclodextrin composite ceramics precursor sol, so that gel inducing agents and cyclodextrin group
Dress forms cyclodextrin composite ceramics aqueous precursor gel.
According at least one embodiment of the disclosure, element polymer includes poly- silicon-carbon alkane, poly- silicon borine, poly- silicon nitrogen
Alkane, PVDF hollow fiber membrane, the poly- silicon-carbon alkane containing metal any one, two or more any mixture.
Gel inducing agents include line style poly- silicon-carbon alkane of the average molecular weight greater than 1000, poly- silicon borine, polysilazane, contain gold
Belong to poly- silicon-carbon alkane and line style organic polymer polyethylene glycol, polypropylene glycol, polycaprolactone, polystyrene, polypropylene, poly- carbon
Acid esters, polyvinyl chloride any one, two or more any mixture.
Solvent includes alkane, alkene, aromatic series organic reagent, heterocyclic organic molecule, dimethylformamide (DMF) or diformazan
Base sulfoxide (DMSO).
Cyclodextrin includes any one of α-, β-, gamma-cyclodextrin and its derivative, arbitrarily two or more is mixed
Object is closed, and without being limited thereto.
According at least one embodiment of the disclosure, the mass concentration of element polymer is in element polymer solution
1%~30% and/or element polymer-gel inducing agents solution in gel inducing agents mass concentration be 0.5%~20%.
Cyclodextrin solution and element polymer solution solvent for use are same reagent, and cyclodextrin solution and element are high
Molecule-gel inducing agents solution volume ratio is 1:10~1:50.
According at least one embodiment of the disclosure, the speed of stirring is 500~3000rpm, the time of stirring is 1~
24 hours.
The mode of heating cyclodextrin composite ceramics precursor sol includes baking oven heating, heating water bath or oil bath heating, is added
The target temperature of heat is 50~80 DEG C, and heating rate is 1 DEG C/min to 15 DEG C/min.
According to the second aspect of the disclosure, a kind of cyclodextrin composite ceramics presoma with gel spinning function, packet
Include element polymer, cyclodextrin and gel inducing agents；Or it is prepared according to above-mentioned any preparation method.
The technical solution of the disclosure is further described below by way of several embodiments and in conjunction with attached drawing.However, selected
Embodiment be merely to illustrate the disclosure, without limiting the scope of the present disclosure.
Embodiment 1:
It takes 1 gram of poly- silicon-carbon alkane to be substantially dissolved in it in 99 grams of toluene, it is molten to be prepared into the poly- silicon-carbon alkane that mass fraction is 1%
Liquid A, then 0.5 gram of poly- silicon borine is added thereto, it stirs 30 minutes under magnetic stirring, is prepared into element polymer-gel and lures
Lead agent composite solution.10 grams of gamma-cyclodextrins are dissolved in 100 grams of toluene, then by volume ratio be 1:10 cyclodextrin solution with
Above-mentioned composite solution mixing, stirs 24 hours at 500 rpm, is then statically placed in water-bath, with the heating rate of 1 DEG C/min
50 DEG C are heated to, the cyclodextrin composite ceramics presoma with sol-gel spinning function is prepared.The ceramic forerunner
Colloidal sol figure and gel figure difference are referring to figs. 2 and 3.
Embodiment 2:
It takes 30 grams of poly- silicon-carbon alkane to be substantially dissolved in it in 100 grams of metacresols, is prepared into the poly- silicon that mass fraction is 23%
Carbon alkane solution A, then the polyethylene glycol that 5 gram-molecular weights are 2000 is added thereto, it stirs 30 minutes, is prepared under magnetic stirring
Element polymer-gel inducing agents composite solution.5 grams of gamma-cyclodextrins are dissolved in 100 grams of metacresols, then be by volume ratio
The gamma-cyclodextrin solution of 1:50 is mixed with above-mentioned composite solution, is stirred 14 hours, is then statically placed in baking oven at 1500 rpm,
With the heating rate of 5 DEG C/min to 80 DEG C, the cyclodextrin composite ceramics forerunner with sol-gel spinning function is prepared
Body.
Embodiment 3:
It takes 1 gram of polysilazane to be substantially dissolved in it in 99 grams of hexamethylenes, is prepared into the polysilazane that mass fraction is 1%
Solution A, then the polycaprolactone that 1 gram-molecular weight is 20000 is added thereto, it stirs 30 minutes under magnetic stirring, is prepared into member
Plain macromolecule-gel inducing agents composite solution.15 grams of beta-cyclodextrins are dissolved in 1000 grams of hexamethylenes, then by volume ratio be 1:
20 beta-cyclodextrin solution is mixed with above-mentioned composite solution, is stirred 1 hour, is then statically placed in baking oven, with 15 at 3,000 rpm
DEG C/heating rate of min to 80 DEG C, the cyclodextrin composite ceramics presoma with sol-gel spinning function is prepared.It should
The scanning electron microscope diagram of ceramic forerunner colloidal sol is referring to fig. 4.
Embodiment 4:
Take 10 grams of PVDF hollow fiber membranes to be substantially dissolved in it in 80 grams of dimethylbenzene, be prepared into mass fraction be 11.1% it is poly-
Borosilicate azane solution A, then the polypropylene glycol that 0.5 gram-molecular weight is 5000 is added thereto, it stirs 60 minutes under magnetic stirring,
It is prepared into element polymer-gel inducing agents composite solution.5 grams of alpha-cyclodextrins are dissolved in 150 grams of dimethylbenzene, then by volume
Than being mixed for the alpha-cyclodextrin solution of 1:30 with above-mentioned composite solution, is stirred 10 hours at 2000rpm, be then statically placed in oil bath
In pot, with the heating rate of 10 DEG C/min to 70 DEG C, the cyclodextrin composite ceramics with sol-gel spinning function are prepared
Presoma.The scanning electron microscope diagram of the ceramic forerunner colloidal sol is referring to Fig. 5.
Embodiment 5:
It takes 20 grams of polysilazanes to be substantially dissolved in it in 80 grams of octanes, is prepared into the polysilazane that mass fraction is 20%
Solution A, then the polypropylene that 25 gram-molecular weights are 10000 is added thereto, it stirs 120 minutes under magnetic stirring, is prepared into member
Plain macromolecule-gel inducing agents composite solution.5 grams of methyl beta-cyclodextrins are dissolved in 100 grams of octanes, then by volume ratio be 1:
40 methyl beta-cyclodextrin solution is mixed with above-mentioned composite solution, is stirred 20 hours at 1000rpm, is then statically placed in oil bath pan
In, with the heating rate of 5 DEG C/min to 70 DEG C, before the cyclodextrin composite ceramics with sol-gel spinning function are prepared
Drive body.The scanning electron microscope diagram of the ceramic forerunner colloidal sol is referring to Fig. 6.
Embodiment 6:
It takes 30 grams of poly- silicon-carbon alkane to be substantially dissolved in it in 70 grams of dimethylbenzene, is prepared into the poly- silicon-carbon that mass fraction is 30%
Alkane solution A, then the polystyrene that 4 gram-molecular weights are 10000 is added thereto, it stirs 120 minutes, is prepared under magnetic stirring
Element polymer-gel inducing agents composite solution.5 grams of gamma-cyclodextrins are dissolved in 100 grams of dimethylbenzene, then be by volume ratio
The gamma-cyclodextrin solution of 1:20 is mixed with above-mentioned composite solution, is stirred 22 hours at 800 rpm, is then statically placed in oil bath pan
In, with the heating rate of 15 DEG C/min to 60 DEG C, before the cyclodextrin composite ceramics with sol-gel spinning function are prepared
Drive body.The scanning electron microscope diagram of the ceramic forerunner colloidal sol refers to Fig. 7.
In view of the deficiencies of the prior art with the limitation of material, present disclose provides a kind of cyclodextrin composite ceramics forerunners
Body has the function of sol-gel spinning, directly can form gelatinous fibre through sol-gel transition spinning, or colloidal sol-occurs
Gel conversion forms injection aquagel ceramic forerunner, can be used for the serialization solution-polymerized SBR of ceramic fibre, room temperature dry method is spun
Silk and centrifugal drying silk.Have using the cyclodextrin composite ceramics presoma with sol-gel spinning function that the disclosure provides
Hope the continuous spinning preparation for realizing special-shaped ceramics fiber, porous ceramic fiber.
It will be understood by those of skill in the art that above embodiment is used for the purpose of clearly demonstrating the disclosure, and simultaneously
Non- be defined to the scope of the present disclosure.For those skilled in the art, may be used also on the basis of disclosed above
To make other variations or modification, and these variations or modification are still in the scope of the present disclosure.
Claims (10)
1. a kind of preparation method of the cyclodextrin composite ceramics presoma with gel spinning function, which is characterized in that the system
Preparation Method includes
In a solvent by element polymer dissolution, it is configured to element polymer solution；
Gel inducing agents are added to the element polymer solution, are configured to element polymer-gel inducing agents solution；
By cyclodextrin in the solvent, it is configured to cyclodextrin solution；
The cyclodextrin solution is added to the element polymer-gel inducing agents solution, stirs evenly, it is compound to form cyclodextrin
Ceramic forerunner colloidal sol；And
The cyclodextrin composite ceramics precursor sol is heated, so that the gel inducing agents and the cyclodextrin assemble, is formed
Cyclodextrin composite ceramics aqueous precursor gel.
2. preparation method according to claim 1, which is characterized in that the element polymer includes poly- silicon-carbon alkane, poly- silicon
Borine, polysilazane, PVDF hollow fiber membrane, the poly- silicon-carbon alkane containing metal any one, two or more any mixture.
3. preparation method according to claim 1, which is characterized in that the gel inducing agents include that average molecular weight is greater than
The poly- silicon-carbon alkane of 1000 line style, polysilazane, contains the poly- silicon-carbon alkane of metal and the poly- second two of line style organic polymer at poly- silicon borine
Alcohol, polypropylene glycol, polycaprolactone, polystyrene, polypropylene, polycarbonate, polyvinyl chloride any one, it is two kinds or two any
Kind or more mixture.
4. preparation method according to claim 1, which is characterized in that the solvent includes that alkane, alkene, aromatic series are organic
Reagent, heterocyclic organic molecule, dimethylformamide or dimethyl sulfoxide.
5. preparation method according to claim 1, which is characterized in that element high score described in the element polymer solution
The mass concentration of son is the quality of gel inducing agents described in 1%~30% and/or element polymer-gel inducing agents solution
Concentration is 0.5%~20%.
6. preparation method according to claim 1, which is characterized in that the cyclodextrin include α-, β-, gamma-cyclodextrin and
Its derivative any one, two or more any mixture.
7. preparation method according to claim 1, which is characterized in that the cyclodextrin solution and the element polymer-
The volume ratio of gel inducing agents solution is 1:10~1:50.
8. preparation method according to claim 1, which is characterized in that the speed of the stirring is 500~3000rpm, is stirred
The time mixed is 1~24 hour.
9. preparation method according to claim 1, which is characterized in that it is described heating include baking oven heating, heating water bath or
Oil bath heating；And/or the target temperature of the heating is 50~80 DEG C；And/or the heating rate of the heating be 1 DEG C/min extremely
15℃/min。
10. a kind of cyclodextrin composite ceramics presoma with gel spinning function, which is characterized in that the cyclodextrin composite ceramic
Porcelain presoma includes the element polymer, the cyclodextrin and the gel inducing agents；Or before the cyclodextrin composite ceramics
Body is driven to be prepared to 9 described in any item preparation methods according to claim 1.
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