JPS62231010A - Fiber having knotlike bulge and production thereof - Google Patents

Abstract

PURPOSE:To obtain the titled fibers, having a high tensile strength and useful for mats, etc., by softening a composition softening by heating, discharging the softened composition onto a rotating disk while pulsating the through-put and flying out the composition from the disk by centrifugal force to form fibers having knotlike bulge parts. CONSTITUTION:A composition of SiO2 and Al2O3 is softened in a vessel 4 having small holes 5 at the bottom by heating with heat radiation from a heater at 1,850 deg.C to give 1P viscosity and the composition is discharged from the small holes 5 onto a disk 1 rotating at 0.5-400m/sec peripheral speed to fly out and fiberize the composition from the disk 1 by centrifugal force. In the process, the through-put from the small holes 5 is adjusted by a flow rate adjusting rod 6 to pulsate the composition and afford the aimed fibers having knotlike bulge parts consisting of the same composition as that in the fibers and the ratio of the maximum diameter of the knotlike parts within the range of 0.1-10,000 and the ratio of the maximum diameter of the knotlike parts to the diameter of the fiber parts within the range of 1.2-200.

Description

Detailed Description of the Invention [Field of Industrial Application] The present invention relates to a fiber having knob-like bulges having the same composition as the fiber and a method for producing the same. The present invention relates to fibers having knob-like bulges suitable for use in mats (also referred to as blankets) used as bodies, fiber reinforced plastics (FRP) in which fibers are used as reinforcing materials for plastics, etc., and a method for producing the same.

[Description of prior art]

Conventionally, methods for manufacturing fibers made of a composition that softens when heated include a blowing method in which the stream flows out through pores and is then blown with high-pressure air or high-pressure steam, and a method in which the stream falls onto the side of a disk rotating at high speed. The centrifugal force causes the trickle to flow to the next high-speed rotating disk,
A method such as a spinning method in which such operations are performed in two or three stages is known.

Conventional rams obtained by these methods are generally characterized in that most of the fibers are straight, the fiber diameter does not change, and the fiber cross section has a shape close to a perfect circle.

Therefore, mats (blankets) that use fibers as a blanket-like laminate are less likely to get entangled with each other.
Since the fam constituting this material easily slips out, it has the disadvantage of low tensile strength.

In addition, in the case of fiber-reinforced plastics (FRP) that use fibers as reinforcing materials for plastics, etc., the physical bond between the matrix of the plastic and the fibers is weak, and when stress is generated in the material, the interface between the fibers and the matrix Since slipping occurs and the stress is not reliably transmitted from the matrix to the fibers, it has the disadvantage that it is not sufficiently effective as a reinforcing material.

By the way, as conventional techniques aimed at solving the above-mentioned drawbacks, Japanese Patent Laid-Open Nos. 50-35434 and 5
There are inventions disclosed in JP-A-0-118720, JP-A-50-118029, JP-A-51-99124, and the like. In short, these inventions are characterized in that bump-like protrusions are formed in a scattered manner by mixing foreign matter or undissolved matter into the fiber or on the fiber surface. And m! obtained by these inventions! Both of them have defects as fibers, that is, weak parts exist at the interface of foreign substances or undissolved substances, and in most cases, when tensile stress is applied to the fibers,
A mat (blanket) that has sufficient tensile strength or F with a strong reinforcing effect can be used to cut from this defective part or to cut from the defective part when mixed with the matrix.
There were drawbacks such as the inability to provide RP, etc.

[Means for solving the problems and their effects] The present invention provides fibers that solve the drawbacks of the fibers obtained by the prior art, that is, the intertwining between the fibers is improved, and Ia males are difficult to escape. The purpose is to provide fibers that can improve the physical bond between fibers and mats (blanket) or matrix with high tensile strength, and can exhibit excellent reinforcing effects as reinforcing materials for FRP, etc. It is.

The present invention will be explained in detail below.

The fiber of the present invention is a fiber having knob-like bulges having the same composition as the fiber. The Fam has a ratio of the distance between the knob-like parts and the maximum diameter of the knob-like parts to 0.
．． The ratio of the maximum diameter of the knob to the diameter of the fiber portion is in the range of 1.2 to 200. The reason for this is that if the ratio of the distance between the knob-like parts and the maximum diameter of the knob-like parts is 0.1 or less, the intervals between the knob-like parts are too narrow and the matte (
In FRP, the entanglement between fibers is weak, and in FRP, the effect of increasing the physical bond between fibers and matrix is weak.In contrast, if it is 10,000 or more, the spacing between the knobs is too wide and the tensile strength is insufficient. Strong mat (
blanket) or because FRP with a strong reinforcing effect cannot be used, the most suitable range is 0.1 to 10,000.

If the ratio between the maximum diameter of the knob and the diameter of the fiber portion is less than 1.2, the difference is too small as described above and a sufficient effect cannot be obtained, and conversely, if it is more than 200, the difference is too small.

As a fiber, there are drawbacks, namely 1! ! When a weak portion exists at the interface between the fibers and the knob-shaped portion, and tensile stress is applied to most of the fibers, cutting occurs from this defective portion or when mixing with the matrix, cutting occurs from this defective portion, Since mats (blanket) with sufficient tensile strength or FRP with strong reinforcing effect cannot be made, a range of 1.2 to 200 was most suitable.

The fiber of the present invention has an A fL20. In the case of ceramic fibers mainly composed of and S i O, when the content of AmO3 is 75% by weight or more, the viscous resistance of the melt becomes too small, making it difficult to form into fibers and not forming into shots, that is, TA fibers. There were so many ball-shaped things that S i O.

On the other hand, if it exceeds 70% by weight, the melt viscosity resistance becomes too high, making it difficult to stretch and resulting in very thick fibers.
A composition of 0.30 to 70% by weight of Si and 0.225 to 70% by weight of Si is desirable.

Hereinafter, a method for producing a fiber having a knob-like bulge according to the present invention, which is characterized by forming a knob-shaped bulge portion having the same composition as the #I fiber in the Fa fiber, will be described in detail.

A method for appropriately forming knob-shaped portions having the same composition as the fibers in the above-mentioned fibers will be described below.

That is, FIG. 1 is a longitudinal sectional view showing an example of the fiber manufacturing apparatus of the present invention. Reference numeral (1) is a disk, which is rotated at high speed by a rotating shaft (2) attached to the lower center of the disk. A heater is fixed to the lower part of the disk (1), and the disk is heated by heat radiation from the heater.

At the top of the disc, there is a container (4) for heating a composition that is softened by heating, and in the center of the bottom of the container (4), a pore (5) is provided to allow the composition that is softened by heating to flow out. ing.

In the apparatus configured as described above, 500~
The composition is rotated at a high speed of 15,000 rpm, and the composition softened by heating flows out from the pores (5) and is introduced into a disc. The composition is ejected from the disc by centrifugal force and becomes fibers. However, by appropriately changing the flow rate of the composition from the container in this fiberizing operation, a bead-shaped portion having the same composition as the composition, that is, a knob-shaped bulge, can be appropriately formed in the fibers to be formed. fibers are obtained.

As a method for appropriately changing the flow rate of the composition from the container, a flow rate adjustment rod (6) as shown in the 1g1 diagram is provided at the upper center of the pore (5), and this rod (8) is moved up and down as appropriate. The most effective method was to change the cross-sectional area of the composition passing through the pores by
Very good results were obtained within the range of 1111. However, in addition to this method, if the amount of flow flowing onto the disk is changed appropriately, fibers in which bead-shaped portions having the same composition as the composition described above can be appropriately formed can be obtained. Yes, but it is not limited to this method.

Next, the disk used in the present invention will be explained.

The disc used in the present invention has a lower part of the disc in order to keep the composition at a temperature higher than the softening temperature of the composition so that the composition that softens when heated is ejected from the disc by centrifugal force and solidified before being turned into fibers. It is preferable to install a heater. As the heater, nichrome wire, Kanthal wire, molybdenum, tungsten, etc. can be used as appropriate depending on the composition to be converted into wtm. In addition, as a means for heating the disc, other than the heat radiation method using a heater, the temperature of the disc may be maintained at a temperature higher than the softening temperature of the composition to be made into fibers, and the method is not limited to this method.

Regarding the material of the disk, stainless steel, molybdenum, tungsten, etc. are used depending on the composition that turns into fibers.
If the size of the disk is too large, it may cause vibration due to high-speed rotation, resulting in safety problems, and wear and tear on the bearings that fix the rotating shaft attached to the bottom of the center of the disk.If the size of the disk is too small, the production volume There is a problem with less than 100 to 3
A range of 00 layers is desirable.

Next, we will explain the composition that softens upon heating used in the present invention. Examples of the softening composition used in the present invention include silica/alumina, silica-alumina, calcia, magnesia, boric acid, and silica/alumina/calcia/boric acid. Compositions for inorganic fibers, such as those based on magnesia, are advantageous. However, the surface tension when softened by heating is 1 to 800 dyn.
As a result of repeated research, we have found that the zero surface tension can be applied to compositions for organic fibers as well as compositions for organic fibers, as long as the composition has a
If the composition is smaller than n/c+s, the surface tension is too small and it is difficult to form beads, and if the layer is f100dyn/c or more, the surface tension is too high, making it difficult to form into fibers, and the shot content becomes very high.1 ~800dyn/cs+ was found to be good, preferably 50~200dyn
/c was most suitable for making the reinforcing fiber of the present invention.

〔Example〕

Next, examples of the present invention will be described.

A composition containing 50% by weight of SiOl and 0.50% by weight of A fL was heated to 1850°C by heating with thermal radiation from a W heater in a molybdenum container having pores with a diameter of 7 layers at the bottom. After softening to a viscosity of 1 poise, a conical pointed rod with a 30° tip inserted from the upper center of the pore is moved up and down at intervals of 0.2 seconds,
The molybdenum disk was eluted at a rate of 10 g per drop at 0.2 second intervals, and 1 molybdenum disk was eluted by heat radiation from a W heater fixed at the bottom of the disk.
heated to 850°C and at a speed of 5000 rpm to
When a 0φ disc was rotated and fiberized, most of the fiber diameters were within the range of 1.51L to 2.2L, and the average diameter was 2IL, and most of the fibers had diameters of 40 to 100L with the same composition.
The fiber length is mostly within the range of 100 to 300 mm and the average length is 1.
50m5+ fiber and separated shot content is 2%
A blanket-like laminate having a bulk specific gravity of 0.30 g/am'' was prepared from the fibers obtained in this way, and the tensile strength was determined, and the physical properties were as shown in Table 1. A fiber having the following properties was obtained.

Sin, 52% by weight, A fL, 0312% by weight, Ca
A composition containing 20% by weight of O, 5% by weight of Mg, and 0.11% by weight of B was heated in a molybdenum container with 7 mm diameter pores in the bottom in the same manner as in Example 1 by heating with thermal radiation from a W heater. After softening at 1850°C to a viscosity of 30 poise, a conical pointed rod with a 30° tip inserted from the upper center of the pore was heated at 51°C at intervals of 0.2 seconds.
The molybdenum disk was eluted at 0.2 second intervals by vertical movement at a rate of 5 g per drop, and the molybdenum disk was heated to 1650°C by thermal radiation from a W heater fixed at the bottom of the disk, and a circle with a diameter of 200φ was heated at a speed of 8000 rpm. When the plate was rotated and fiberized, most of the fiber diameters were within the range of 6 to 8 μl, with an average diameter of 7 μm.
The diameter of the same composition in the fiber is mostly 100-180 u
Within the range of
It was possible to form fibers with a shot content of 2%, in which the fiber lengths were mostly within the range of 150 to 350 mm at intervals of m, and were separated from the fibers by an average of 180 mm.

The bulk specific gravity of the fiber thus obtained is 0.20 g/cr
A blanket-like laminate of n' was prepared and the tensile strength was determined as shown in Table 1.

Support 1” S i O, 50% by weight, A text, 10335% by weight, M
h.

A 15 wt% composition was softened in advance in a molybdenum container with a diameter of 7H at the bottom at a temperature of 1700° C. and a viscosity of 80 voids by heating with thermal radiation from a W heater, and then inserted from the upper center of the pore. The provided tip is 30
Move a pointed conical stick of ° up and down 5 ■ at intervals of 0.2 seconds,
The molybdenum disk was eluted at 0.2 second intervals at a rate of 2 g per drop, and 17% of the molybdenum disk was heated by heat radiation from a W heater fixed at the bottom of the disk.
Heat to 00°C and reduce the diameter to 20°C at a speed of 7000rpo+.
When a 0φ disk was rotated to make one fiber, most of the fiber diameters were within the range of 10 to 14 IL, with an average of 12 L, and most of the diameters of the fibers with the same composition were within the range of 150 to 250 IL. The fiber length is mostly within the range of 100 to 250 t+a, and the shot content is 3%.
It was possible to form fibers of

The bulk specific gravity of the fiber thus obtained is 0.1 g/c
A blanket-like laminate of m' was prepared and the tensile strength was determined as shown in Table 1.

Ratio "L Example" Engineering SiO, 50% by weight 1. I'll add 0.50% by weight of the composition to the bottom in advance as in Example 1. Ill
After softening to a temperature of 1,850°C and a viscosity of 1 poise by heating with thermal radiation from a W heater in a molybdenum container having pores with a diameter of When masculinization was carried out using the conventional method of blowing high-speed air at kg/cm' into the stream, it was found that most of the fiber diameters were within the range of 1 to 3 colors, with an average of 2 JL, and there were no beads in the fibers except at both ends of the fibers. Fibers with no shaped parts! The a length is mostly within the range of 30 to 150 tL, and the average is 85 t+s
It was possible to form fibers with a shot content of 30% that were largely separated from the fibers.

This is how it was obtained! Bulk specific gravity of a fiber 0.1g/am
A blanket-like laminate was prepared and the tensile strength was determined as shown in Table 1.

"No Shibori 1" SiO, 52% by weight, A cross 0112% by weight, CA02
A composition of 0% by weight, 5% by weight of Mg, and 11% by weight of Bo was heated to a temperature of IE150 by heating with thermal radiation from a W heater in a molybdenum container having 7II11 diameter pores in the bottom in the same manner as in Example 1. After softening to a viscosity of 30 poise at °C, it was formed into a trickle through the pores at a rate of 1500 g per minute, and fiberization was performed using the conventional method of blowing high-speed air at a pressure cuff of kg/am' into the trickle. , the fiber diameter is mostly within the range of 50 to 180 cm, with an average of 90 cm.
It was possible to form fibers with a shot content of 25% that were separated from the TA fibers using Rinho.

The bulk specific gravity of the fiber thus obtained is 0.208/c
A blanket-like 8&layer body of m' was prepared and the tensile strength was determined as shown in Table 1.

"Saramosquito" Si 0.50% by weight, Asha 0.35% by weight, Mg0
A 15% by weight composition was softened in a molybdenum container with a diameter of 7 mm at the bottom by heating with thermal radiation from a W heater at a temperature of 1700°C to a viscosity of 80 poise, and then the pores were softened at a rate of BOOg per minute. Fiberization was performed using the conventional method of forming a trickle through a pressure cuff and blowing high-speed air at a pressure cuff of kg/am'' into the trickle.

The fiber diameter is mostly within the range of 6-15g, with an average of 12p
It was possible to form fibers with a shot content of 20% that had no bead-shaped parts in the fibers other than the ends of the fibers, had fiber lengths within the range of 60 to 20 hm, and were separated from the fibers by an average of 110 mm. .

A blanket-like laminate with a bulk specific gravity of 0.10 g/c was made from the fibers obtained in this way, and the tensile strength was determined.
It was as shown in Table 1.

The m and it diameters obtained by the same method as in Example 1 were mostly within the range of 1.5 to 2.2 mm, with an average of 2 mm, and the diameters of the fibers with the same composition were mostly 40 mm. ~ 100 dos, with an average of 50 bead-shaped parts, with #a fiber length being mostly 10 at intervals of 0.5 mm.
Fibers with a shot content of 5%, which are within the range of 0 to 300 m weight and separated from the fibers by an average of 150 mm, are
% in an aqueous solution of minosilane, I! ! After excessive separation, the fibers are dried at 130°C and the surface of the fibers is coated with an aminosilane coupling agent.Next, the fibers are poured into water to form a slurry, and the slurry is gradually introduced into the same cylindrical container. Pressurized water is sent through the side wall to generate a thin stream, and in the eddy stream, the fibers are untangled, and at the same time, the shot content and large diameter fibers that have been separated from the fibers are separated, and after drying, they are processed using a roller press. Smash.

Most of the fibers whose surfaces were coated with the 7-minosilane coupling agent had a diameter of 1.4 to 1.9 J.
Within the range of L, the average is 1.81L, and the fiber length is mostly 1.
It is within the range of 00 to 250 IL with an average of 125. .

Fibers with a shot content of 0.1% separated from the fibers and 70 wt% of nylon 6 resin pellets were blended, mixed and kneaded in an extruder, and then injection molded to obtain a fiber composite plastic molded article.

Most of the fiber diameters obtained by the same method as Comparative Example 1 were within the range of 1 to 3 L, with an average of 2 L, and there were no bead-shaped parts in the fibers except at both ends. Fiber length is mostly 30-1
Fibers with a shot content of 30% that are within the range of 50 mm and separated from fibers with an average diameter of 65 mm are coated on the surface with an aminosilane coupling agent in the same manner as in Example 4. Most of the fibers have a diameter of 1 to 2. The fiber length is mostly within the range of 100 to 250 IL and the average is 125 JL, and the shot content separated from the fiber is 8% @ll-30wt% and nylon. 6 resin pellets were blended, mixed and kneaded using an extruder, and then injection molded to obtain a fiber composite plastic molded product.

The fiber composite plastic molded article thus obtained was subjected to the physical property evaluation test shown below, and the results are shown in Table 2.

The tensile strength is based on ASTM D638.

The flexural modulus is according to ASTM 0790.

(The following is a blank space) Table 1 Table 2 [Effects of the Invention] As described above, according to the present invention, the following effects are produced.

(1) The intertwining between laM and mM became stronger, and the tensile strength of the mat made from the blanket-like end layer of fibers was significantly improved.

(2) Excellent reinforcing effect can be obtained by combining Fjll fibers and plastic. By using the fibers of the present invention in fiber composite plastics, the physical bond between the plastic and the fibers is strengthened, resulting in better mechanical strength. In particular, the tensile strength was significantly improved.

[Brief explanation of drawings]

FIG. 1 is a schematic cross-sectional view of an apparatus for producing a fiber having knob-like bulges according to the present invention, and FIG. 2 is a diagram showing the shape of the fiber obtained according to the present invention and a conventional mra. ■... High-speed rotating plate 2... Rotating shaft 3... Heater 4... Heating container 5... Pore 6... Flow rate so-called 1! L rod 7... Reinforcing fiber of the present invention 8... Conventional fiber patent applicant IBIDEN Co., Ltd. Figure IBZ country 1,000 6d #1 official book (auto-5e4> January 29, 1978) Director of the Japanese Patent Office Kuro January 2016, 2.95 Name of Patent Application No. 72068, 161 Related Patent Applicant Address 3rd floor, Marukichi Building, 2-111 Kanda-cho, Ogaki City, Gifu Prefecture 500 m (0582) 66-74:10 (Representative)
5. Date of amendment order (voluntary) 6. Subject of amendment (1) Specification - 2. “Claims” column (2) Specification;
``Detailed Description of the Invention II J Column (3) 17I Page 7 Contents of Amendment (1) The ``Claims'' of the specification of the present application are amended as shown in the attached sheet. (2) IJ11 Fine Dimensions, page 3, line 10 and line 1
In the second line, "disc" is corrected to "disc". (3) Page 13, line 7 to line 8 of the specification [in 1]. It says, "Fibers with physical properties as shown in Table 1 were made into #11 fibers." Correct to read, "They were as shown in Table 1." (4) In the specification, page 14, line 15 +1. The expression "r l 5 wt%" is corrected to "r15 wt%". (5) On page 14 of the specification: line 515, 17 m
``The diameter of m'' is corrected to ``a pore with a diameter of r7 mm''. (6) On page 16, line 8 of the specification, “30 to 150
r3. Correct it to O~150mmJ. (7) In the 9th line of page 16 of the TJL Specification, the phrase ``fiber and bulk and separation'' has been amended to read ``fiber and separation.'' (8) On page 16, line 15 of the specification, rcAOJ is corrected to rcaOJ. (10) In the fifth line of page 17 of the specification, the phrase "The majority of the fiber diameter is within the range of 50 to 180 mm" has been replaced with "The majority of the fiber diameter is within the range of 3 to 1 OIL." The average length of the fibers is 7μ, there are no bead-shaped portions in the fibers other than the ends of the fibers, and the length of the fibers is mostly within the range of 50 to 180 mm. (!■) On page 17, line 13 of the specification. It is corrected to read "a pore with a diameter of r7 mm". (12) On page 19, line 12 of the specification. r 70 wt%" is corrected to "70 wt 5%). (13) In the first line of page 20 of the specification. 1
Correct it to 50mmJ. (14) On page 20, line 7 and line 8 of the specification, the phrase "r w t%" is amended to read "weight b)%." (151J) In Table 1 on page 21 of the specification, the units in the "Tensile strength" column shown on the left side are corrected to "r K g / cm J". (16 ) Among the drawings of the present application, Figure 1 is amended as shown in the attached sheet. 8. List of attached documents (L) 1 document stating the scope of claims (2) Drawing (Figure 1) 1 sheet ( Attachment) 2. Claims 1), m,! The ta male has a knob-like bulge made of the same composition as the fiber, and the ratio of the distance between the knob-shaped parts and the maximum diameter of the knob-shaped part is 0.1 to
It is within the range of 1000G, and the maximum diameter of the knob-like part and the H of the part other than the knob-shaped part! The ratio to the diameter of the Ala part is 1.2~
A fiber having a knob-like bulge, characterized in that the fiber has a bulge in the range of 200. 2) The knob-shaped fiber according to claim 1, wherein the fiber is a ceramic fiber mainly containing 30 to 75% by weight of A-O and 25 to 70% by weight of SiO. Fibers with bulge. 3) After softening the composition that softens by heating, 0
．． The composition is poured onto a disc rotating at a circumferential speed of 5 to 400 a/sec, and the composition is ejected from the upper plate by centrifugal force.
A knob-like bulge characterized by producing a fiber having a knob-shaped bulge having the same composition as the composition in the fiber formed by pulsating the outflow amount of the composition by forming aia. A method for producing a fiber having 4) As a method for pulsating the flow rate of a composition that softens by heating from a container, the composition that softens by heating is softened in a container having pores at the bottom, and the pores through which the composition passes are cut. 4. The method for producing fibers having knob-like bulges according to claim 3, characterized in that a flow rate adjustment rod that changes the area is moved up and down. Figure 1

Claims (1)

[Scope of Claims] 1) A fiber having a knob-like bulge having the same composition as the fiber, the distance between the knob-shaped parts and the maximum diameter of the knob-shaped part Ratio is 0.1-10
000, and the ratio of the maximum diameter of the knob-shaped portion to the diameter of the fiber portion other than the knob-shaped portion is in the range of 1.2 to 200. 2), the fibers mainly contain 30 to 75 Al_2O_3
The fiber having knob-like bulges according to claim 1, which is a ceramic fiber containing 25 to 70% by weight of SiO_2. 3) After softening the composition that softens by heating, 0.
Flow out onto a disc rotating at a circumferential speed of 5 to 400 m/s,
By ejecting the composition from above the disk using centrifugal force and turning it into fibers, the fibers formed by pulsating the outflow amount of the composition have knob-like bulges having the same composition as the composition. A method for producing fibers having knob-like bulges, the method comprising producing fibers. 4) As a method for pulsating the flow rate of the composition that softens by heating from a container, the composition that softens by heating is softened in a container having pores at the bottom, and the pores through which the composition passes are cut. 4. The method for producing fibers having knob-like bulges according to claim 3, characterized in that a flow rate adjustment rod that changes the area is moved up and down.