CN110528272B - Polyimide fiber fibrillation treatment method - Google Patents
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/76—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon oxides or carbonates
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/15—Proteins or derivatives thereof
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/70—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment combined with mechanical treatment
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
The invention relates to a polyimide fiber fibrillation treatment method, and belongs to the technical field of papermaking. The method comprises the steps of blending short-cut polyimide fibers, protein micro-nano powder and calcium carbonate powder to form a mixture, putting the blended mixture into a grinding device for grinding, adding NaOH solution into the ground mixture to separate the protein micro-nano powder, adding HCl solution to separate the calcium carbonate powder to obtain fibrillated polyimide fibers, and rubbing the polyimide fibers, the protein micro-nano powder and the calcium carbonate powder to generate static electricity to adsorb the protein micro-nano powder and the calcium carbonate powder onto the polyimide fibers in the grinding process, so that the polyimide fibers are separated, the probability of agglomeration of the polyimide fibers in the grinding device is reduced, the efficiency of grinding treatment of the polyimide fibers is improved, the production time is reduced, and a large amount of production cost is saved.
Description
Technical Field
The invention relates to a polyimide fiber fibrillation treatment method, and belongs to the technical field of papermaking.
Background
The polyimide fiber has excellent heat resistance, low temperature resistance, insulation, oxidation resistance, ultraviolet resistance, radiation resistance, stable chemical property, high strength, high toughness, high modulus, strong creep resistance, excellent friction performance, no toxicity, good water absorption, corrosion resistance and other excellent performances, so the polyimide fiber has wide application in a plurality of fields of environmental protection, aerospace, special and high temperature heat insulation, machinery, electrical appliances, chemical industry, microelectronics and the like, and the polyimide fiber also has wide application as a material of special paper in recent years. The polyimide fiber is required to be processed into an ultrashort polyimide fiber form with the length of 1-2mm in the process of applying the polyimide fiber to papermaking, but the conventional preparation of the polyimide fiber into the ultra-short polyimide fiber with the length of 1-2mm still has the problem of low efficiency, because the official moisture regain of the polyimide fiber is low, the conductivity is low under the conventional temperature and humidity conditions, static electricity is easily generated due to mutual friction among the polyimide fibers, the polyimide fibers are easily intertwined and cohered to form a group, the polyimide fiber has extremely strong toughness and is difficult to be ground off, so the volume of cohesive groups of the polyimide fiber is increased in the grinding process, the grinding treatment of the polyimide fiber is influenced finally, and the long-time grinding treatment is needed to slowly reduce the conglomerate volume of the polyimide fiber to the ultra-short polyimide fiber with the length of 1-2 mm. For example, chinese patent publication No. CN107675288A, published 2018, 2, and 9, entitled "an ultrashort polyimide fiber and a method for preparing the same", discloses that in a process of preparing a polyimide fiber, the dispersion and ultrashort characteristics of the fiber are more easily achieved by a physical mechanical method in a state where the polyimide fiber is not completely imidized, then the complete imidization is achieved by high temperature treatment, and finally the ultrashort polyimide fiber is obtained by a method of mechanical crushing, grinding and sieving again. The method has the disadvantages that in the process, the polyimide fiber needs to be subjected to eight-step physical and chemical treatment to form the polyimide ultrashort fiber, the operation is complex, the efficiency is low, and the production cost is increased.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a method for fibrillating polyimide fibers, which comprises:
a polyimide fiber fibrillation treatment method comprises the steps of polyimide fiber chopping in a polyimide fiber fibrillation process, polyimide fiber disintegration treatment, wherein the polyimide fiber disintegration treatment is to add calcium carbonate powder with the particle size of 5-20 mu m and protein micro-nano powder with the particle size of 0.1-5 mu m into a polyimide fiber disintegration device with the diameter of 10-40 mu m and the length of 6000 mu m after chopping, add the calcium carbonate powder and the protein micro-nano powder into the disintegration device for disintegration treatment for 90-120min, add NaOH solution with the concentration of 0.01% into the polyimide fiber, the calcium carbonate powder and the protein micro-nano powder after disintegration for dissolution, separate and dry the mixture in a filtering device to obtain the polyimide fiber and the calcium carbonate powder, add HCl with the concentration of 0.03% into the mixture of the polyimide fiber and the calcium carbonate powder for dissolution of the calcium carbonate powder, separating the polyimide fibers in a filtering device and drying to obtain fibrillated polyimide fibers;
the mass percentages of the protein micro-nano powder and the calcium carbonate powder added into the polyimide fiber are respectively as follows:
5 to 30 percent of polyimide fiber
40 to 50 percent of protein micro-nano powder
30 to 45 percent of calcium carbonate powder
The protein micro-nano powder is wool powder or silk powder.
Due to the adoption of the technical scheme, the protein micro-nano powder and the calcium carbonate powder are added into the polyimide fiber for blending on the premise of not changing the conventional polyimide fiber fibrillation treatment process, so that the added protein micro-nano powder and the added calcium carbonate powder are placed in a grinding and decomposing device along with the polyimide fiber for grinding and decomposing treatment. Because the official moisture regain of polyimide fiber is low, under the conventional humiture condition, the conductivity is low, and conventional mode grinds and separates, produces static between polyimide fiber and the polyimide fiber to make cohesion group between the polyimide fiber, reduced the area of contact of the face of grinding and separating, increased the time of grinding and separating, reduced the efficiency of grinding and separating. When the protein micro-nano powder and the calcium carbonate powder are added into the polyimide fibers, the protein micro-nano powder and the calcium carbonate powder are mutually rubbed to generate static electricity, the protein micro-nano powder and the calcium carbonate powder are small in size and light in weight relative to the polyimide fibers, the protein micro-nano powder and the calcium carbonate powder can be adsorbed on the surfaces of the polyimide fibers, the polyimide fibers are separated due to the existence of the protein micro-nano powder and the calcium carbonate powder, and the polyimide fibers are filled with the protein micro-nano powder and the calcium carbonate powder.
The protein micro-nano powder, the calcium carbonate powder and the polyimide fiber mixture are ground, the probability of mutual entanglement and cohesion of polyimide fibers is reduced, and the mutual entanglement and cohesion of polyimide fibers in the same time is small, so that the time required by polyimide fiber fibrillation is shortened, the problem that the polyimide fibers are entangled and conglobated due to static electricity is solved, and the grinding efficiency of the polyimide fibers is improved.
The micro-nano powder of protein is less for calcium carbonate powder's particle diameter, when the polyimide fiber is ground and separate, calcium carbonate powder is preferred to be ground and separate with the polyimide fiber, the micro-nano powder of protein fills between calcium carbonate powder's space afterwards, grind with the polyimide fiber and separate, thereby make the indirect polyimide fiber pass through the micro-nano powder of protein and calcium carbonate powder and completely with grind the mutual contact who separates the device, compare with the technology that conventional polyimide fiber ground and separate, the area of contact between polyimide fiber and the device of grinding and separating has been increased, the polyimide fiber is ground and separate the probability further to have increased, the fibrillation efficiency of polyimide fiber has been improved.
Meanwhile, the calcium carbonate powder has higher hardness and the protein micro-nano powder has lower hardness, when the content ratio of the calcium carbonate powder is 30-49 percent and the content ratio of the protein micro-nano powder is 40-50 percent, the protein micro-nano powder, the calcium carbonate powder and the polyimide fiber have hard grinding decomposition of the calcium carbonate powder and the polyimide fiber and also have soft grinding decomposition of the protein micro-nano powder and the polyimide fiber during grinding decomposition, the polyimide fiber has higher breakage degree due to the hard grinding decomposition of the calcium carbonate powder and the polyimide fiber, then the polyimide fiber breakage part obtains the grinding decomposition with lower degree due to the soft grinding decomposition of the protein micro-nano powder and the polyimide fiber, and the polyimide fiber realizes fibrillation during grinding decomposition due to the synergistic effect of the protein micro-nano powder and the calcium carbonate powder, the method effectively prevents the polyimide fiber from directly jumping from the fiber to fibrillate and directly reaching the state of the powder due to the hard grinding decomposition of the calcium carbonate powder, and also solves the problem of low efficiency caused by the soft grinding decomposition of the protein micro-nano powder.
Therefore, by adopting the technical scheme, the protein micro-nano powder with small particle size and small hardness and the calcium carbonate powder with large particle size and large hardness are added to accompany and grind the polyimide fibers, so that the volume and the agglomeration probability of the polyimide fibers, which are caused by static electricity, are reduced, the polyimide fibers are prevented from being completely ground to be in a powder state, the polyimide fiber fibrillation efficiency is improved, the polyimide fiber fibrillation time is shortened, and the production cost is reduced.
Drawings
FIG. 1 is an electron micrograph of a polyimide fiber sample.
FIG. 2 is an electron micrograph of a polyimide fiber after fibrillation in example 12.
Detailed Description
The polyimide fiber fibrillation treatment method according to the present invention will be described in further detail with reference to the following specific examples:
a polyimide fiber fibrillation treatment method comprises polyimide fiber chopping and polyimide fiber fibrillation treatment in a polyimide fiber fibrillation process, wherein the polyimide fiber disintegration treatment is to add calcium carbonate powder with the particle size of 5-20 mu m and protein micro-nano powder with the particle size of 0.1-5 mu m into a polyimide fiber disintegration device with the diameter of 10-40 mu m and the length of 6000 mu m after chopping for disintegration treatment in the disintegration device for 90-120min, add NaOH solution with the concentration of 0.01% into the disintegrated polyimide fiber, calcium carbonate powder and protein micro-nano powder for dissolution, separate and dry in a filter device to obtain polyimide fiber and calcium carbonate powder, add HCl with the concentration of 0.03% into the obtained mixture of the polyimide fiber and the calcium carbonate powder for dissolution of the calcium carbonate powder, separating the polyimide fibers in a filtering device and drying to obtain fibrillated polyimide fibers;
the mass percentages of the protein micro-nano powder and the calcium carbonate powder added into the polyimide fiber are respectively as follows:
5 to 30 percent of polyimide fiber
40 to 50 percent of protein micro-nano powder
30 to 45 percent of calcium carbonate powder
The protein micro-nano powder is wool powder or silk powder.
The protein micro-nano powder and the calcium carbonate powder are added to carry out companion grinding with the polyimide fibers and then are ground, so that the volume size and the clustering probability of the polyimide fibers due to static electricity are reduced, the polyimide fiber fragmentation treatment efficiency is improved, the grinding time of the polyimide fibers is shortened, and the production cost is reduced.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
Adding the chopped polyimide fiber with the diameter of 40 mu m and the length of 6000 mu m, calcium carbonate powder with the particle size of 5 mu m and wool powder with the particle size of 0.1 mu m into a millstone machine at the same time for grinding and decomposing for 90min, wherein the polyimide fiber: wool powder: the mass ratio of the calcium carbonate powder is 5%: 50%: 45 percent, adding NaOH solution with the concentration of 0.01 percent into the ground polyimide fiber, calcium carbonate powder and wool powder to dissolve the wool powder, separating and drying in a filter device to obtain the polyimide fiber and the calcium carbonate powder, adding HCl with the concentration of 0.03 percent into the obtained mixture of the polyimide fiber and the calcium carbonate powder to dissolve the calcium carbonate powder, separating the polyimide fiber in a funnel and drying to obtain fibrillated polyimide fiber; the length of the polyimide fiber obtained was observed and tested in an optical microscope, and the length results are shown in Table 1. The grinding disc machine adopts a grinding disc introduced in the name of 'grinding disc for processing organic nano powder' which is published by China patent grant publication No. CN1268434C, 8/9/2006.
Example 2
Adding the chopped polyimide fiber with the diameter of 40 mu m and the length of 6000 mu m, calcium carbonate powder with the particle size of 10 mu m and wool powder with the particle size of 0.1 mu m into a millstone machine at the same time for grinding and decomposing for 90min, wherein the polyimide fiber: wool powder: the mass ratio of the calcium carbonate powder is 5%: 50%: 45 percent, adding NaOH solution with the concentration of 0.01 percent into the ground polyimide fiber, calcium carbonate powder and wool powder to dissolve the wool powder, separating and drying in a filter device to obtain the polyimide fiber and the calcium carbonate powder, adding HCl with the concentration of 0.03 percent into the obtained mixture of the polyimide fiber and the calcium carbonate powder to dissolve the calcium carbonate powder, separating the polyimide fiber in a funnel and drying to obtain fibrillated polyimide fiber; the length of the polyimide fiber obtained was observed and tested in an optical microscope, and the length results are shown in Table 1. The grinding disc machine in this embodiment is the same as that in embodiment 1.
Example 3
Adding the chopped polyimide fiber with the diameter of 40 mu m and the length of 6000 mu m, calcium carbonate powder with the particle size of 20 mu m and wool powder with the particle size of 0.1 mu m into a millstone machine at the same time for grinding and decomposing for 90min, wherein the polyimide fiber: wool powder: the mass ratio of the calcium carbonate powder is 5%: 50%: 45 percent, adding NaOH solution with the concentration of 0.01 percent into the ground polyimide fiber, calcium carbonate powder and wool powder to dissolve the wool powder, separating and drying in a filter device to obtain the polyimide fiber and the calcium carbonate powder, adding HCl with the concentration of 0.03 percent into the obtained mixture of the polyimide fiber and the calcium carbonate powder to dissolve the calcium carbonate powder, separating the polyimide fiber in a funnel and drying to obtain fibrillated polyimide fiber; the length of the polyimide fiber obtained was observed and tested in an optical microscope, and the length results are shown in Table 1. The grinding disc machine in this embodiment is the same as that in embodiment 1.
Example 4
Adding the chopped polyimide fiber with the diameter of 40 mu m and the length of 6000 mu m, calcium carbonate powder with the particle size of 20 mu m and wool powder with the particle size of 3 mu m into a millstone machine at the same time for grinding and decomposing for 90min, wherein the polyimide fiber: wool powder: the mass ratio of the calcium carbonate powder is 5%: 50%: 45 percent, adding NaOH solution with the concentration of 0.01 percent into the ground polyimide fiber, calcium carbonate powder and wool powder to dissolve the wool powder, separating and drying in a filter device to obtain the polyimide fiber and the calcium carbonate powder, adding HCl with the concentration of 0.03 percent into the obtained mixture of the polyimide fiber and the calcium carbonate powder to dissolve the calcium carbonate powder, separating the polyimide fiber in a funnel and drying to obtain fibrillated polyimide fiber; the length of the polyimide fiber obtained was observed and tested in an optical microscope, and the length results are shown in Table 1. The grinding disc machine in this embodiment is the same as that in embodiment 1.
Example 5
Adding the chopped polyimide fiber with the diameter of 40 mu m and the length of 6000 mu m, calcium carbonate powder with the particle size of 20 mu m and wool powder with the particle size of 5 mu m into a millstone machine at the same time for grinding and decomposing for 90min, wherein the polyimide fiber: wool powder: the mass ratio of the calcium carbonate powder is 5%: 50%: 45 percent, adding NaOH solution with the concentration of 0.01 percent into the ground polyimide fiber, calcium carbonate powder and wool powder to dissolve the wool powder, separating and drying in a filter device to obtain the polyimide fiber and the calcium carbonate powder, adding HCl with the concentration of 0.03 percent into the obtained mixture of the polyimide fiber and the calcium carbonate powder to dissolve the calcium carbonate powder, separating the polyimide fiber in a funnel and drying to obtain fibrillated polyimide fiber; the length of the polyimide fiber obtained was observed and tested in an optical microscope, and the length results are shown in Table 1. The grinding disc machine in this embodiment is the same as that in embodiment 1.
Example 6
Adding the chopped polyimide fiber with the diameter of 40 mu m and the length of 6000 mu m, calcium carbonate powder with the particle size of 20 mu m and wool powder with the particle size of 5 mu m into a millstone machine at the same time for milling treatment for 105min, wherein the polyimide fiber: wool powder: the mass ratio of the calcium carbonate powder is 5%: 50%: 45 percent, adding NaOH solution with the concentration of 0.01 percent into the ground polyimide fiber, calcium carbonate powder and wool powder to dissolve the wool powder, separating and drying in a filter device to obtain the polyimide fiber and the calcium carbonate powder, adding HCl with the concentration of 0.03 percent into the obtained mixture of the polyimide fiber and the calcium carbonate powder to dissolve the calcium carbonate powder, separating the polyimide fiber in a funnel and drying to obtain fibrillated polyimide fiber; the length of the polyimide fiber obtained was observed and tested in an optical microscope, and the length results are shown in Table 1. The grinding disc machine in this embodiment is the same as that in embodiment 1.
Example 7
Adding the chopped polyimide fiber with the diameter of 40 mu m and the length of 6000 mu m, calcium carbonate powder with the particle size of 20 mu m and wool powder with the particle size of 5 mu m into a millstone machine at the same time for grinding and decomposing for 120min, wherein the polyimide fiber: wool powder: the mass ratio of the calcium carbonate powder is 5%: 50%: 45 percent, adding NaOH solution with the concentration of 0.01 percent into the ground polyimide fiber, calcium carbonate powder and wool powder to dissolve the wool powder, separating and drying in a filter device to obtain the polyimide fiber and the calcium carbonate powder, adding HCl with the concentration of 0.03 percent into the obtained mixture of the polyimide fiber and the calcium carbonate powder to dissolve the calcium carbonate powder, separating the polyimide fiber in a funnel and drying to obtain fibrillated polyimide fiber; the length of the polyimide fiber obtained was observed and tested in an optical microscope, and the length results are shown in Table 1. The grinding disc machine in this embodiment is the same as that in embodiment 1.
Example 8
Adding the chopped polyimide fiber with the diameter of 40 mu m and the length of 6000 mu m, calcium carbonate powder with the particle size of 20 mu m and wool powder with the particle size of 5 mu m into a millstone machine at the same time for grinding and decomposing for 120min, wherein the polyimide fiber: wool powder: the mass ratio of calcium carbonate powder is 15%: 45%: 40 percent, adding NaOH solution with the concentration of 0.01 percent into the ground polyimide fiber, calcium carbonate powder and wool powder to dissolve the wool powder, separating and drying in a filter device to obtain the polyimide fiber and the calcium carbonate powder, adding HCl with the concentration of 0.03 percent into the obtained mixture of the polyimide fiber and the calcium carbonate powder to dissolve the calcium carbonate powder, separating the polyimide fiber in a funnel and drying to obtain fibrillated polyimide fiber; the length of the polyimide fiber obtained was observed and tested in an optical microscope, and the length results are shown in Table 1. The grinding disc machine in this embodiment is the same as that in embodiment 1.
Example 9
Adding the chopped polyimide fiber with the diameter of 40 mu m and the length of 6000 mu m, calcium carbonate powder with the particle size of 20 mu m and wool powder with the particle size of 5 mu m into a millstone machine at the same time for grinding and decomposing for 120min, wherein the polyimide fiber: wool powder: the mass ratio of the calcium carbonate powder is 30%: 40%: 30 percent, adding NaOH solution with the concentration of 0.01 percent into the ground polyimide fiber, calcium carbonate powder and wool powder to dissolve the wool powder, separating and drying in a filter device to obtain the polyimide fiber and the calcium carbonate powder, adding HCl with the concentration of 0.03 percent into the obtained mixture of the polyimide fiber and the calcium carbonate powder to dissolve the calcium carbonate powder, separating the polyimide fiber in a funnel and drying to obtain fibrillated polyimide fiber; the length of the polyimide fiber obtained was observed and tested in an optical microscope, and the length results are shown in Table 1. The grinding disc machine in this embodiment is the same as that in embodiment 1.
Example 10
Adding the chopped polyimide fiber with the diameter of 40 mu m and the length of 6000 mu m, calcium carbonate powder with the particle size of 20 mu m and wool powder with the particle size of 5 mu m into a millstone machine at the same time for grinding and decomposing for 120min, wherein the polyimide fiber: wool powder: the mass ratio of the calcium carbonate powder is 30%: 40%: 30 percent, adding NaOH solution with the concentration of 0.01 percent into the ground polyimide fiber, calcium carbonate powder and wool powder to dissolve the wool powder, separating and drying in a filter device to obtain the polyimide fiber and the calcium carbonate powder, adding HCl with the concentration of 0.03 percent into the obtained mixture of the polyimide fiber and the calcium carbonate powder to dissolve the calcium carbonate powder, separating the polyimide fiber in a funnel and drying to obtain fibrillated polyimide fiber; the length of the polyimide fiber obtained was observed and tested in an optical microscope, and the length results are shown in Table 1. The grinding disc machine in this embodiment is the same as that in embodiment 1.
Example 11
Adding the chopped polyimide fiber with the diameter of 25 microns and the length of 6000 microns, calcium carbonate powder with the particle size of 20 microns and wool powder with the particle size of 5 microns into a millstone machine at the same time for grinding and decomposing for 120min, wherein the polyimide fiber: wool powder: the mass ratio of the calcium carbonate powder is 30%: 40%: 30 percent, adding NaOH solution with the concentration of 0.01 percent into the ground polyimide fiber, calcium carbonate powder and wool powder to dissolve the wool powder, separating and drying in a filter device to obtain the polyimide fiber and the calcium carbonate powder, adding HCl with the concentration of 0.03 percent into the obtained mixture of the polyimide fiber and the calcium carbonate powder to dissolve the calcium carbonate powder, separating the polyimide fiber in a funnel and drying to obtain fibrillated polyimide fiber; the length of the polyimide fiber obtained was observed and tested in an optical microscope, and the length results are shown in Table 1. The grinding disc machine in this embodiment is the same as that in embodiment 1.
Example 12
Adding the chopped polyimide fiber with the diameter of 10 microns and the length of 6000 microns, calcium carbonate powder with the particle size of 20 microns and wool powder with the particle size of 5 microns into a millstone machine at the same time for grinding and decomposing for 120min, wherein the polyimide fiber: wool powder: the mass ratio of the calcium carbonate powder is 30%: 40%: 30 percent, adding NaOH solution with the concentration of 0.01 percent into the ground polyimide fiber, calcium carbonate powder and wool powder to dissolve the wool powder, separating and drying in a filter device to obtain the polyimide fiber and the calcium carbonate powder, adding HCl with the concentration of 0.03 percent into the obtained mixture of the polyimide fiber and the calcium carbonate powder to dissolve the calcium carbonate powder, separating the polyimide fiber in a funnel and drying to obtain fibrillated polyimide fiber; the length of the polyimide fiber obtained was measured by observation under an optical microscope, and the length results are shown in Table 1, and an electron micrograph was taken by a Nova NanoSEM 450 as shown in FIG. 2. A comparison of the electron micrographs of fig. 1 and 2 shows that the polyimide fibers were fibrillated, as in example 1 with the abrasive disc machine of this example.
Example 13
Adding the chopped polyimide fibers with the diameter of 10 microns and the length of 6000 microns, calcium carbonate powder with the particle size of 20 microns and silk powder with the particle size of 5 microns into a millstone machine at the same time for grinding treatment for 120min, wherein the polyimide fibers: silk powder: the mass ratio of the calcium carbonate powder is 30%: 40%: 30 percent, adding NaOH solution with the concentration of 0.01 percent into the ground polyimide fiber, calcium carbonate powder and silk powder to dissolve the silk powder, separating and drying in a filter device to obtain the polyimide fiber and the calcium carbonate powder, adding HCl with the concentration of 0.03 percent into the obtained mixture of the polyimide fiber and the calcium carbonate powder to dissolve the calcium carbonate powder, separating the polyimide fiber in a funnel and drying to obtain fibrillated polyimide fiber; the length of the polyimide fibers obtained by the observation and measurement in an optical microscope is shown in Table 1, and the grinding wheel machine in this example is the same as that in example 1.
As can be seen from table 1, the smaller the proportion of the polyimide fibers in the mixture is, the higher the proportion of the protein micro-nano powder and the calcium carbonate powder is, the larger the particle sizes of the protein micro-nano powder and the calcium carbonate powder are, the finer the polyimide fibers are, the longer the grinding time is, the higher the fibrillation treatment efficiency of the polyimide fibers is, and the less the influence of the split silk powder and wool on the fibrillation efficiency of the polyimide fibers is.
TABLE 1 comparison of polyimide fiber lengths after fibrillation treatment
Claims (2)
1. A polyimide fiber fibrillation treatment method comprises polyimide fiber chopping and polyimide fiber grinding treatment in a polyimide fiber fibrillation process, and is characterized in that:
the grinding treatment of the polyimide fiber refers to that the polyimide fiber with the diameter of 10-40 mu m and the length of 6000 mu m, the calcium carbonate powder with the particle size of 5-20 mu m and the protein micro-nano powder with the particle size of 0.1-5 mu m are simultaneously added into a grinding device for grinding treatment for 90-120min, NaOH solution with the concentration of 0.01 percent is added into the ground polyimide fiber, the calcium carbonate powder and the protein micro-nano powder to dissolve the protein micro-nano powder, separating and drying in a filter device to obtain polyimide fiber and calcium carbonate powder, adding HCl with the concentration of 0.03 percent into the obtained mixture of the polyimide fiber and the calcium carbonate powder to dissolve the calcium carbonate powder, separating the polyimide fibers in a filtering device and drying to obtain fibrillated polyimide fibers;
the mass percentages of the protein micro-nano powder and the calcium carbonate powder added into the polyimide fiber are respectively as follows:
5 to 30 percent of polyimide fiber
40 to 50 percent of protein micro-nano powder
30 to 45 percent of calcium carbonate powder.
2. A polyimide fiber fibrillation treatment method as claimed in claim 1, wherein: the protein micro-nano powder is wool powder or silk powder.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2689530A1 (en) * | 1992-04-07 | 1993-10-08 | Aussedat Rey | New complex product based on fibers and fillers, and method of manufacturing such a new product. |
| JP2000144105A (en) * | 1998-11-06 | 2000-05-26 | Akebono Brake Res & Dev Center Ltd | Friction material and aramid fiber mass therefor |
| CN101691700A (en) * | 2009-10-15 | 2010-04-07 | 金东纸业（江苏）股份有限公司 | Pulp-grinding method for improving fibre brooming and application thereof in papermaking |
| CN102093694A (en) * | 2009-12-14 | 2011-06-15 | 上海兰邦工业纤维有限公司 | Polyacrylonitrile pulp master batch |
| CN102720087A (en) * | 2012-06-15 | 2012-10-10 | 金东纸业（江苏）股份有限公司 | Size preparation method, size and paper made of size |
| CN105220262A (en) * | 2015-08-24 | 2016-01-06 | 江苏先诺新材料科技有限公司 | A kind of polyimides (PI) pulp and preparation method thereof |
| CN107059482A (en) * | 2017-04-24 | 2017-08-18 | 李志全 | A kind of heat-resisting anti-aging insulating paper and its preparation method and application |
| CN107675288A (en) * | 2017-10-19 | 2018-02-09 | 长春高琦聚酰亚胺材料有限公司 | A kind of polyimides superbhort fiber and preparation method thereof |
| EP3501298A1 (en) * | 2017-12-22 | 2019-06-26 | Omya International AG | Surface-reacted calcium carbonate as extrusion aid |
-
2019
- 2019-09-16 CN CN201910870792.0A patent/CN110528272B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2689530A1 (en) * | 1992-04-07 | 1993-10-08 | Aussedat Rey | New complex product based on fibers and fillers, and method of manufacturing such a new product. |
| JP2000144105A (en) * | 1998-11-06 | 2000-05-26 | Akebono Brake Res & Dev Center Ltd | Friction material and aramid fiber mass therefor |
| CN101691700A (en) * | 2009-10-15 | 2010-04-07 | 金东纸业（江苏）股份有限公司 | Pulp-grinding method for improving fibre brooming and application thereof in papermaking |
| CN102093694A (en) * | 2009-12-14 | 2011-06-15 | 上海兰邦工业纤维有限公司 | Polyacrylonitrile pulp master batch |
| CN102720087A (en) * | 2012-06-15 | 2012-10-10 | 金东纸业（江苏）股份有限公司 | Size preparation method, size and paper made of size |
| CN105220262A (en) * | 2015-08-24 | 2016-01-06 | 江苏先诺新材料科技有限公司 | A kind of polyimides (PI) pulp and preparation method thereof |
| CN107059482A (en) * | 2017-04-24 | 2017-08-18 | 李志全 | A kind of heat-resisting anti-aging insulating paper and its preparation method and application |
| CN107675288A (en) * | 2017-10-19 | 2018-02-09 | 长春高琦聚酰亚胺材料有限公司 | A kind of polyimides superbhort fiber and preparation method thereof |
| EP3501298A1 (en) * | 2017-12-22 | 2019-06-26 | Omya International AG | Surface-reacted calcium carbonate as extrusion aid |
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