CN109023579B - High-pull-out-strength building reinforced polyacrylonitrile chopped fiber and preparation method and application thereof - Google Patents
High-pull-out-strength building reinforced polyacrylonitrile chopped fiber and preparation method and application thereof Download PDFInfo
- Publication number
- CN109023579B CN109023579B CN201710425436.9A CN201710425436A CN109023579B CN 109023579 B CN109023579 B CN 109023579B CN 201710425436 A CN201710425436 A CN 201710425436A CN 109023579 B CN109023579 B CN 109023579B
- Authority
- CN
- China
- Prior art keywords
- fiber
- polyacrylonitrile
- chopped
- same
- steam
- 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.)
- Active
Links
Images
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/38—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds comprising unsaturated nitriles as the major constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01G—PRELIMINARY TREATMENT OF FIBRES, e.g. FOR SPINNING
- D01G1/00—Severing continuous filaments or long fibres, e.g. stapling
- D01G1/02—Severing continuous filaments or long fibres, e.g. stapling to form staple fibres not delivered in strand form
- D01G1/04—Severing continuous filaments or long fibres, e.g. stapling to form staple fibres not delivered in strand form by cutting
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G1/00—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
- D02G1/004—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by heating fibres, filaments, yarns or threads so as to create a temperature gradient across their diameter, thereby imparting them latent asymmetrical shrinkage properties
Abstract
The invention relates to a high-pull-out-strength building reinforced polyacrylonitrile chopped fiber, a preparation method and application thereof, and mainly solves the problem that the fiber in the prior art has poor compression resistance in building reinforced materials. The building reinforced polyacrylonitrile chopped fiber is prepared from polyacrylonitrile-based precursor fibers, and is characterized in that a straightening section is arranged in the middle of the fiber, and curling sections are arranged at two ends of the fiber, the curling density of the curling sections is 0.1-2/mm, and the total length of the curling sections is 1-10 mm.
Description
Technical Field
The invention relates to a building reinforced polyacrylonitrile chopped fiber, a preparation method and application thereof, in particular to a building cement reinforced polyacrylonitrile fiber, a preparation method and application thereof.
Background
The cement material is a base material widely used in building materials, has a series of advantages of good processability, simple construction process, low price and the like, and can be used for manufacturing building materials such as cement mortar, cement concrete and the like. During the use of materials such as cement mortar and cement concrete, along with the volatilization of moisture in the materials and the solidification and molding of the materials, a large number of pores are formed in the materials, the pores are easy to become the defect that the materials are broken when the materials are stressed, the cement materials have the defects of easy cracking, high brittleness and the like due to the large number of pores, the performance of the reinforced materials is obviously reduced in the application process, and potential risks are brought to the life and industrial application of the reinforced materials.
The addition of organic or inorganic fibers to cementitious materials is a widely used method of inhibiting cracking of cementitious materials. The role of fibers in cementitious materials is mainly three-fold: (1) the cracking stress of the cement material is improved, and the cracking of the cement under low stress is avoided; (2) the deformation capacity of the cement material is increased through the toughness of the organic fiber and the characteristic of energy absorption, and the toughness of the cement material is more important than the strength of the material in some aspects; (3) the fibers may further inhibit the further development of cracks after the material cracks and reduce the average crack spacing.
The organic fiber is widely used in building reinforcing materials due to the advantages of good processability, good mechanical property and the like, and the commonly used organic fiber mainly comprises the following components: polyacrylonitrile fibers, aramid fibers, polypropylene fibers, polyvinyl alcohol fibers, polyethylene fibers, polyester fibers, polyimide fibers, and the like. The polyacrylonitrile fiber has the advantages of good contact with cement material matrix, acid and alkali resistance, high temperature resistance, low price and the like, and is widely applied as building reinforcing fiber.
The pullout strength of the polyacrylonitrile chopped fiber reinforced material obviously influences the compression resistance of the reinforced building material, and the preparation of the polyacrylonitrile chopped fiber with high pullout strength is a key point and a difficulty in production, research and development of the polyacrylonitrile chopped fiber reinforced material.
The preparation method of the polyacrylonitrile fiber has various preparation modes, and the polyacrylonitrile fiber prepared by the one-step method with the dimethyl sulfoxide as the solvent has the advantages of high solid content of spinning solution and good economical efficiency and is widely used in many enterprises.
The preparation process of the building reinforced polyacrylonitrile chopped fiber comprises the steps of polymerization, demonomerization, defoaming, solidification forming, multistage solidification drafting, multistage hot water drafting, water washing, primary oiling, drying densification, steam drafting, heat setting, secondary oiling, oil solution re-drying, short cutting and the like. All the steps in the preparation process influence the mechanical property of the fiber and the binding force of the fiber and cement mortar, and finally influence the performance of the cement reinforced material.
Japanese patents JP58120811A, JP60021905A, JP61163149A, JP06115989A, JP08003812A disclose 5 polyacrylonitrile fiber production processes, but none of them show the characteristics of polyacrylonitrile chopped fiber and its specific production process to make the material have high pullout strength.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
One of the main technical problems to be solved by the invention is the problem of poor compression resistance of the polyacrylonitrile chopped fiber building reinforcing material in the prior art. Provides the building reinforced polyacrylonitrile chopped fiber with high pull-out strength, and has the characteristic of high compression resistance of the reinforced material.
The second technical problem to be solved by the invention is to provide a preparation method of building reinforced polyacrylonitrile chopped fiber corresponding to the first technical problem.
The invention aims to solve the third technical problem and provides application of the building reinforced polyacrylonitrile chopped fiber corresponding to one of the technical problems.
In order to solve one of the above technical problems, the technical scheme adopted by the invention is as follows: the building reinforced polyacrylonitrile chopped fiber is prepared from polyacrylonitrile-based precursor fibers, wherein a straight section is arranged in the middle of the fiber, curled sections are arranged at two ends of the fiber, the curling density of the curled sections is 0.1-2/mm, and the total length of the curled sections is 1-10 mm.
In the technical scheme, the total length of the fibers is preferably 5-32mm, and the linear density of the fibers is preferably 0.7-20 dtex.
In the above-described embodiment, the shape of the curl is preferably at least one of a spiral shape, a hook shape, an S shape, an L shape, an N shape, an M shape, and a W shape.
In the above technical solution, the crimp density of the crimped section is preferably 0.1-1.2 pieces/mm, and more preferably 0.2-1 pieces/mm.
In the above technical solution, the total length of the curled segment is preferably 2-6 mm.
In the above technical solution, the ratio of the total length of the curled section to the length of the straightened section is preferably 1:32-2: 1.
In the above technical solution, a further preferred solution is: the total length of the polyacrylonitrile chopped fiber is 6-26 mm; the linear density of the fiber is 1-18 dtex; the crimp shape is at least one of N type and M type, and the inventor surprisingly finds that the compressive performance of the polyacrylonitrile chopped fiber building reinforcing material can be improved by more than 30 percent.
In order to solve the second technical problem, the invention adopts the technical scheme that: a preparation method of the building reinforced polyacrylonitrile chopped fiber in any technical scheme for solving one of the technical problems comprises the following steps:
(1) carrying out steam short cutting on the polyacrylonitrile-based protofilament by a fiber short cutting machine to obtain a short fiber;
(2) and (2) generating curled sections with the curling density and the total length of the curled sections at two ends of the chopped fiber obtained in the step (1) under the action of a thermal mechanism, and straightening the middle part of the fiber to obtain the architectural reinforced polyacrylonitrile chopped fiber.
In the technical scheme, the characteristic viscosity number of the spinning solution for preparing the polyacrylonitrile protofilament is 3-6 dL/g; the polyacrylonitrile-based precursor is further preferably prepared by coagulation forming, drafting and water washing, oiling, drying densification, steam drafting and heat setting, secondary oiling and oil solution redrying of spinning solution with the intrinsic viscosity of 3-6 dL/g.
In the technical scheme, the washing temperature is preferably 60-90 ℃, and the washing draft ratio is preferably not less than-1%.
In the above technical solution, the steam draft absolute pressure is preferably 0.1 to 1MPa, and the draft ratio is preferably 1 to 5.
In the above technical solution, the heat setting temperature is preferably 100-150 ℃, and the draw ratio is preferably 0.9-1.0.
In the above technical solution, a further preferred solution is: the intrinsic viscosity of the spinning solution for preparing the polyacrylonitrile protofilament is 3.2-5.8 dL/g; the washing temperature for preparing the polyacrylonitrile protofilament is 60-90 ℃, and the washing drafting ratio is not less than-0.8%; the drying densification temperature of the prepared polyacrylonitrile protofilament is 85-148 ℃, and the draw ratio is 0.94-1.0; the steam drafting absolute pressure for preparing the polyacrylonitrile protofilament is 0.2-0.7MPa, and the drafting ratio is 1.5-3.5; the heat setting temperature for preparing the polyacrylonitrile protofilament is 105-145 ℃, and the draw ratio is 0.92-1.0; the oil agent for preparing the polyacrylonitrile protofilament is dried at the temperature of 105-125 ℃; the thermomechanical action is preferably a steam combined mechanical action, such as in a steam chopper, at a steam pressure of 0.7MPa and combined with a mechanical action that will crimp and cut the fibers.
In the above technical solution, a further preferred solution is: the intrinsic viscosity of the spinning solution for preparing the polyacrylonitrile protofilament is 3.2-5.2; the washing temperature for preparing the polyacrylonitrile protofilament is 60-80 ℃, and the washing drafting ratio is not less than-0.7%; the drying densification temperature for preparing the polyacrylonitrile protofilament is 110-140 ℃, and the draw ratio is 0.96-1.0; the steam drafting absolute pressure for preparing the polyacrylonitrile protofilament is 0.2-0.7MPa, and the drafting ratio is 1.8-3.5; the oil agent for preparing the polyacrylonitrile protofilament is dried at the temperature of 110-120 ℃; the temperature of the first path of coagulating liquid for preparing the polyacrylonitrile protofilament is 20-70 ℃, more preferably 20-65 ℃, the concentration is 30-60 wt%, more preferably 40-55 wt%, and the temperature of the second path of coagulating liquid for preparing the polyacrylonitrile protofilament is 30-60 ℃, more preferably 40-55 ℃; the concentration of the third coagulating liquid for preparing the polyacrylonitrile protofilament is 10 wt% to 40 wt%, more preferably 10 wt% to 25 wt%, and the temperature of the third coagulating liquid is 20 ℃ to 70 ℃, more preferably 55 ℃ to 70 ℃.
In order to solve the third technical problem, the technical scheme adopted by the invention is as follows: the application of the architectural reinforced polyacrylonitrile chopped fiber in any one of the technical schemes for solving the technical problems.
In the above technical solutions, the application is not strictly limited, and those skilled in the art can apply the building reinforcing material in combination with the prior art according to the disclosure of the present invention.
The number of crimps of the fiber is defined as: one crimp is from one crimp peak to an adjacent crimp peak of the fiber. Crimp density is defined as the number of crimps per mm of fibre, for example a crimp density of 0.1 fibre per mm if the number of crimps in a 10mm fibre is 1.
The polyacrylonitrile chopped fiber has a special structure with two ends curled and the middle straightened, the two sections curled can enable the two sections to bear more drawing force in the drawing process, the straightened state of the middle section can ensure that the fiber directly bears stress when the polyacrylonitrile fiber composite building material cracks, and the average crack length is prevented from being further increased. The length of the short fiber is controlled to avoid the agglomeration of the reinforced polyacrylonitrile fiber in the preparation process of the building material caused by too long or too short length, and the interface combination of the fiber and the building material is kept in a better state.
The test method of the pull-out strength of the chopped fibers in the cement mortar is a fiber monofilament pull-out strength test method, the pre-buried length of the fibers in the cement mortar is half of the length of the fibers, and the test speed is 1 mm/min.
By adopting the technical scheme of the invention, because the special short-cut fiber which has a certain crimp length and crimp density and is crimped at two ends and straightened in the middle is adopted, the compressive property of the reinforced material of the polyacrylonitrile short-cut fiber in the reinforced material of the building is obviously improved, the pull-out strength of the short-cut fiber in cement mortar can reach 4.1MPa, and better technical effect is achieved.
The invention is further illustrated by the following examples.
Drawings
FIG. 1 is a schematic view of a fiber structure in which both ends of the fiber are spirally wound in example 1;
FIG. 2 is a schematic view of the structure of the fiber of example 2 in which both ends are S-shaped in the crimp shape;
FIG. 3 is a schematic view of the structure of fibers having both ends curled in a hook shape in example 3;
FIG. 4 is a schematic view of the structure of the fiber of example 4 in which both ends are curled in L-shape;
FIG. 5 is a schematic view of the structure of the fiber of example 5 in which both end crimp shapes are N-type;
FIG. 6 is a schematic view of the structure of the fiber of example 6 in which both end crimp shapes are M-shaped.
The fiber crimp shape structure in examples 7-10 is the same as the N and M forms of fiber crimp in fig. 5 and 6.
Detailed Description
[ example 1 ]
1. Preparing stock solution: adding refined acrylonitrile, sodium methyl propenyl sulfonate and methyl acrylate into a reactor according to the mass ratio of 99.6:0.2:0.2 and the solid content of 15 percent, wherein azodiisobutyronitrile accounts for 0.2 percent by weight of a comonomer, taking dimethyl sulfoxide as a solvent, and reacting for 20 hours at a constant temperature of 50 ℃ under the protection of nitrogen to obtain a polymerization stock solution with the intrinsic viscosity of 3.2 dL/g. And (3) performing vacuum-nitrogen replacement, demonomerization and vacuum defoamation, and performing 2-micron precision filtration to prepare the spinning stock solution.
2. Solidification and forming: and (2) preparing nascent fiber by adopting wet spinning, accurately metering a spinning stock solution by a metering pump, filtering again, feeding the spinning stock solution into a first coagulating bath through a spinneret plate, and carrying out two-stage coagulating drafting at a coagulating temperature of 25 ℃, a concentration of 50% and a drafting ratio of-20% subsequently, wherein the drafting ratio is respectively 1.0 and 1.05, so as to obtain the coagulated fiber.
3. Drawing and water washing: the three hot water drafting temperatures are respectively 90, 98 and 99 ℃, and the drafting ratios are respectively 1.8, 2.0 and 2.4; the water washing temperature was 60 ℃ and the draft ratio was 1.0.
4. Primary oiling and dry densification: and (3) oiling the fiber obtained in the step (3) for the first time, and then performing drying densification, wherein the drying densification temperature is in a stepped heating mode, the drying densification temperature of the 1 st step is 88 ℃, and the drying densification temperature of the 2 nd step is 145 ℃.
5. Steam drawing and heat setting: and (3) drafting the fiber obtained in the step (4) by 3.2 times in steam of 0.6MPa, and then performing heat setting in steam of 130 ℃, wherein the heat setting drafting ratio is-2%.
6. Secondary oiling and oil solution redrying: and (4) oiling the fiber obtained in the step (5) for the second time, and drying the fiber at the temperature of 120 ℃ after the oil solution is dried again.
7. Steam chopping of fibers: crimping and cutting the fibers obtained in the step 6 in a steam chopping machine under the steam pressure of 0.7MPa in combination with mechanical action; the obtained fiber has the two-end crimp density of 0.6 piece/mm, the two-end crimp length of 2mm, the two-end crimp shape of spiral shape, the chopped fiber length of 6mm and the fiber linear density of 1.5 dtex.
The chopped fibers obtained were tested for pullout strength in cement mortar of 3.7 MPa.
[ example 2 ]
1. Preparing stock solution: same as example 1, step 1.
2. Solidification and forming: same as example 1, step 2.
3. Drawing and water washing: same as example 1, step 3.
4. Primary oiling and dry densification: same as example 1, step 4.
5. Steam drawing and heat setting: same as example 1, step 5.
6. Secondary oiling and oil solution redrying: same as example 1, step 6.
7. Steam chopping of fibers: crimping and cutting the fibers obtained in the step 6 in a steam chopping machine under the steam pressure of 0.7MPa in combination with mechanical action; the obtained fiber has the two-end crimp density of 0.6 piece/mm, the two-end crimp length of 2mm, the two-end crimp shape of S-shaped, the chopped fiber has the length of 6mm, and the linear density of the fiber is 1.5 dtex.
The resulting chopped fibers were tested for a pullout strength of 3.72MPa in cement mortar.
[ example 3 ]
1. Preparing stock solution: same as example 1, step 1.
2. Solidification and forming: same as example 1, step 2.
3. Drawing and water washing: same as example 1, step 3.
4. Primary oiling and dry densification: same as example 1, step 4.
5. Steam drawing and heat setting: same as example 1, step 5.
6. Secondary oiling and oil solution redrying: same as example 1, step 6.
7. Steam chopping of fibers: crimping and cutting the fibers obtained in the step 6 in a steam chopping machine under the steam pressure of 0.7MPa in combination with mechanical action; the obtained fiber has the two-end crimp density of 0.6 piece/mm, the two-end crimp length of 2mm, the two-end crimp shape of hook-shaped, the chopped fiber has the length of 6mm, and the linear density of the fiber is 1.5 dtex.
The resulting chopped fibers were tested for a pullout strength of 3.75MPa in cement mortar.
[ example 4 ]
1. Preparing stock solution: same as example 1, step 1.
2. Solidification and forming: same as example 1, step 2.
3. Drawing and water washing: same as example 1, step 3.
4. Primary oiling and dry densification: same as example 1, step 4.
5. Steam drawing and heat setting: same as example 1, step 5.
6. Secondary oiling and oil solution redrying: same as example 1, step 6.
7. Steam chopping of fibers: crimping and cutting the fibers obtained in the step 6 in a steam chopping machine under the steam pressure of 0.7MPa in combination with mechanical action; the obtained fiber has the two-end crimp density of 0.6 piece/mm, the two-end crimp length of 2mm, the two-end crimp shape of L-shaped, the chopped fiber has the length of 6mm, and the linear density of the fiber is 1.5 dtex.
The resulting chopped fibers were tested for a pullout strength of 3.65MPa in cement mortar.
[ example 5 ]
1. Preparing stock solution: same as example 1, step 1.
2. Solidification and forming: same as example 1, step 2.
3. Drawing and water washing: same as example 1, step 3.
4. Primary oiling and dry densification: same as example 1, step 4.
5. Steam drawing and heat setting: same as example 1, step 5.
6. Secondary oiling and oil solution redrying: same as example 1, step 6.
7. Steam chopping of fibers: crimping and cutting the fibers obtained in the step 6 in a steam chopping machine under the steam pressure of 0.7MPa in combination with mechanical action; the obtained fiber has the two-end crimp density of 0.6 piece/mm, the two-end crimp length of 2mm, the two-end crimp shape of N type, the chopped fiber length of 6mm and the fiber linear density of 1.5 dtex.
The resulting chopped fibers were tested for a pullout strength of 3.85MPa in cement mortar.
[ example 6 ]
1. Preparing stock solution: same as example 1, step 1.
2. Solidification and forming: same as example 1, step 2.
3. Drawing and water washing: same as example 1, step 3.
4. Primary oiling and dry densification: same as example 1, step 4.
5. Steam drawing and heat setting: same as example 1, step 5.
6. Secondary oiling and oil solution redrying: same as example 1, step 6.
7. Steam chopping of fibers: crimping and cutting the fibers obtained in the step 6 in a steam chopping machine under the steam pressure of 0.7MPa in combination with mechanical action; the obtained fiber has the two-end crimp density of 0.6 piece/mm, the two-end crimp length of 2mm, the two-end crimp shape of M-shaped, the chopped fiber has the length of 6mm, and the linear density of the fiber is 1.5 dtex.
The resulting chopped fibers were tested for a pullout strength of 3.95MPa in cement mortar.
[ example 7 ]
1. Preparing stock solution: same as example 1, step 1.
2. Solidification and forming: the diameter of the spinneret was adjusted to 2.6 times the diameter of the spinneret in example 1, and the remaining solidification forming conditions were the same as in step 2 of example 1.
3. Drawing and water washing: same as example 1, step 3.
4. Primary oiling and dry densification: same as example 1, step 4.
5. Steam drawing and heat setting: same as example 1, step 5.
6. Secondary oiling and oil solution redrying: same as example 1, step 6.
7. Steam chopping of fibers: crimping and cutting the fibers obtained in the step 6 in a steam chopping machine under the steam pressure of 0.7MPa in combination with mechanical action; the obtained fiber has the two-end crimp density of 1/mm, the two-end crimp length of 3mm, the two-end crimp shape of M-shaped, the chopped fiber has the length of 8mm, and the linear density of the fiber is 10 dtex.
The resulting chopped fibers were tested for a pullout strength of 4.1MPa in cement mortar.
[ example 8 ]
1. Preparing stock solution: same as example 1, step 1.
2. Solidification and forming: same as example 7, step 2.
3. Drawing and water washing: same as example 1, step 3.
4. Primary oiling and dry densification: same as example 1, step 4.
5. Steam drawing and heat setting: same as example 1, step 5.
6. Secondary oiling and oil solution redrying: same as example 1, step 6.
7. Steam chopping of fibers: crimping and cutting the fibers obtained in the step 6 in a steam chopping machine under the steam pressure of 0.7MPa in combination with mechanical action; the obtained fiber has the two-end crimp density of 0.8 piece/mm, the two-end crimp length of 3mm, the two-end crimp shape of N-type, the chopped fiber length of 24mm and the linear density of 10 dtex.
The resulting chopped fibers were tested for a pullout strength of 4.0MPa in cement mortar.
[ example 9 ]
1. Preparing stock solution: same as example 1, step 1.
2. Solidification and forming: same as example 1, step 2.
3. Drawing and water washing: same as example 1, step 3.
4. Primary oiling and dry densification: same as example 1, step 4.
5. Steam drawing and heat setting: same as example 1, step 5.
6. Secondary oiling and oil solution redrying: same as example 1, step 6.
7. Steam chopping of fibers: steam chopping the fibers obtained in step 6, and curling and cutting the fibers under the steam pressure of 0.7MPa in combination with mechanical action; the obtained fiber has the two-end crimp density of 0.6 piece/mm, the two-end crimp length of 2mm, one end of the crimp shape is M-shaped, the other end is N-shaped, the chopped fiber has the length of 6mm, and the linear density of the fiber is 1.5 dtex.
The resulting chopped fibers were tested for a pullout strength of 3.90MPa in cement mortar.
[ example 10 ]
Carrying out steam chopping on commercially available Shanghai petrochemical uncrimped polyacrylonitrile protofilament fibers, and curling and cutting the fibers under the steam pressure of 0.7MPa in combination with mechanical action; the obtained fiber has the two-end crimp density of 0.8 piece/mm, the two-end crimp length of 6mm, the crimp shape of the two ends of the fiber is M-shaped, the length of the chopped fiber is 24mm, and the linear density of the fiber is 0.75 dtex.
The resulting chopped fibers were tested for a pullout strength of 1.0MPa in cement mortar.
[ COMPARATIVE EXAMPLE 1 ]
1. Preparing stock solution: same as example 1, step 1.
2. Solidification and forming: same as example 1, step 2.
3. Drawing and water washing: same as example 1, step 3.
4. Primary oiling and dry densification: same as example 1, step 4.
5. Steam drawing and heat setting: same as example 1, step 5.
6. Secondary oiling and oil solution redrying: same as example 1, step 6.
7. Fiber chopping: the fibers obtained in step 6 were directly chopped into fibers having a length of 6mm without both ends curled and a linear density of 1.5dtex, respectively.
The pull-out strengths of the 6mm chopped fibers in cement mortar obtained by the test were 3.0MPa respectively.
[ COMPARATIVE EXAMPLE 2 ]
1. Preparing stock solution: same as example 1, step 1.
2. Solidification and forming: the diameter of the spinneret was adjusted to 3.8 times that of the spinneret of example 1, and the remaining solidification forming conditions were the same as in step 2 of example 1.
3. Drawing and water washing: same as example 1, step 3.
4. Primary oiling and dry densification: same as example 1, step 4.
5. Steam drawing and heat setting: same as example 1, step 5.
6. Secondary oiling and oil solution redrying: same as example 1, step 6.
7. Fiber chopping: crimping and cutting the fibers obtained in step 6 under a steam pressure of 0.7MPa in combination with mechanical action; the obtained fiber has the two-end crimp density of 0.6 piece/mm, the two-end crimp length of 2mm, the two-end crimp shape of spiral shape, the length of 6mm after the fiber is chopped, and the linear density of 22 dtex.
The resulting chopped fibers were tested for a pullout strength of 3.2MPa in cement mortar.
[ COMPARATIVE EXAMPLE 3 ]
1. Preparing stock solution: same as example 1, step 1.
2. Solidification and forming: same as example 1, step 2.
3. Drawing and water washing: same as example 1, step 3.
4. Primary oiling and dry densification: same as example 1, step 4.
5. Steam drawing and heat setting: same as example 1, step 5.
6. Secondary oiling and oil solution redrying: same as example 1, step 6.
7. Steam chopping of fibers: crimping and cutting the fibers obtained in the step 6 in a steam chopping machine under the steam pressure of 0.7MPa in combination with mechanical action; the obtained fiber has the two-end crimp density of 0.02 piece/mm, the two-end crimp length of 2mm, the chopped length of 6mm and the linear density of 1.5 dtex.
The resulting chopped fibers were tested for a pullout strength of 2.1MPa in cement mortar.
[ COMPARATIVE EXAMPLE 4 ]
1. Preparing stock solution: same as example 1, step 1.
2. Solidification and forming: same as example 1, step 2.
3. Drawing and water washing: same as example 1, step 3.
4. Primary oiling and dry densification: same as example 1, step 4.
5. Steam drawing and heat setting: same as example 1, step 5.
6. Secondary oiling and oil solution redrying: same as example 1, step 6.
7. Steam chopping of fibers: crimping and cutting the fibers obtained in the step 6 in a steam chopping machine under the steam pressure of 0.7MPa in combination with mechanical action; the obtained fiber has the two-end crimp density of 0.6 piece/mm, the two-end crimp length of 12mm, the two-end crimp shape of S-shaped, the chopped fiber has the length of 36mm, and the linear density of the fiber is 1.5 dtex.
The fiber agglomeration is obvious in the processing, and the average pull-out strength of the obtained chopped fiber in cement mortar is 2 MPa.
[ COMPARATIVE EXAMPLE 5 ]
1. Preparing stock solution: same as example 1, step 1.
2. Solidification and forming: same as example 1, step 2.
3. Drawing and water washing: same as example 1, step 3.
4. Primary oiling and dry densification: same as example 1, step 4.
5. Steam drawing and heat setting: same as example 1, step 5.
6. Secondary oiling and oil solution redrying: same as example 1, step 6.
7. Steam chopping of fibers: crimping and cutting the fibers obtained in the step 6 in a steam chopping machine under the steam pressure of 0.7MPa in combination with mechanical action; the obtained fiber had a crimp density of 0.1 piece/mm, was completely crimped, had a length of 6mm after chopping and a linear density of 1.5 dtex.
The resulting chopped fibers were tested for a pullout strength of 2.2MPa in cement mortar.
[ COMPARATIVE EXAMPLE 6 ]
1. Preparing stock solution: same as example 1, step 1.
2. Solidification and forming: same as example 1, step 2.
3. Drawing and water washing: same as example 1, step 3.
4. Primary oiling and dry densification: same as example 1, step 4.
5. Steam drawing and heat setting: same as example 1, step 5.
6. Secondary oiling and oil solution redrying: same as example 1, step 6.
7. Steam chopping of fibers: crimping and cutting the fibers obtained in the step 6 in a steam chopping machine under the steam pressure of 0.7MPa in combination with mechanical action; the obtained fiber has the two-end crimp density of 3/mm, the two-end crimp length of 2mm and the two-end crimp shape of spiral shape, the chopped fiber has the length of 6mm and the linear density of 1.5 dtex.
The resulting chopped fibers were tested for a pullout strength of 3.3MPa in cement mortar.
[ COMPARATIVE EXAMPLE 7 ]
As in example 10, commercially available Shanghai stoned uncrimped polyacrylonitrile strands were directly chopped into fully straight chopped fibers having a length of 24mm and a linear fiber density of 0.75 dtex.
The obtained chopped fibers were tested for a pullout strength of 0.6MPa in cement mortar.
Claims (11)
1. The building reinforced polyacrylonitrile chopped fiber is prepared from polyacrylonitrile-based protofilaments and is characterized in that a straightening section is arranged in the middle of the fiber, crimping sections are arranged at two ends of the fiber, the crimping density of the crimping sections is 0.1-2/mm, and the total length of the crimping sections is 1-10 mm.
2. The chopped strand architectural reinforced polyacrylonitrile according to claim 1, characterized in that the total length of the fiber is 5-32mm, and the linear density of the fiber is 0.7-20 dtex.
3. The chopped strand architectural reinforced polyacrylonitrile according to claim 1, characterized in that the crimped shape is at least one of a spiral, a hook, an S-shape, an L-shape, an N-shape, an M-shape, a W-shape.
4. The architectural reinforced polyacrylonitrile staple fiber according to claim 1, characterized in that the crimp density is 0.1-1.2 pieces/mm.
5. The architectural reinforced polyacrylonitrile staple fiber according to claim 4, characterized in that the crimp density is 0.2-1 per mm.
6. The chopped strand architectural reinforced polyacrylonitrile according to claim 1, characterized in that the total length of the crimped section is 2-6 mm.
7. The chopped strand architectural reinforced polyacrylonitrile according to claim 1, characterized in that the ratio of the total length of the crimped sections to the length of the straightened sections is 1:32-2: 1.
8. A method for preparing the architectural reinforced polyacrylonitrile chopped fiber according to any one of claims 1 to 7, comprising the following steps:
(1) carrying out steam short cutting on the polyacrylonitrile-based protofilament by a fiber short cutting machine to obtain a short fiber;
(2) and (3) generating curled sections with the curled density and the total length of the curled sections at two ends of the chopped fiber under the action of thermal machinery, and keeping the middle of the fiber straight to obtain the architectural reinforced polyacrylonitrile chopped fiber.
9. The method for preparing the architectural reinforced polyacrylonitrile chopped fiber according to claim 8, characterized in that the polyacrylonitrile-based precursor fiber is prepared by coagulation forming, drafting and water washing, oiling, drying densification, steam drafting and heat setting, secondary oiling and oil solution redrying of a spinning solution with the intrinsic viscosity of 3-6 dL/g.
10. The method for preparing the architectural reinforced polyacrylonitrile chopped fiber according to claim 9, characterized in that the washing temperature is 60-90 ℃, and the washing draft ratio is not less than-1%; the absolute pressure of the steam drafting is 0.1-1MPa, and the drafting ratio is 1-5; the heat setting temperature is 100-150 ℃, and the draw ratio is 0.9-1.0.
11. Use of the architectural reinforced polyacrylonitrile staple fiber according to any one of claims 1 to 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710425436.9A CN109023579B (en) | 2017-06-08 | 2017-06-08 | High-pull-out-strength building reinforced polyacrylonitrile chopped fiber and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710425436.9A CN109023579B (en) | 2017-06-08 | 2017-06-08 | High-pull-out-strength building reinforced polyacrylonitrile chopped fiber and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109023579A CN109023579A (en) | 2018-12-18 |
| CN109023579B true CN109023579B (en) | 2020-12-29 |
Family
ID=64629080
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710425436.9A Active CN109023579B (en) | 2017-06-08 | 2017-06-08 | High-pull-out-strength building reinforced polyacrylonitrile chopped fiber and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109023579B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1217402A (en) * | 1997-11-18 | 1999-05-26 | 中国科学院山西煤炭化学研究所 | Process and apparatus for spinning and weaving fire-retardant fabric of preliminaril oxidized silk |
| CN1305441A (en) * | 1998-05-14 | 2001-07-25 | 布伊格斯公司 | Concrete comprising organic fibres dispersed in cement matrix, concrete cement matrix and premixes |
| CN1578856A (en) * | 2001-12-28 | 2005-02-09 | 三菱丽阳株式会社 | Highly shrinkable acrylic fiber, pile compositions containing the same and napped fabrics made by using the compositions |
| CN101104962A (en) * | 2007-07-31 | 2008-01-16 | 浙江杭州湾腈纶有限公司 | Method for preparing acrylic fibre used for building |
| CN101270501A (en) * | 2008-04-02 | 2008-09-24 | 浙江杭州湾腈纶有限公司 | Method for preparing acrylic fibre with wet-process |
| CN101445967A (en) * | 2008-12-12 | 2009-06-03 | 浙江杭州湾腈纶有限公司 | Preparation method of flat acrylic fiber |
| CN102260960A (en) * | 2011-06-27 | 2011-11-30 | 吉林市双鹏碳材料科技开发有限公司 | Preparation method of polyacrylonitrile-based preoxidized fiber felt |
| CN106460242A (en) * | 2014-04-30 | 2017-02-22 | 三菱丽阳株式会社 | Acrylic fibers, method for manufacturing same, and spun yarn and knitted fabric using said fibers |
-
2017
- 2017-06-08 CN CN201710425436.9A patent/CN109023579B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1217402A (en) * | 1997-11-18 | 1999-05-26 | 中国科学院山西煤炭化学研究所 | Process and apparatus for spinning and weaving fire-retardant fabric of preliminaril oxidized silk |
| CN1305441A (en) * | 1998-05-14 | 2001-07-25 | 布伊格斯公司 | Concrete comprising organic fibres dispersed in cement matrix, concrete cement matrix and premixes |
| CN1578856A (en) * | 2001-12-28 | 2005-02-09 | 三菱丽阳株式会社 | Highly shrinkable acrylic fiber, pile compositions containing the same and napped fabrics made by using the compositions |
| CN101104962A (en) * | 2007-07-31 | 2008-01-16 | 浙江杭州湾腈纶有限公司 | Method for preparing acrylic fibre used for building |
| CN101270501A (en) * | 2008-04-02 | 2008-09-24 | 浙江杭州湾腈纶有限公司 | Method for preparing acrylic fibre with wet-process |
| CN101445967A (en) * | 2008-12-12 | 2009-06-03 | 浙江杭州湾腈纶有限公司 | Preparation method of flat acrylic fiber |
| CN102260960A (en) * | 2011-06-27 | 2011-11-30 | 吉林市双鹏碳材料科技开发有限公司 | Preparation method of polyacrylonitrile-based preoxidized fiber felt |
| CN106460242A (en) * | 2014-04-30 | 2017-02-22 | 三菱丽阳株式会社 | Acrylic fibers, method for manufacturing same, and spun yarn and knitted fabric using said fibers |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109023579A (en) | 2018-12-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101724922B (en) | Method for preparing high-strength polyacrylonitrile-based precursor for carbon fiber | |
| CN101768791B (en) | Polyacrylonitrile-based hollow carbon fiber precursor preparation method | |
| CN109402792B (en) | Low-diameter high-strength polyacrylonitrile-based carbon fiber and preparation method thereof | |
| CN1536107A (en) | Preparation method of polyacrylonitrile carbon raw yarn | |
| CN106012111A (en) | Preparation method of carbon fiber precursor | |
| CN101275303B (en) | Stretch-tension-relax setting method for polyphenyl thioether short fibre | |
| CN109023579B (en) | High-pull-out-strength building reinforced polyacrylonitrile chopped fiber and preparation method and application thereof | |
| JPS6211089B2 (en) | ||
| CN109023578B (en) | Building reinforced polyacrylonitrile chopped fiber and preparation method thereof | |
| CN112760752B (en) | PAN-based carbon fiber and preparation method thereof | |
| CN111088558B (en) | Preparation method of polyacrylonitrile-based carbon fiber | |
| CN109023574B (en) | Polyacrylonitrile chopped fiber for building reinforcement and preparation method thereof | |
| CN109023575B (en) | Building reinforced polyacrylonitrile chopped fiber and preparation method thereof | |
| CN109023577A (en) | Build the preparation method of reinforced polypropylene nitrile chopped strand | |
| CN109023563B (en) | Preparation method of polyacrylonitrile chopped fiber for building reinforcement | |
| CN111088559A (en) | Preparation method of low-silicon-content polyacrylonitrile-based carbon fiber | |
| CN101709129B (en) | Gel spinning solution of polyacrylonitrile-based carbon fiber precursor without skin-core structure and preparation thereof | |
| JP4446991B2 (en) | Method for producing acrylonitrile-based precursor fiber for carbon fiber | |
| CN110685041B (en) | Preparation method of polyacrylonitrile-based carbon fiber | |
| CN111088536B (en) | Oiling method of polyacrylonitrile protofilament | |
| CN109023576B (en) | High-interface bonding strength building reinforced polyacrylonitrile chopped fiber and preparation method and application thereof | |
| CN113862811B (en) | Acrylic fiber and preparation method thereof, and preparation method of carbon fiber | |
| CN113862812A (en) | Special polyacrylonitrile-based carbon fiber precursor for carbon paper and preparation method thereof | |
| CN111996825B (en) | Zirconium oxide continuous fiber braided rope and preparation method thereof | |
| JP2010024581A (en) | Flameproof fiber and method for producing the same |
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 |