CN112359483A - Polyimide thermal insulation flocculus and preparation method thereof - Google Patents
Polyimide thermal insulation flocculus and preparation method thereof Download PDFInfo
- Publication number
- CN112359483A CN112359483A CN202011110795.3A CN202011110795A CN112359483A CN 112359483 A CN112359483 A CN 112359483A CN 202011110795 A CN202011110795 A CN 202011110795A CN 112359483 A CN112359483 A CN 112359483A
- Authority
- CN
- China
- Prior art keywords
- polyimide
- flocculus
- fibers
- heat
- insulation layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4374—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece using different kinds of webs, e.g. by layering webs
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/44—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
- D04H1/46—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/44—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
- D04H1/46—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
- D04H1/492—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres by fluid jet
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/58—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives
- D04H1/593—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives to layered webs
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention discloses a polyimide heat-insulating flocculus and a preparation method thereof, wherein the flocculus at least comprises a heat-insulating layer formed by porous polyimide fibers and a heat-insulating layer formed by blending one or more of cellulose fibers, polyester fibers and polyamide fibers with the porous polyimide fibers. In the preparation method, the flocculus is prepared by opening, forming and lapping fibers, wherein the porous polyimide component is prepared by performing thermal imidization on polyamide acid protofilaments after the opening or forming step. The polyimide heat insulation flocculus provided by the invention adopts the polyimide fiber with a porous structure to enhance the heat insulation capability, and simultaneously adjusts the thermal imidization step in the preparation process, so as to avoid the damage to the porous structure of the fiber caused by premature thermal imidization, and ensure that the prepared flocculus has the optimal heat insulation effect.
Description
Technical Field
The invention belongs to the field of polyimide materials, and particularly relates to a polyimide thermal insulation flocculus and a preparation method thereof.
Background
In recent years, the application field of fiber products is gradually expanded, and some high-performance fibers are widely applied to the aerospace military industry and civil markets, and the porous polyimide fiber flocculus is representative of the high-performance fibers. For military personnel who train in the field for a long time and perform tasks and astronauts who carry people in space flight and narrow space stations, when the personnel work for a long time, after sweating and heat extraction on the body surface, the water vapor is condensed into water vapor to collect in the heat-insulating layer after meeting cold, the more the water vapor, the more the heat-insulating property is reduced, and the more the heat-insulating property of traditional materials such as down feather, cotton and the like is reduced by more than 50%. The corresponding solution is to make the materials such as down and cotton undergo the water-repellent treatment, but the water-repellent property of the post-treatment will be reduced with the washing times.
The flocculus felt serving as a warm-keeping filling material is widely applied to a series of cold-proof products such as cold-proof clothes, cold-proof quilts and the like, the flocculus felt in the market mainly adopts polyester fibers as a raw material, the application field of high-performance fiber flocculus products is enlarged year by year, and the flocculus felt has wide military and civil markets. The porous polyimide fiber is different from common polyimide fibers in domestic and foreign markets, a plurality of porous spaces are distributed in the fiber and on the surface of the fiber, due to the special physical structure of the porous polyimide fiber, an air heat insulation layer is formed in the fiber, the density is lower, the number of the fibers is more under the condition of the same quality, the structure of the formed inner space is denser, the heat insulation effect and the heat insulation effect are improved, the porous polyimide fiber is particularly suitable for the cold environment with severe conditions, and a new selection scheme is provided for the market of flocculus felts.
The preparation of the flocculus felt usually needs to carry out operations such as opening and carding on fibers, the process can cause certain damage to the fibers, and the polyimide fibers are not very compact in monofilament structure due to the porous structure of the polyimide fibers, and can be damaged and destroyed to a certain degree in the flocculus preparation process.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a polyimide heat-insulation flocculus and a preparation method thereof, wherein the flocculus comprises a heat-insulation layer formed by porous polyimide fibers and a heat-insulation layer formed by blending one or more of cellulose fibers, polyester fibers and polyamide fibers with the porous polyimide fibers, and the porous polyimide component in the flocculus is prepared by performing thermal imidization on polyamide acid protofilaments after the step of opening or forming a net in the flocculus preparation process.
In order to solve the technical problems, the invention adopts the technical scheme that:
the invention provides a polyimide heat-insulating flocculus which at least comprises a heat-insulating layer formed by porous polyimide fibers and a heat-insulating layer formed by blending one or more of cellulose fibers, polyester fibers and polyamide fibers with the porous polyimide fibers; the heat-insulating layer comprises 60-90 wt% of porous polyimide fibers and 10-40 wt% of other fibers.
In the scheme, the components in the flocculus mainly comprise porous polyimide fibers, warm air can be wrapped in the fibers by the porous polyimide fibers, the body temperature is kept, the external cold air is isolated, and the prepared flocculus has permanent heat-insulating property, is warmer than the same light flocculus and is an excellent functional heat-insulating fabric.
The further scheme of the invention is as follows: the part of the porous polyimide fiber, which is close to the periphery of the radial section, is in a hole shape, the part, which is close to the center of the radial section, is solid, and the area ratio of the hole part to the solid part on the radial section is 0.7-1.2: 1.
In the above scheme, the hole part in the polyimide is close to the periphery of the fiber, and the occupied area of the hole part on the radial cross section of the fiber is relatively large, so that the fiber structure is deviated and loose, and after a fabric is formed, a plurality of air heat insulation layers can be generated to play a good heat insulation effect.
The further scheme of the invention is as follows: the gram weight of the flocculus is 800-1000 g/m2The thickness is 1-100 mm, and the heat preservation quantity is not less than 2m2·K/W。
The invention also provides a preparation method of the polyimide heat-preservation flocculus, wherein the flocculus is prepared by opening, forming and laying fibers, and the porous polyimide component in the flocculus is prepared by thermally imidizing polyamide acid precursor after the opening or forming step.
In the scheme, the hole parts of the porous polyimide fibers are mostly arranged at the positions close to the periphery of the fibers, when the flocculus is prepared subsequently, the porous structure can be greatly damaged by the tearing, beating and dividing actions in the opening and loosening process, and the porous structure can be damaged to a certain extent by the actions of the working roller and the roller in the later carding process. In addition, thermal imidization also causes damage to the porous structure formed during the curing of the polyamic acid fiber. The heat preservation effect of the polyimide flocculus is just from an air heat insulation layer brought by a porous structure of the polyimide flocculus, so that the order of thermal imidization treatment is adjusted, and the polyamide acid protofilaments are loosened or formed into a net and then subjected to thermal imidization treatment, so that the porous structure is prevented from being further damaged by premature thermal imidization.
According to the preparation method, the thermal imidization adopts a gradient heating mode, and the time and the temperature of the polyamide acid protofilament passing through each temperature zone are respectively as follows: the temperature of the first temperature zone is 210-230 ℃ for 3.5-4.5 min, the temperature of the second temperature zone is 380-420 ℃ for 1.5-3 min, and the temperature of the third temperature zone is 550-600 ℃ for 1-2 min.
In the scheme, the structure of the polyamide acid protofilament is more complex compared with that of a monofilament after opening or opening and net forming, so that three-stage gradient thermal imidization is adopted, and imidization of the polyamide acid protofilament is more uniform and thorough; the adoption of the gradient mode can also make the imidization process more stable and avoid the damage of excessive porous structures.
According to the preparation method, the polyamide acid protofilaments are subjected to thermal imidization treatment after opening and web forming, and then are subjected to web laying to prepare a heat insulation layer in the flocculus; preferably, the web is formed by a carding machine.
According to the preparation method, the polyamide acid protofilaments are subjected to thermal imidization treatment after being opened, and are mixed with one or more of opened cellulose fibers, polyester fibers and polyamide fibers, and then the mixed fibers are subjected to web formation and lapping to prepare the heat insulation layer in the flocculus; preferably, the net formation is air-laid.
In the scheme, in the preparation process of the heat insulation layer, the polyamide acid protofilaments are subjected to thermal imidization treatment after opening and web forming, and the web forming can be carried out by a carding machine after the thermal imidization is carried out after the opening and web forming. The heat-insulating layer is prepared by mixing polyimide fibers and other fibers, and the other fibers cannot resist high-temperature treatment of thermal imidization, so that the polyamide acid fibers are subjected to thermal imidization after opening and then are mixed with the other fibers, and the damage of contact such as friction to a fiber porous structure can be reduced by adopting an air-laid mode.
According to the preparation method, the heat insulation layer and the heat preservation layer are combined into the flocculus through a needling, spunlace or viscose process, and the thickness ratio of the heat insulation layer to the heat preservation layer is 1-1.3: 2-2.5.
In the scheme, the adhesive process sprays adhesive on the adhesive surface of the heat-insulating layer or the heat-insulating layer, and then the flocculus is prepared by processes of heating forming, shaping, ironing and the like.
According to the preparation method, cross lapping or vertical lapping is adopted for lapping.
According to the preparation method, the polyamic acid protofilament is prepared by solidifying a spinning solution formed by condensation polymerization of dianhydride and diamine in a solvent at 40-80 ℃, wherein the solvent is selected from dimethyl sulfoxide or N-methyl pyrrolidone, and the coagulating bath comprises one or more of water, ethylene glycol, xylene or acetone.
In the scheme, the dianhydride is selected from one of pyromellitic dianhydride, benzophenone tetracarboxylic dianhydride or diphenyl ether dianhydride; the diamine is o-phenylenediamine or m-phenylenediamine.
Specifically, the polyimide heat-insulating flocculus is prepared by the following method:
(1) preparing a heat insulation layer: opening and carding polyamide acid protofilaments into a net, then performing gradient thermal imidization treatment, and sending the treated fiber net into a lapping machine to prepare a heat insulation layer;
(2) preparing a heat insulation layer: opening polyamide acid protofilaments, performing gradient thermal imidization treatment, mixing with one or more of opened cellulose fibers, polyester fibers and polyamide fibers, and then forming and paving a net on the mixed fibers to obtain a heat-insulating layer;
(3) and (3) merging the layers: combining the heat insulation layer and the heat insulation layer into a flocculus by adopting a needling, spunlace or viscose process, wherein the thickness ratio of the heat insulation layer to the heat insulation layer is 1-1.3: 2-2.5.
The flocculus comprises the porous polyimide fiber and other types of fibers, so that the heat retention rate and the Crohn value of the flocculus felt can be obviously improved, the heat retention performance of the flocculus felt is greatly improved under the condition of the same areal density, and the novel porous polyimide fiber heat-retention flocculus provides a new filling scheme for a cold-proof tool and has a better heat-retention effect. Meanwhile, the porous polyimide fiber has natural water repellency, the heat preservation performance can not be reduced due to the sweat and heat extraction of the body surface, the porous polyimide fiber flocculus felt has excellent heat preservation performance and flame retardant performance, the heat preservation performance is provided, the flexibility is not reduced, and the flame retardant performance is realized.
After adopting the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. the preparation method of the polyimide flocculus adjusts the thermal imidization step so as to avoid the damage to the porous structure of the fiber caused by the premature thermal imidization, so that the prepared flocculus has the optimal heat preservation and insulation effect;
2. the preparation method of the polyimide flocculus adopts three-stage gradient thermal imidization reaction, so that imidization of the polyamide acid protofilament is more uniform and thorough, the imidization process is more stable, and excessive porous structures are prevented from being damaged.
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention, are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention without limiting the invention to the right. It is obvious that the drawings in the following description are only some embodiments, and that for a person skilled in the art, other drawings can be derived from them without inventive effort. In the drawings:
FIG. 1 is a schematic representation of the radial cross-sectional structure of polyimide fibers in a batt of the present invention;
FIG. 2 is a schematic representation of the radial cross-sectional structure of polyimide fibers in a batt of the present invention;
FIG. 3 is a pictorial representation of a batt of the present invention.
It should be noted that the drawings and the description are not intended to limit the scope of the inventive concept in any way, but to illustrate it by a person skilled in the art with reference to specific embodiments.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and the following embodiments are used for illustrating the present invention and are not intended to limit the scope of the present invention.
Example 1
In this example, cellulose batting was prepared as follows:
(1) preparing a heat insulation layer: opening and carding polyamide acid protofilaments to form a web, then performing gradient thermal imidization treatment, and sending the treated web to a lapping machine to prepare a heat insulation layer, wherein the gradient thermal imidization comprises the following steps: the polyamide acid fiber takes 4.5min to pass through a first temperature zone with the temperature of 210 ℃, then takes 3min to pass through a second temperature zone with the temperature of 420 ℃, and finally takes 1min to pass through a third temperature zone with the temperature of 550 ℃;
(2) preparing a heat insulation layer: opening polyamic acid protofilament, then performing gradient thermal imidization treatment, uniformly mixing the polyamic acid protofilament with one or more of opened cotton fiber (belonging to cellulose fiber, commercially available product), polyester fiber and polyamide fiber, and then performing web formation and laying on the mixed fiber to obtain a heat-insulating layer, wherein the gradient thermal imidization comprises the following steps: the polyamide acid fiber takes 3.5min to pass through a first temperature zone with the temperature of 215 ℃, then takes 2min to pass through a second temperature zone with the temperature of 400 ℃, and finally takes 1.5min to pass through a third temperature zone with the temperature of 600 ℃, and the mass ratio of the polyimide fiber to other fibers in the heat-insulating layer is 90: 10;
(3) and (3) merging the layers: the heat insulation layer and the heat insulation layer with the thickness ratio of 1.3:2 are combined into a flocculus by adopting a needling process.
The batt prepared in this example had a grammage of 900g/m2Thickness of 10mm and heat preservation of 2.07m2·K/W。
Example 2
In this example, cellulose batting was prepared as follows:
(1) preparing a heat insulation layer: opening and carding polyamide acid protofilaments to form a web, then performing gradient thermal imidization treatment, and sending the treated web to a lapping machine to prepare a heat insulation layer, wherein the gradient thermal imidization comprises the following steps: the polyamide acid fiber takes 4.5min to pass through a first temperature zone with the temperature of 230 ℃, then takes 1.5min to pass through a second temperature zone with the temperature of 420 ℃, and finally takes 1min to pass through a third temperature zone with the temperature of 550 ℃;
(2) preparing a heat insulation layer: carrying out gradient thermal imidization treatment after opening polyamic acid protofilament, uniformly mixing the polyamic acid protofilament with opened bamboo fiber (belonging to cellulose fiber, commercially available products), and then forming and lapping the mixed fiber to obtain a heat-insulating layer, wherein the gradient thermal imidization comprises the following steps of: the polyamide acid fiber takes 4min to pass through a first temperature zone with the temperature of 225 ℃, then takes 2min to pass through a second temperature zone with the temperature of 400 ℃, and finally takes 1.5min to pass through a third temperature zone with the temperature of 580 ℃, and the mass ratio of the polyimide fiber to other fibers in the heat-insulating layer is 90: 10;
(3) and (3) merging the layers: the thermal insulation layer and the heat insulation layer with the thickness ratio of 1.3:2.5 are combined into a flocculus by adopting a spunlace process.
The grammage of the flakes prepared in this example was 1000g/m2The thickness is 98mm, and the heat preservation quantity is 2.23m2·K/W。
Example 3
In this example, cellulose batting was prepared as follows:
(1) preparing a heat insulation layer: opening and carding polyamide acid protofilaments to form a web, then performing gradient thermal imidization treatment, and sending the treated web to a lapping machine to prepare a heat insulation layer, wherein the gradient thermal imidization comprises the following steps: the polyamide acid fiber takes 3.5min to pass through a first temperature zone with the temperature of 210 ℃, then takes 1.5min to pass through a second temperature zone with the temperature of 420 ℃, and finally takes 1min to pass through a third temperature zone with the temperature of 600 ℃;
(2) preparing a heat insulation layer: carrying out gradient thermal imidization treatment after opening polyamic acid protofilament, uniformly mixing the polyamic acid protofilament with opened terylene (belonging to polyester fiber, sold in the market), and then forming and lapping the mixed fiber to prepare a heat-insulating layer, wherein the gradient thermal imidization comprises the following steps of: the polyamide acid fiber takes 4.5min to pass through a first temperature zone with the temperature of 220 ℃, then takes 3min to pass through a second temperature zone with the temperature of 380 ℃, and finally takes 2min to pass through a third temperature zone with the temperature of 590 ℃, and the mass ratio of the polyimide fiber to other fibers in the heat-insulating layer is 80: 20;
(3) and (3) merging the layers: and combining the heat insulating layer and the heat insulating layer with the thickness ratio of 1:2.3 into a flocculus by adopting an adhesive process.
The batt prepared in this example had a grammage of 850g/m2The thickness is 85mm, and the heat preservation quantity is 2.13m2·K/W。
Example 4
In this example, cellulose batting was prepared as follows:
(1) preparing a heat insulation layer: opening and carding polyamide acid protofilaments to form a web, then performing gradient thermal imidization treatment, and sending the treated web to a lapping machine to prepare a heat insulation layer, wherein the gradient thermal imidization comprises the following steps: the polyamide acid fiber takes 4min to pass through a first temperature zone with the temperature of 220 ℃, then takes 2.5min to pass through a second temperature zone with the temperature of 390 ℃, and finally takes 1.5min to pass through a third temperature zone with the temperature of 580 ℃;
(2) preparing a heat insulation layer: opening polyamide acid protofilament, then carrying out gradient thermal imidization treatment, uniformly mixing the polyamide acid protofilament with opened polyamide (belonging to polyamide fiber, commercially available products), and then forming a net and paving the net on the mixed fiber to obtain the heat-insulating layer, wherein the gradient thermal imidization comprises the following steps: the polyamide acid fiber takes 4min to pass through a first temperature zone with the temperature of 230 ℃, then takes 2min to pass through a second temperature zone with the temperature of 410 ℃, and finally takes 1min to pass through a third temperature zone with the temperature of 600 ℃, and the mass ratio of the polyimide fiber to other fibers in the heat-insulating layer is 60: 40;
(3) and (3) merging the layers: the heat insulation layer and the heat insulation layer with the thickness ratio of 1.1:2 are combined into a flocculus by adopting a needling process.
The grammage of the batt prepared in this example was 950g/m2The thickness is 53mm, and the heat preservation quantity is 2.11m2·K/W。
Example 5
In this example, cellulose batting was prepared as follows:
(1) preparing a heat insulation layer: opening and carding polyamide acid protofilaments to form a web, then performing gradient thermal imidization treatment, and sending the treated web to a lapping machine to prepare a heat insulation layer, wherein the gradient thermal imidization comprises the following steps: the polyamide acid fiber takes 3.5min to pass through a first temperature zone with the temperature of 210 ℃, then takes 1.5min to pass through a second temperature zone with the temperature of 420 ℃, and finally takes 1min to pass through a third temperature zone with the temperature of 600 ℃;
(2) preparing a heat insulation layer: carrying out gradient thermal imidization treatment after opening polyamic acid protofilament, uniformly mixing the polyamic acid protofilament with opened terylene (belonging to polyester fiber, sold in the market), and then forming and lapping the mixed fiber to prepare a heat-insulating layer, wherein the gradient thermal imidization comprises the following steps of: the polyamide acid fiber takes 4.5min to pass through a first temperature zone with the temperature of 220 ℃, then takes 3min to pass through a second temperature zone with the temperature of 380 ℃, and finally takes 2min to pass through a third temperature zone with the temperature of 590 ℃, and the mass ratio of the polyimide fiber to other fibers in the heat-insulating layer is 80: 20;
(3) and (3) merging the layers: the heat insulation layer and the heat insulation layer with the thickness ratio of 1.2:2.1 are combined into a flocculus by adopting a spunlace process.
The batt prepared in this example had a grammage of 800g/m215mm in thickness and 2.10m in heat preservation2·K/W。
Comparative example 1
This comparative example was conducted by adjusting the thermal imidization steps in steps (1) and (2) to be before opening, i.e., by subjecting the polyamic acid precursor fiber to a gradient thermal imidization step, based on example 3, and then obtaining a batt according to the embodiment of example 3.
Experimental example 1
In this experimental example, the performance of the batts prepared in examples 1 to 5 and comparative example 1 was tested, specifically including the mass per unit area (tested by the method described in FZ/T60003) and the kr value (tested by the method described in GB/T11048-2008), and the results are shown in the following table:
| mass per unit area (g/m)2) | Crohn value (m)2·K/W) | |
| Example 1 | 900 | 2.07 |
| Example 2 | 1000 | 2.23 |
| Example 3 | 850 | 2.13 |
| Example 4 | 950 | 2.11 |
| Example 5 | 800 | 2.10 |
| Comparative example 1 | 850 | 1.63 |
As can be seen from the above table, the flocculus provided in the embodiment of the present invention has a higher clo value because the imidization treatment process of the polyamic acid precursor fiber is delayed in the preparation process of the flocculus, so that the porous structure of the polyimide fiber is prevented from being damaged too much, and the finally prepared flocculus has a good heat preservation effect. Comparative example 1 the polyamide acid precursor fiber was heat imidized before opening, which resulted in the destruction of some of the porous structure in the polyamide acid precursor fiber, which resulted in further damage to the porous structure of the polyimide fiber during subsequent opening and web formation, and the insulation of the finally obtained batt was inferior to that of example 3.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The polyimide heat-insulation flocculus is characterized by at least comprising a heat-insulation layer formed by porous polyimide fibers and a heat-insulation layer formed by blending one or more of cellulose fibers, polyester fibers and polyamide fibers with the porous polyimide fibers; the heat-insulating layer comprises 60-90 wt% of porous polyimide fibers and 10-40 wt% of other fibers.
2. The polyimide insulation batt of claim 1, wherein the porous polyimide fibers are porous at a portion near the outer periphery of the radial cross section, solid at a portion near the center of the radial cross section, and the ratio of the area occupied by the porous portion to the solid portion in the radial cross section is 0.7-1.2: 1.
3. The polyimide insulation batt of claim 2, wherein the batt has a grammage of 800 to 1000g/m2The thickness is 10-100 mm, and the heat preservation quantity is not less than 2m2·K/W。
4. A method for preparing the polyimide insulation flocculus according to any one of claims 1 to 3, wherein the flocculus is prepared by opening, forming and lapping fibers, and the porous polyimide component in the flocculus is prepared by performing thermal imidization on polyamide acid precursor after the opening or forming step.
5. The preparation method of the polyimide thermal insulation flocculus according to claim 4, wherein the thermal imidization is performed by a gradient heating method, and the time and the temperature of the polyamic acid protofilament passing through each temperature zone are respectively as follows:
the temperature of the first temperature zone is 210-230 ℃ for 3.5-4.5 min, the temperature of the second temperature zone is 380-420 ℃ for 1.5-3 min, and the temperature of the third temperature zone is 550-600 ℃ for 1-2 min.
6. The method for preparing the polyimide insulation flocculus according to claim 4, wherein the polyamic acid protofilament is subjected to thermal imidization treatment after opening and web forming, and then is subjected to web laying to prepare the insulation layer in the flocculus;
preferably, the web is formed by a carding machine.
7. The method for preparing the polyimide thermal insulation flocculus according to claim 4, wherein the polyamide acid precursor is subjected to thermal imidization treatment after opening and is mixed with one or more of the opened cellulose fiber, the polyester fiber and the polyamide fiber, and then the mixed fiber is subjected to web forming and laying to prepare the thermal insulation layer in the flocculus;
preferably, the net formation is air-laid.
8. The preparation method of the polyimide insulation flocculus according to claim 6 or 7, wherein the insulation layer and the insulation layer are combined into the flocculus through a needling, spunlace or viscose process, and the thickness ratio of the insulation layer to the insulation layer is 1-1.3: 2-2.5.
9. The method for preparing the polyimide thermal insulation flocculus according to claim 6 or 7, wherein the lapping adopts cross lapping or vertical lapping.
10. The method for preparing the polyimide thermal insulation flocculus according to claim 4, wherein the polyamic acid precursor is prepared by curing a spinning solution obtained by polycondensation of dianhydride and diamine in a solvent at 40-80 ℃, wherein the solvent is selected from dimethyl sulfoxide or N-methyl pyrrolidone, and the coagulation bath comprises one or more of water, ethylene glycol, xylene or acetone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011110795.3A CN112359483B (en) | 2020-10-16 | 2020-10-16 | Polyimide thermal insulation flocculus and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011110795.3A CN112359483B (en) | 2020-10-16 | 2020-10-16 | Polyimide thermal insulation flocculus and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112359483A true CN112359483A (en) | 2021-02-12 |
| CN112359483B CN112359483B (en) | 2022-03-04 |
Family
ID=74506786
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011110795.3A Active CN112359483B (en) | 2020-10-16 | 2020-10-16 | Polyimide thermal insulation flocculus and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112359483B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114103365A (en) * | 2021-12-13 | 2022-03-01 | 厦门安踏体育用品有限公司 | Lightweight warming functional flocculus and preparation method thereof |
| CN114232205A (en) * | 2021-12-27 | 2022-03-25 | 厦门安踏体育用品有限公司 | Multidimensional thermal cotton with heat reflection function and production method and application thereof |
| CN114262982A (en) * | 2022-01-06 | 2022-04-01 | 北京金轮沃德科技有限公司 | Flame-retardant windproof flocculus and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104178837A (en) * | 2013-05-28 | 2014-12-03 | 北京航空航天大学 | Porous polyimide fiber and preparation method thereof |
| KR20160126893A (en) * | 2015-04-22 | 2016-11-02 | 동화 바이텍스 주식회사 | Felt Manufacturing Method for Nano Membrane Cartridge Bag Filter using Electrospinning |
| CN106591999A (en) * | 2015-10-19 | 2017-04-26 | 中国石油化工股份有限公司 | Preparation method of polyimide fiber |
| CN208630022U (en) * | 2018-08-01 | 2019-03-22 | 江苏奥神新材料股份有限公司 | A kind of fire-retardant warm keeping blanket of polyimides |
| CN109778424A (en) * | 2019-02-26 | 2019-05-21 | 段宇晶 | Phase transformation insulation flocculus and preparation method thereof |
| CN209368469U (en) * | 2018-09-03 | 2019-09-10 | 上海伊贝纳纺织品有限公司 | A kind of warming carbonization type flocculus of permanent fire retardant |
-
2020
- 2020-10-16 CN CN202011110795.3A patent/CN112359483B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104178837A (en) * | 2013-05-28 | 2014-12-03 | 北京航空航天大学 | Porous polyimide fiber and preparation method thereof |
| KR20160126893A (en) * | 2015-04-22 | 2016-11-02 | 동화 바이텍스 주식회사 | Felt Manufacturing Method for Nano Membrane Cartridge Bag Filter using Electrospinning |
| CN106591999A (en) * | 2015-10-19 | 2017-04-26 | 中国石油化工股份有限公司 | Preparation method of polyimide fiber |
| CN208630022U (en) * | 2018-08-01 | 2019-03-22 | 江苏奥神新材料股份有限公司 | A kind of fire-retardant warm keeping blanket of polyimides |
| CN209368469U (en) * | 2018-09-03 | 2019-09-10 | 上海伊贝纳纺织品有限公司 | A kind of warming carbonization type flocculus of permanent fire retardant |
| CN109778424A (en) * | 2019-02-26 | 2019-05-21 | 段宇晶 | Phase transformation insulation flocculus and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 何建新: "《新型纤维材料学》", 31 July 2014, 东华大学出版社 * |
| 孙卫国: "《纺纱技术》", 31 July 2005, 中国纺织出版社 * |
| 高连勋: "《聚酰亚胺纤维》", 31 May 2017, 国防工业出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114103365A (en) * | 2021-12-13 | 2022-03-01 | 厦门安踏体育用品有限公司 | Lightweight warming functional flocculus and preparation method thereof |
| CN114232205A (en) * | 2021-12-27 | 2022-03-25 | 厦门安踏体育用品有限公司 | Multidimensional thermal cotton with heat reflection function and production method and application thereof |
| CN114232205B (en) * | 2021-12-27 | 2023-09-22 | 厦门安踏体育用品有限公司 | Multidimensional thermal insulation cotton with heat reflection function and production method and application thereof |
| CN114262982A (en) * | 2022-01-06 | 2022-04-01 | 北京金轮沃德科技有限公司 | Flame-retardant windproof flocculus and preparation method thereof |
| CN114262982B (en) * | 2022-01-06 | 2022-10-25 | 北京金轮沃德科技有限公司 | Flame-retardant windproof flocculus and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112359483B (en) | 2022-03-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112359483B (en) | Polyimide thermal insulation flocculus and preparation method thereof | |
| KR20080090570A (en) | Extensible absorbent composites | |
| CN104911809A (en) | Profiled fiber non-woven fabric and manufacturing method thereof | |
| CN101457444B (en) | Nonwoven flax cloth sandwich and method for producing the same | |
| KR101669204B1 (en) | Graphite sheet and method for preparing same | |
| CN102268782A (en) | Method for producing leather fiber base cloth | |
| US6112385A (en) | Process for manufacturing a non-woven fabric by hydrodynamic needling, and product of said manufacturing process | |
| KR20100129987A (en) | Polypropylene spunbond nonwoven fabric and the preparing process thereof | |
| CN114277506B (en) | Pre-oxidized silk hot air cotton and preparation method thereof | |
| CN103757936A (en) | Production method of collagen and sea-island fiber leather | |
| KR101050831B1 (en) | Cleaning nonwoven fabric and manufacturing method thereof | |
| CN104452102A (en) | Technology for processing natural kapok fiber hot-rolled non-woven cloth | |
| CN105297284B (en) | A kind of manufacture method of nonwoven needled jacquard pad | |
| CN108505215B (en) | Degradable hot air non-woven fabric and preparation method thereof | |
| KR101977472B1 (en) | Multilayer nonwoven fabric insulation material comprising long-fiber nonwoven fabric and method of making same | |
| CN110616509B (en) | Novel spun-bonded spunlace non-woven fabric for spring wrapping cloth and preparation method thereof | |
| CN115074917A (en) | Novel bacterium-blocking breathable fabric and preparation method thereof | |
| CN110804877B (en) | Polyurethane impregnating solution and super-thick high-gram-weight superfine fiber synthetic leather base cloth prepared from same | |
| CN113186645A (en) | Demoulded breathable felt and preparation method and application thereof | |
| CN109881420B (en) | Tentering and heat setting process for spun-bonded spunlace non-woven fabric | |
| CN114261161A (en) | Multi-layer composite fabric for down jackets and preparation method thereof | |
| CN114575168A (en) | Preparation method of synthetic leather and synthetic leather | |
| CN111996667A (en) | Tough environment-friendly type carex meyeriana non-woven fabric with good heat preservation performance and preparation method thereof | |
| CN108823789B (en) | Net-free quilt and processing method thereof | |
| CN206251963U (en) | A kind of thermal insulation layer for fire-entry suit |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |