CN108948414A - A kind of aromatic polysulfonamide aeroge and preparation method thereof - Google Patents
A kind of aromatic polysulfonamide aeroge and preparation method thereof Download PDFInfo
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- CN108948414A CN108948414A CN201810644604.8A CN201810644604A CN108948414A CN 108948414 A CN108948414 A CN 108948414A CN 201810644604 A CN201810644604 A CN 201810644604A CN 108948414 A CN108948414 A CN 108948414A
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- aromatic polysulfonamide
- aeroge
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- polysulfonamide
- aromatic
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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
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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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
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
- C08J2201/0482—Elimination of a frozen liquid phase the liquid phase being organic
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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
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
Abstract
The invention discloses a kind of preparation methods of aromatic polysulfonamide aeroge, polymeric aerogels are prepared as raw material using aromatic polysulfonamide chopped strand, aromatic polysulfonamide chopped strand is dissolved in the mixed solution of tetrabutylammonium bromide and dimethyl sulfoxide, organic wet gel is obtained by heating and cooling down, aromatic polysulfonamide aeroge is obtained using aging and freeze-drying, effectively avoid critical conditions and complex process required when monomer synthesis, and method is simple time-consuming short, by utilizing the interaction force between polymeric, form intramolecular or intermolecular hydrogen bond, to connect into three-dimensional net structure, obtained aeroge has intensity high, the small feature of shrinking percentage, further development for the preparation method and application field of polymeric aerogels is had laid a good foundation.
Description
Technical field
The invention belongs to functional material and its preparation fields, and in particular to a kind of aromatic polysulfonamide aeroge and its preparation side
Method.
Background technique
Aeroge is referred to as " ultimate heat-insulation material ", " super sponge ", in international top authoritative scholarly journal " section
Learn " on the 250th phase (2015), aeroge is listed in one of ten big hot topic science and technology, referred to as can change the more of the world
Function new material.By the research of many decades, scientists discovery aeroge can make numerous industries, subject generate qualitative leap,
There is unique advantageous property in mechanics, acoustics, calorifics, optics, chemistry, physics.In building energy conservation, chemical industry, catalysis, safety
The research in the fields such as production, environmental protection, aerospace, military project, sports goods, engineering plastics has been proven that aeroge is wide and answers
Use prospect.Research is most widely SiO for silica-based aerogel2Aeroge is widely used in pollutant absorption water-oil separating etc.
Field, and there is good heat-proof quality, but due to its mechanical property deficiency, limit application range.Different from tradition
Silicon systems aeroge, polymeric aerogels generally all have good mechanical property.According to the good characteristic of polymer itself, knot
Conventional aeroge technology of preparing is closed, the polymeric aerogels material with better performance can be developed.
Currently, common polymeric aerogels material has polyimide aerogels, polyurethane aeroge, polyureas aeroge
Deng.It is synthesized by monomer, adds crosslinking agent, prepared by the way of chemical crosslinking, and pass through exchange of solvent, supercritical drying
It is dry to reduce its shrinking percentage so that experimental period is long, high production cost.Therefore, design a kind of period is short, production cost is low, receive
The low polymeric aerogels preparation method of shrinkage is a research emphasis of aeroge preparation field.
Summary of the invention
The object of the present invention is to provide a kind of aromatic polysulfonamide aeroges and preparation method thereof, by utilizing polymer high score
Interaction force between son forms intramolecular or intermolecular hydrogen bond to connect into three-dimensional net structure and utilizes fiber itself
The characteristic of intrinsic property and prepared aeroge realizes its extensive use.
To achieve the goals above, the technical solution adopted by the present invention is that,
A kind of preparation method of aromatic polysulfonamide aeroge, comprising the following steps:
Step 1, it takes aromatic polysulfonamide chopped strand to wash and dries stand-by to over dry；
Step 2, take tetrabutylammonium bromide that dimethyl sulfoxide, stirring to transparent and homogeneous is added；
Step 3, the resulting aromatic polysulfonamide chopped strand of step 1 is dissolved in the resulting solution of step 2；
Step 4, step 3 gained mixture is heated, obtains aromatic polysulfonamide colloidal sol；
Step 5, step 4 gained aromatic polysulfonamide colloidal sol is cooling to get the organic wet gel for arriving aromatic polysulfonamide fiber；
Step 6, the resulting wet gel of step 5 is obtained into aromatic polysulfonamide aeroge by aging and freeze-drying.
It is washed in step 1 using acetone or dehydrated alcohol, washing times are 3~5 times, aromatic polysulfonamide are chopped fine
Dimension is dried under the conditions of 105 DEG C.
In step 2, the mass ratio of tetrabutylammonium bromide and dimethyl sulfoxide is (3~10): 100.
In the solvent of step 2, combine to obtain with any quaternary ammonium salt containing halogen including dimethyl sulfoxide.
In step 3, the mass ratio of aromatic polysulfonamide chopped strand and dimethyl sulfoxide is (1~3): 100.
In step 4, oil bath heating is used to step 3 gained mixture, heating temperature is 110~140 DEG C, and heating time is
20min。
In step 6, wet gel carries out aging at room temperature, and ageing time is 1d~2d, then does in freeze drier again
Dry 2d.
A kind of aromatic polysulfonamide aeroge, molecular structural formula are as follows:
N is
Positive integer.
Compared with prior art, the present invention at least has the advantages that the present invention provides a kind of aromatic polysulfonamide gas
The preparation method of gel prepares polymeric aerogels as raw material using chopped strand, effectively avoids required when monomer synthesis
Critical conditions and complex process, dimethyl sulfoxide fusing point is high and low boiling point, respectively 18.4 DEG C and 189 DEG C, directly use
The method of freeze-drying removes it, and method is simple time-consuming short, by being formed using the interaction force between polymeric
Intramolecular or intermolecular hydrogen bond, to connect into three-dimensional net structure, obtained aeroge has intensity height, shrinking percentage
Small, the further development for the preparation method and application field of polymeric aerogels is had laid a good foundation.
Detailed description of the invention
Fig. 1 is the strand change procedure prepared in aerogel process；
Fig. 2 is aeroge ageing process schematic diagram prepared by the present invention.
Fig. 3 is aromatic polysulfonamide aeroge load-deformation curve prepared by the embodiment of the present invention 3.
Specific embodiment
The present invention is further explained in detail combined with specific embodiments below.
A kind of preparation method of aromatic polysulfonamide aeroge, specifically includes the following steps:
Step 1, take aromatic polysulfonamide chopped strand wash, washed with dehydrated alcohol or acetone, washing times be 3~
5 times, it is stand-by that aromatic polysulfonamide chopped strand is dried to over dry under the conditions of 105 DEG C；
Step 2, it takes tetrabutylammonium bromide that dimethyl sulfoxide is added, dimethyl is added with preset ratio in tetrabutylammonium bromide
Sulfoxide, mechanical stirring to homogeneous and transparent solution, wherein the mass ratio of tetrabutylammonium bromide and dimethyl sulfoxide is (3~10):
100；
Step 3, the resulting aromatic polysulfonamide chopped strand of step 1 is dissolved in the resulting solution of step 2, aromatic polysulfonamide
The mass ratio of chopped strand and dimethyl sulfoxide is (1~3): 100；
Step 4, step 3 gained mixture is heated, mixture uses oil bath heating, and temperature is 110 DEG C~140 DEG C, obtains
To aromatic polysulfonamide colloidal sol；
Step 5, step 4 gained aromatic polysulfonamide colloidal sol is cooling to get the organic wet gel for arriving aromatic polysulfonamide fiber；
Step 6, the resulting wet gel of step 5 is obtained into aromatic polysulfonamide aeroge by aging and freeze-drying, it is wet
Gel ageing time is 1-2d, then dries 2d in freeze drier again, prepares the strand change procedure in aerogel process
As shown in Figure 1, wet gel ageing process is as shown in Figure 2.
The molecular structure of the aromatic polysulfonamide aeroge obtained using preparation method of the present invention is as follows:
N is
Positive integer.
Dimethyl sulfoxide fusing point height and low boiling point, respectively 18.4 DEG C and 189 DEG C, directly will using the method for freeze-drying
It is removed.
Embodiment 1
0.6g tetrabutylammonium bromide is dissolved in 20mL by the preparation method of one of the present embodiment aromatic polysulfonamide aeroge
In dimethyl sulfoxide, 0.2g aromatic polysulfonamide chopped strand is then added and is heated to 130 DEG C, obtains faint yellow colloidal liquid, it will
The liquid is cooling, forms gel, makes its aging 1d at room temperature, reuses the dry 2d of freeze drier, obtains aromatic polysulfonamide
Aeroge.
The present embodiment experimental period is 72h；After tested, the aromatic polysulfonamide aeroge compressive strength of the preparation of embodiment 1 is
0.30Mpa, compression rebound rate are 80%.
Embodiment 2
The preparation method of polymeric aerogels of one of the present embodiment based on aromatic polysulfonamide chopped strand, by 1g tetra-
Butylammonium bromide is dissolved in 20mL dimethyl sulfoxide, and 0.4g aromatic polysulfonamide chopped strand is then added, is heated to 120 DEG C, obtains
It is cooling to the liquid to faint yellow colloidal liquid, gel is formed, its aging 1d at room temperature is made, it is dry to reuse freeze drier
Dry 2d to get arrive aromatic polysulfonamide aeroge.
The present embodiment experimental period is 72h；After tested, the aromatic polysulfonamide aeroge compressive strength of the preparation of embodiment 2 is
1.11Mpa, compression rebound rate are 75%.
Embodiment 3
2g tetrabutylammonium bromide is dissolved in 20mL bis- by the preparation method of one of the present embodiment aromatic polysulfonamide aeroge
In methyl sulfoxide, 0.6g aromatic polysulfonamide chopped strand is then added, is heated to 140 DEG C, faint yellow colloidal liquid is obtained, to this
Liquid is cooling, forms gel, makes its aging 1d at room temperature, reuses the dry 2d of freeze drier to get aromatic polysulfonamide is arrived
Aeroge.
The present embodiment experimental period is 72h, and after tested, aromatic polysulfonamide aeroge compressive strength prepared by embodiment 3 is
3.16Mpa as shown in Figure 3；Compression rebound rate is 73%.
Embodiment 4
1.2g tetrabutylammonium bromide is dissolved in 20mL by the preparation method of one of the present embodiment aromatic polysulfonamide aeroge
In dimethyl sulfoxide, 0.4g aromatic polysulfonamide chopped strand is then added, is heated to 140 DEG C, obtains faint yellow colloidal liquid, to
The liquid is cooling, forms gel, makes its aging 1d at room temperature, reuses the dry 2d of freeze drier to get polyarylsulfone (PAS) acyl is arrived
Amine aeroge.
The present embodiment experimental period is 72h；After tested, the aromatic polysulfonamide aeroge compressive strength of the preparation of embodiment 3 is
2.13Mpa, compression rebound rate are 75%.
Embodiment 5
1.6g tetrabutylammonium bromide is dissolved in 20mL by the preparation method of one of the present embodiment aromatic polysulfonamide aeroge
In dimethyl sulfoxide, 0.6g aromatic polysulfonamide chopped strand is then added, is heated to 140 DEG C, obtains faint yellow colloidal liquid, to
The liquid is cooling, forms gel, makes its aging 1d at room temperature, reuses the dry 2d of freeze drier, obtains aromatic polysulfonamide
Aeroge.
The present embodiment experimental period is 72h, and after tested, aromatic polysulfonamide aeroge compressive strength prepared by embodiment 3 is
3.28Mpa, compression rebound rate are 72%.
Claims (8)
1. a kind of preparation method of aromatic polysulfonamide aeroge, which comprises the following steps:
Step 1, it takes aromatic polysulfonamide chopped strand to wash and dries stand-by to over dry；
Step 2, take tetrabutylammonium bromide that dimethyl sulfoxide, stirring to transparent and homogeneous is added；
Step 3, the resulting aromatic polysulfonamide chopped strand of step 1 is dissolved in the resulting solution of step 2；
Step 4, step 3 gained mixture is heated, obtains aromatic polysulfonamide colloidal sol；
Step 5, step 4 gained aromatic polysulfonamide colloidal sol is cooling to get the organic wet gel for arriving aromatic polysulfonamide fiber；
Step 6, the resulting wet gel of step 5 is obtained into aromatic polysulfonamide aeroge by aging and freeze-drying.
2. the preparation method of aromatic polysulfonamide aeroge according to claim 1, which is characterized in that use third in step 1
Ketone or dehydrated alcohol are washed, and washing times are 3~5 times, and aromatic polysulfonamide chopped strand is dried under the conditions of 105 DEG C.
3. the preparation method of aromatic polysulfonamide aeroge according to claim 1, which is characterized in that in step 2, the tetrabutyl
The mass ratio of ammonium bromide and dimethyl sulfoxide is (3~10): 100.
4. the preparation method of aromatic polysulfonamide aeroge according to claim 1, which is characterized in that in the solvent of step 2,
It combines to obtain with any quaternary ammonium salt containing halogen including dimethyl sulfoxide.
5. the preparation method of aromatic polysulfonamide aeroge according to claim 1, which is characterized in that in step 3, polyarylsulfone (PAS)
The mass ratio of amide chopped strand and dimethyl sulfoxide is (1~3): 100.
6. the preparation method of aromatic polysulfonamide aeroge according to claim 1, which is characterized in that in step 4, to step
3 gained mixtures use oil bath heating, and heating temperature is 110~140 DEG C, heating time 20min.
7. the preparation method of aromatic polysulfonamide aeroge according to claim 1, which is characterized in that in step 6, wet gel
Aging is carried out at room temperature, and ageing time is 1d~2d, then dries 2d in freeze drier again.
8. the aromatic polysulfonamide aeroge obtained using any one of claim 1~7 preparation method, which is characterized in that point
Subformula are as follows:
Wherein n is positive integer.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554548A (en) * | 2013-10-24 | 2014-02-05 | 华南理工大学 | Preparation method of wood fiber biomass aerogel |
| WO2017116598A1 (en) * | 2015-12-30 | 2017-07-06 | The Regents Of The University Of Michigan | Gels and nanocomposites containing aramid nanofibers |
-
2018
- 2018-06-21 CN CN201810644604.8A patent/CN108948414A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554548A (en) * | 2013-10-24 | 2014-02-05 | 华南理工大学 | Preparation method of wood fiber biomass aerogel |
| WO2017116598A1 (en) * | 2015-12-30 | 2017-07-06 | The Regents Of The University Of Michigan | Gels and nanocomposites containing aramid nanofibers |
Non-Patent Citations (3)
| Title |
|---|
| DU L, ET AL.: ""A new nanoporous aramid fiber aerogel"", 《SEN I GAKKAISHI》 * |
| SHAO ZZ,ET AL.: ""Preparation of p-aramid aerogels using supercritical CO2"", 《SEN I GAKKAISHI》 * |
| 胡宏玫等: "《非石棉垫片复合材料设计与性能》", 31 March 2006, 上海大学出版社 * |
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Application publication date: 20181207 |