JPS5943112A - Manufacture of polyvinyl alcohol synthetic fiber - Google Patents
Manufacture of polyvinyl alcohol synthetic fiberInfo
- Publication number
- JPS5943112A JPS5943112A JP14964082A JP14964082A JPS5943112A JP S5943112 A JPS5943112 A JP S5943112A JP 14964082 A JP14964082 A JP 14964082A JP 14964082 A JP14964082 A JP 14964082A JP S5943112 A JPS5943112 A JP S5943112A
- Authority
- JP
- Japan
- Prior art keywords
- cement
- fiber
- polyvinyl alcohol
- fibers
- coagulation bath
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B16/00—Use of organic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of organic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B16/04—Macromolecular compounds
- C04B16/06—Macromolecular compounds fibrous
- C04B16/0616—Macromolecular compounds fibrous from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B16/0641—Polyvinylalcohols; Polyvinylacetates
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Artificial Filaments (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は,ポリビニルアルコール(以下PVAと略記す
る。)系合成繊維の製造法に関するものであり,更に詳
しく(徒セメント補強材として好適なPVA系合成繊維
の製造法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing polyvinyl alcohol (hereinafter abbreviated as PVA)-based synthetic fiber, and more specifically relates to a method for producing PVA-based synthetic fiber suitable as a reinforcing material for cement. It is something.
PVA系合成繊維の湿式紡糸法としては,第一にPVA
系水溶液を硫酸ナトリウム(以下ボウ硝と略す。)等の
飽和水溶液の凝固浴に紡出する方法が知られている。こ
の方法で得られる繊維の横断面は馬蹄形で二重構造を有
l〜てbる。ただ,この繊維tま強度及びヤング率がそ
れほど高くないのでセメント等の補強材としては充分な
効果を有するものではない。第二にPVA系水溶液を濃
厚力性アルカリの凝固浴に紡出する方法が知られている
。この方法で得られる繊維は高い強度及びヤング率?有
するが,繊維の横断面は円形である。第三にPVA水溶
液にキレート架橋が成立するホウ酸や銅塩等を添加し少
量のカ性アルカリと飽和ボウ硝水溶液の凝固浴に紡出す
る方法が知られている。この方法で得られる繊維の性能
は高い強度及びヤング率を有するが,fR卸の横断面I
tsI靖円形である。The first wet spinning method for PVA-based synthetic fibers is PVA
A method is known in which a system aqueous solution is spun into a coagulation bath of a saturated aqueous solution such as sodium sulfate (hereinafter abbreviated as sulfate). The fibers obtained by this method have a horseshoe-shaped cross section and a double structure. However, since the fiber strength and Young's modulus are not so high, it is not sufficiently effective as a reinforcing material for cement, etc. A second known method is to spin a PVA-based aqueous solution into a concentrated alkaline coagulation bath. Does the fiber obtained by this method have high strength and Young's modulus? However, the cross section of the fiber is circular. Thirdly, a method is known in which boric acid, copper salt, etc. that form chelate crosslinking are added to an aqueous PVA solution, and the resulting solution is spun into a coagulation bath of a small amount of caustic alkali and a saturated aqueous salt solution. The performance of the fiber obtained by this method is high strength and Young's modulus, but the cross section of fR wholesale I
It is a tsI circular shape.
一方,セメントをベースにした成形品,各種構築物等に
必要とされる材料特性としては曲げ強度,衝撃強度及び
ひび割れ強度等があげられ.このグこめ各種の補強材が
使用されている。すなわち,補強材として無機繊維や有
機繊維をセメントマトリックスの中に分散さすことが行
われている,.無機繊維としそは石綿を配合したスレー
ト板が代表的であり,又耐アルカリガラス繊維を配合し
たガラス繊維強化セメント成形品.ある1いは鋼繊維等
を補強材としたセメント成?形品も知られている。一方
,有機繊維としてはポリエチレン系.PVA系あるいは
ポリプロピレン系等の合成繊維も一部補強材として使用
されている。On the other hand, material properties required for cement-based molded products and various structures include bending strength, impact strength, and cracking strength. Various reinforcing materials are used for this purpose. In other words, inorganic fibers and organic fibers are being dispersed into the cement matrix as reinforcing materials. A representative example of inorganic fibers is slate boards containing asbestos, and glass fiber-reinforced cement molded products containing alkali-resistant glass fibers. Or is it made of cement with reinforcing materials such as steel fibers? Shapes are also known. On the other hand, polyethylene is an organic fiber. Some synthetic fibers such as PVA or polypropylene are also used as reinforcing materials.
しかしながら・石!VC″Aては発ガ7性物質と認定さ
れ健康障害の問題があり..又供給のすべてを輸入にた
よっており不安定アあるという問題がある。又スレート
板は性能面で衝撃強度が.低いという問題がある。又,
耐:アルカリガラス繊維は耐アルカリ性がそれ程完全で
はなく,セメント成形後時間と共に曲け強度が低下する
という問題があるので,その用途はカーテンウオールや
外壁バネルK使用され非構造材に限定されているし,又
作業性についても皮膚障害が発生するという問題がある
。一方,合成繊維については前記PVA系合.:成*’
Mに見られる如く繊維の横断面形状が円形や..楕円1
2.杉あるいは馬蹄形であるのでセメントとの接“’I
M種”’JE%(,又ヤング率がセメントマトリックス
より小さいためにひび割れ強度に問題を残しているジこ
れに対し,繊維横断面異形化PVA系合成繊維として,
!I?開昭56−140113号公報に炭酸カルシウム
等,特開昭56−154513号公報に硫酸マグネシウ
ム等を混合紡糸する方法等が提案されて″′4が・紡調
が不安定1あり・又混合物?一部が浴中に溶出するため
湿熱浴の管理が繁雑であるという問題がある。However, stone! VC''A is recognized as a gas-causing substance and poses a health hazard.Also, all supplies are dependent on imports, resulting in instability.Also, slate boards have low impact strength in terms of performance. .There is a problem that the value is low.Also,
Resistance: Alkali glass fiber does not have perfect alkali resistance, and its bending strength decreases over time after cement formation, so its use is limited to non-structural materials, such as curtain walls and exterior wall panels. However, there is also the problem of workability in that skin disorders occur. On the other hand, regarding synthetic fibers, the PVA-based composites mentioned above. :Nari*'
As seen in M, the cross-sectional shape of the fiber is circular. .. Ellipse 1
2. Because it is cedar or horseshoe-shaped, there is no contact with cement.
In contrast, as a PVA-based synthetic fiber with deformed fiber cross-section,
! I? Japanese Unexamined Patent Publication No. 56-140113 proposed a method of mixing calcium carbonate, etc., and Japanese Unexamined Patent Publication No. 56-154513 proposed a method of mixing and spinning with magnesium sulfate, etc. ``'4 ・Unstable spinning 1 ・Additionally, a mixture? There is a problem in that the management of the moist heat bath is complicated because a part of it is eluted into the bath.
繊維による七メ.ント成形品等の補強に際しては.繊維
の強度及びヤング率が高く仝れば成形品の曲げ強度も高
くなることが一般に認められており,又繊維とセメント
との接着強度が高くなればなる程その補強効果がより充
分なものとなることも一般に認められている。Seven fibers. When reinforcing molded products etc. It is generally accepted that the higher the fiber strength and Young's modulus, the higher the bending strength of the molded product, and the higher the adhesive strength between the fiber and cement, the more sufficient the reinforcing effect will be. It is also generally accepted that
そこで本発明者らは,耐アルカリ性が良好で.強度及び
ヤ・ング率が高く,セメントとの接着性が良好でセメン
トの補強効果が優れ,かつ健康障害や皮膚障害がない繊
維を生産管理・も容易に製造する方法を提供することを
泪的と.・して鋭意研究の結果.ホウ酸又は銅塩を含?
有するP■・A系紡糸原液を特定の凝固浴中に紡出し.
?繊維を・製造することによって上記の泪的が達成でき
るという事実を見い出し.本発明に.到達したもの・・
である。Therefore, the present inventors discovered that the alkali resistance is good. Our mission is to provide a method for easily manufacturing fibers with high strength and young modulus, good adhesion to cement, excellent reinforcing effect on cement, and no health or skin problems. and.・Results of intensive research. Contains boric acid or copper salts?
The P■/A-based spinning stock solution having the following properties is spun into a specific coagulation bath.
? Discovered the fact that the above aspirations can be achieved by manufacturing fibers. To the present invention. What we have reached...
It is.
すなわち本発明は・,ホウ酸又は銅塩を添加したPVA
系紡糸原液をが性アルカリ′濃度(XIl/t)及び脱
水性塩類濃度(Y11/t)が下記(a).(b)−(
c)式の条件を同時に満足する凝固浴・中に紡出し,つ
いで常法の中和,湿熱処理を行った後,水洗,乾燥し.
更K熱延伸を施すことを特徴とするPVA系合成繊維の
製造法である。That is, the present invention is based on PVA to which boric acid or copper salt has been added.
The concentration of alkali (XIl/t) and the concentration of dehydrating salt (Y11/t) of the spinning dope are as follows (a). (b)-(
c) It is spun into a coagulation bath that satisfies the conditions of formula at the same time, and then subjected to conventional neutralization and moist heat treatment, followed by washing with water and drying.
This is a method for producing PVA-based synthetic fibers, which is characterized by subjecting it to further K hot stretching.
Y≦415−1.68X(a)
Y≧850−5X(b)
Y≧185−0.58X(e)
本発明によれば,従来のPVA・系合成繊維のような馬
蹄形,til!円形あるい?は円形の横断面の場合忙は
見られなかった角のある横断面を有し,しかも場合によ
っては1〜3ミ久ロンの突起を有する繊維が得られる。Y≦415-1.68X (a) Y≧850-5X (b) Y≧185-0.58X (e) According to the present invention, the horseshoe-shaped, til! Is it circular? Fibers are obtained which have an angular cross section, which was not observed in the case of a circular cross section, and in some cases have protrusions of 1 to 3 μm.
本発明の方法によってPVA系合成繊維を製造するには
,紡糸原液としてホウ酸又は銅塩を添加したPVA系紡
糸原液を用いることが必要である。In order to produce PVA-based synthetic fibers by the method of the present invention, it is necessary to use a PVA-based spinning dope to which boric acid or copper salt has been added.
本発明に用いられる銅塩としては,たとえば硫酸第一?
銅,硫酸第二銅,硝酸銅などの水溶性銅塩があげられる
が.特に好ましいのは硫酸第二銅である。ホウ酸又は銅
塩の添加量はPVAに対し0.3〜4重量係,好ましく
は0.6〜2重量チである。Examples of copper salts used in the present invention include sulfuric acid-1?
Examples include water-soluble copper salts such as copper, cupric sulfate, and copper nitrate. Particularly preferred is cupric sulfate. The amount of boric acid or copper salt added is 0.3 to 4 parts by weight, preferably 0.6 to 2 parts by weight, based on PVA.
本発明に用いるPVAの好ましい平均重合度は1000
〜2500,特に1300〜1800である。PVAo
ケン化度は特に限定されないが99.5〜98モルチの
ものが好ましい。紡糸原液中のPVAの濃度は10〜2
5重量チ.特に14〜20重量チが好ましい。紡糸原液
のPRは原液がアルカリ性となるとゲル化が起こり,一
方,あまり低くなりすぎると装置等の腐蝕の問題が発生
するので4.0〜548の範囲が好ましい。The preferred average degree of polymerization of PVA used in the present invention is 1000.
~2500, especially 1300-1800. PVAo
Although the degree of saponification is not particularly limited, it is preferably 99.5 to 98 mol. The concentration of PVA in the spinning stock solution is 10-2
5 weight chi. Particularly preferred is 14 to 20 weight. The PR of the spinning dope is preferably in the range of 4.0 to 548, since gelation occurs when the dope becomes alkaline, and on the other hand, if it becomes too low, problems of corrosion of equipment etc. occur.
本発明においては,かかる紡糸原液を.カ性アルカリ濃
度(XI/t>及び脱水性塩類#′度(Y1/t)が前
記(a)−’(b).(c)式の条件を同時に満足する
・従固浴中に紡出することが必要である。In the present invention, such a spinning stock solution is used. The caustic alkali concentration (XI/t> and the degree of dehydrating salts #' degree (Y1/t) simultaneously satisfy the conditions of the above formulas (a)-'(b).(c).Spinning in a solid bath It is necessary to.
第1図は本発明の凝固浴糸件を示ずグラノであり,タテ
軸1・:j−脱水性塩類(/aINF(E//,),ヨ
コ軸は力性アルlil濃度(9//)であり,斜線で囲
まれた部分が本発明のνf固浴須域である。Figure 1 shows the coagulation bath properties of the present invention, but the vertical axis shows the concentration of 1. ), and the area surrounded by diagonal lines is the νf hard bath area of the present invention.
カ性アルカリとしてv」.たとえばカ性ソーダ.カ性カ
リが好土し〈用いらわ、る。カ性アルカリの濃度か13
19/t未イγ4の場合・は.得られる繊テ.{[の横
断而が11′1円形であり.一方209gltを越える
』希合は購断面が円形である。脱水性塩類と1〜て(づ
:,7’Cとえばボウ硝.硫酸カリウノ・,硫酸亜鉛,
値酸マグネシウム,硝酸ソーダなどが川いられるが,!
[♀に好斗しいのC・よボウ硝である。脱水性塩類の濃
度14力性アルカリか130E/tの場合2009/t
でほぼ飽和に達【2.一方64ji/L未満の場合は紡
調が悪い。(a.)5(.:U、!〕高’6:λ度のカ
性アルカリあるいは脱水{’LjXK類k・含むj′f
固浴は脱水性塩類がほぼ飽和に達[7ていl)Li’)
で作成できプrい1−2,又(b)式及び(e)式より
カ性アルカリあるい(rま脱水性塩類が低(農度の場含
ぱ得られる繊、イtの債助而が円形ないし楕円形とkる
。凝固浴の温1{(は35−55℃:.行に40〜55
℃が好一ましい。As a causative alkali v”. For example, caustic soda. Potassium is a good soil. The concentration of caustic alkali is 13
In the case of γ4 without 19/t. The resulting fiber. The cross section of {[ is 11'1 circular. On the other hand, the purchasing surface of "over 209 glt" is circular. Dehydrating salts and
Magnesium acid, sodium nitrate, etc. can be found in the river, but!
[This is C. Yobousou, who is very friendly with the male. If the concentration of dehydrating salts is 14% alkali or 130E/t, 2009/t
It reached almost saturation at [2. On the other hand, if it is less than 64 ji/L, the spinning quality is poor. (a.) 5 (.:U,!] High'6: λ degree caustic alkali or dehydration {'Lj
The solid bath is almost saturated with dehydrating salts.
1-2, and formula (b) and formula (e), the content of caustic alkali or dehydrating salts is low. The temperature of the coagulation bath is 35-55℃: 40-55℃.
℃ is preferable.
木発明Vこおいては。凝固浴を出た糸条を常法1(より
中和,湿熱処理を行った後.水洗.乾燥し,更に熱4!
F;伸する。熱ク1r′.伸(で続いて20旧:以十,
y要すれば好才し〈は230〜2.50Cで熱処理する
。Wood invention V here. After leaving the coagulation bath, the yarn is neutralized using the conventional method 1 (after being subjected to moist heat treatment, washed with water, dried, and further heated to 4!
F: Stretch. Heat 1r'. Shin (followed by 20 old: 10,
If necessary, heat treat at 230 to 2.50C.
本発明の方法に。しり{!!’v:hるPv八系合成恢
肩ずは?).水性で,酊アルカリ性なのでセメントマト
リノクスに充分・馴み.かつセメントマトリックス中で
も侵されない。又高い::IIrIXリ,ヤング率を有
(7ていZ)。従一って9このs:*.pxイpで補強
さナシ/r.セメント成形晶(.li:匣J7−/辷曲
げrjia度及びひび11、+jh.強度を41′干ろ
。To the method of the invention. Shiri {! ! 'v: hru Pv 8 series synthetic combination shoulder? ). It is water-based and alkaline, so it is compatible with cement matrix. And it is not attacked even in cement matrix. It also has a high Young's modulus (7% Z). Juichi 9 this s: *. Not reinforced with px ip/r. Cement forming crystal (.li: box J7-/bending rjia degree and crack 11, +jh. strength 41' drying.
又.本発明の方l,りにより得らノ1,/ζ性N11邑
従フ1クの馬蹄形,1貰円形及び円形の横1新而と&;
tlAなる異形化された11゛^断而4・有する。従一
)て.」=メントに混和された場合,投錨効果によりセ
メントとの接着効果を発揮するものである。又,イ!!
られた慮託は114度な伸17):′7t有ずるので耐
衝撃件dγ善にも効果がある。or. According to the method of the present invention, the horseshoe shape of the /ζ property N11 and the circular shape and the horizontal shape of the circular shape and &;
It has a deformed 11゛^but4 called tlA. Juichi) Te. When mixed with cement, it exhibits an adhesive effect with cement due to its anchoring effect. Again, yes! !
Since the given consideration has an elongation of 114 degrees 17):'7t, it is also effective in improving the impact resistance.
本発明の方法により得らハ,た熾1f.f[を{il.
j川L?5i!式抄造法でセメント積層板を成形する場
合の繊維添加量0寸,セメントマトリックス中での繊糸
tの分散性と曲げ強度乃び衝慇強度を考慮すると,好斗
1,〈は(13〜25M〔惜チ,とくに0.5〜2重E
λ係が,1′{好である。Obtained by the method of the present invention 1f. f[{il.
J river L? 5i! When forming a cement laminate using the paper-making method, considering the fiber addition amount of 0, the dispersibility of the fibers in the cement matrix, the bending strength, and the impact strength, the 25M [Sadly, especially 0.5~2 double E
The λ coefficient is 1'.
以1−゛,実IX(口lJリをあげて本発明をさらに具
体的に説明する。Hereinafter, the present invention will be explained in more detail with reference to Example 1-1.
尚,繊だ1補強セメント板の作成と性能測定r:l:,
PVA系合成糊λzIfと(2て6mml)こ切断した
ものを4!・用L,以}のとおり行った。In addition, the preparation and performance measurement of fiber 1 reinforced cement board r:l:,
PVA-based synthetic glue λzIf (2 to 6 mml) was cut into 4 pieces!・I did it as follows.
(1)曲げ強1戊,四性,衝撃強度
繊維22@部,バルプ3重ト」.部,スペシrルクレイ
10重t部峻び普;ljlボノレトランドセメント85
重M部を混合し2.湿式抄造法(lζてセメン}f一t
層板を成形し,次いで2旧〕,湿空中で2811間養生
1−7セメント板を作成した。このスレート板について
tit口げ強度,シャルピー衝撃強度を測定した。尚靭
性C↓曲げ強度測定チヤ−1一紙より面積比で示した。(1) Bending strength: 1 x 4, impact strength: 22 parts, bulge: 3 parts. part, special clay 10 weight t part sharp; ljl Bonoretland cement 85
2. Mix the heavy M part. Wet papermaking method
The laminate was molded and then cured in humid air for 2811 hours to create a 1-7 cement board. The tit tip strength and Charpy impact strength of this slate board were measured. Toughness C ↓ Bending strength measurement chart 1 It is shown as an area ratio from a piece of paper.
(2)ひび割れ強度
i.:RAJk.普通ボルトランドセメント,硅砂5号
及び水を0.003対1対2対0.5の重h[割合で混
合し,得られたモルタルを用いてリング拘束試験法(鋼
製リングの内径83m.モルタルリング20mm厚さ)
により,ひび割れが発生する日数を求めた。(2) Crack strength i. :RAJk. Ordinary Boltland cement, silica sand No. 5, and water were mixed in a ratio of 0.003:1:2:0.5, and the resulting mortar was tested using the ring restraint test method (steel ring with an inner diameter of 83 m. mortar ring 20mm thick)
The number of days for cracks to occur was determined.
(3)繊維どセメントとの接着性
繊維をセメントに対し0.2重量係添加し,水とセ5メ
ントの比率全05とし,セメントとし,ては普通ボルト
ランドセメントを用いてセメント中Vこiiqa;iを
分散させた。(3) Adhesiveness with fiber cement Add 0.2 weight of fiber to the cement, make the total ratio of water and cement 0.5, and use ordinary boltland cement as cement. iiqa;i was dispersed.
このものを20℃,湿空中で411間養生し七メン}・
仮を得,得られたセメント版を破断し.破断面の繊維の
吐出長を測宇した。(吐出畏の・℃σかい方が接イI′
1.が自好である。)実施例1.2.比較例1〜3
平均重合1131490(7)PVA肴:16%度カ1
6.2,fI〕となるよう水に溶解し,イUらノ1,た
浴液にPVAに対+,i.:3重縫φのボウ酸を添力1
目−.puを57に調整して紡糸原帛を作成した。この
紡糸原液を,水酸化ナトリウム15t)g/t,ボウ硝
1.601!/l−で50Cのアルカリ性のj盆類浴を
凝固浴として紡出1−2,第1ローラーと第2ローラ間
で418IJl〔伸した後,ボウ硝3001/t,硫酸
2511/t金含む酸性の塩戸浴にて40℃で中和処理
いついでボウ硝3’609//,,硫酸20g/tを含
む酸性の塩類浴に?で90で+湿熱処理を行った後水綜
?用い洗浄し,さらに油?剤処理[,.乾燥後235℃
の熱風中に′C4倍臓延伸口次に24(1℃で定長熱処
理を行ってPVA系合成繊維を得た(実施例1)。This material was cured for 411 days at 20℃ in a humid atmosphere.
A temporary template was obtained, and the obtained cement slab was fractured. The discharge length of the fibers at the fracture surface was measured. (The way of discharge is ℃σ is close to I'
1. is selfish. ) Example 1.2. Comparative Examples 1 to 3 Average polymerization 1131490 (7) PVA appetizer: 16% degree strength 1
6.2, fI], and added PVA to the bath solution, i. :Add 1 boric acid of triple stitch φ
Eyes. A spinning fabric was prepared by adjusting pu to 57. This spinning stock solution was mixed with sodium hydroxide (15 t) g/t and sulfate (1.601 g/t). Spinning 1-2 using a 50C alkaline bath as a coagulation bath at /l-, after stretching 418 IJl between the first and second rollers, acid containing gold 3001/t, sulfuric acid 2511/t Neutralized at 40℃ in a Shioto bath, followed by an acidic salt bath containing 3'609//, sulfuric acid and 20g/t of sulfuric acid. So after performing + moist heat treatment at 90? Use, wash, and even oil? agent treatment [,. 235℃ after drying
A PVA-based synthetic fiber was obtained by subjecting it to constant length heat treatment at 24° C. (Example 1).
壕だ,熱延伸倍率を4倍から3.5倍に変?えた他は実
施例1と同一条件でl)VA系合成繊維を得?た(実施
例2)。?
得られた繊維の性能を表−1に示す。又繊維の横断面は
第2図(実施例1)及び第3図(実施例2)雇示すとお
りであった。又,ζの繊維を用いて作成したセメント板
の性能Q」.表−1に示すとおりであった。It's a moat, change the hot stretching ratio from 4x to 3.5x? l) VA-based synthetic fiber was obtained under the same conditions as in Example 1. (Example 2). ? Table 1 shows the performance of the obtained fibers. The cross section of the fiber was as shown in FIG. 2 (Example 1) and FIG. 3 (Example 2). Also, the performance Q of cement board made using ζ fibers. It was as shown in Table-1.
比較のため,凝固浴を以下の通り変えた他?は実施例1
と同一条件セ繊維を製造し.以下実施例1と同様に繊維
及びセメント板の性?能を測定し尼。For comparison, the coagulation bath was changed as shown below. is Example 1
The fibers were produced under the same conditions. Below, as in Example 1, what are the properties of fiber and cement board? Measuring ability.
その結果は表−1に示すとおりであった。反,繊比較例
1;ボウ硝asOg/t,水酸化ナトリウム15117
’l−’mgll1.50C.(第”4図)■′較?例
2:水酸化ナト’U”tム3’50g/t.温度2o?
一?d(麹51鮪)?
:゛ルm4u?3’:ボウ硝42bI/t.温度40℃
(第6図)但し,比較例3は熱延伸4″倍でi試料が採
取できな1かったので′248倍で繊維を製造した。The results were as shown in Table-1. Anti-fiber Comparative Example 1; AsOg/t, sodium hydroxide 15117
'l-'mgll1.50C. (Figure 4) Comparison Example 2: Sodium hydroxide 'U't 3'50g/t. Temperature 2o?
one? d (koji 51 tuna)? :゛ru m4u? 3': Bowsalt 42bI/t. Temperature 40℃
(FIG. 6) However, in Comparative Example 3, it was not possible to collect sample i at 4'' hot stretching, so a fiber was produced at 248 times hot stretching.
対照例二′石綿補強(ス?レート板)
PVA系合成繊維無添加め?セメント積層板1は,ク″
?リソタ:イル?ア亥べ支ト5R”151fC隈部−バ
ルプ3重量部及び普通ボルトランドセメント82重量部
を混合し作成した。?
実施?例1で得られた繊維は比較例1.2の繊維に比べ
若干高いヤン?グ率を示している。又,′繊維横断面は
異形化されている。★施例2で得られだ′+a′維は比
較例1,2の繊維?に比べ低いヤング率,強度を示して
いる。又繊維横断?面は異形化してい1る噌この繊維を
補強材としたセメン?ト:板の性能は実施例め繊維補強
セメントの方が比較例及び対照例より優れて込た。Comparative example 2' Asbestos reinforcement (slate board) PVA-based synthetic fiber additive-free? The cement laminate 1 is
? Risota: Iru? The fibers obtained in Example 1 were slightly higher than the fibers in Comparative Example 1.2. Young's modulus is shown.Furthermore, the fiber cross section is deformed.★The '+a' fiber obtained in Example 2 has a lower Young's modulus and strength than the fibers of Comparative Examples 1 and 2. In addition, the cross-sectional surface of the fibers is irregularly shaped.Cement using this fiber as a reinforcing material: The performance of the board with the fiber-reinforced cement of the example is better than that of the comparison and control examples. Ta.
:実施例2け強度.ヤング率が若干低い繊維を使用した
ものであるが,横断面が異形化してIA′るため補:強
効果が優れるもめと推察される。: Example 2 strength. Although fibers with a slightly lower Young's modulus are used, the cross section is irregularly shaped and becomes IA', so it is presumed that this is due to the excellent reinforcement effect.
突施?例3,比較例・4.5
平均重合度1300のPVAを濃度が18:((’,J
i(%となるよう水に溶解し・.得られたrδ液にP’
iV・A′に対し1.3重量チのホウ酸を添加し1)H
をi5.7に調・整七で紡糸:原液を作成した。この紡
糸原液を水酸化ナト?リウムzoae7t,ボウ硝g’
o./Lで50Cのアルカリ性?の塩類?浴ヲ凝固浴と
し・て紡出し,以下実施例11と全ぐ同様にして繊鼾{
f:′製・造した3,得られた繊維の性能を表−・2・
に?示す。又,緯繊の4/7tlゲ1面け第7図に示す
通りであった。・又,このfJv!ifftを用いて作
成したセメン)・板の性能は表−2の通りであった。・
比較のため,凝固浴を以下の通り変えた他け実,1イl
i[21J2と同−条rトで繊維を製造し,以下実施例
2と同様に4載K4LIi支びセメント板の性能を測定
した。Project? Example 3, Comparative Example 4.5 PVA with an average degree of polymerization of 1300 was used at a concentration of 18:((', J
P' in the resulting rδ liquid.
Add 1.3 weight of boric acid to iV・A' and
was adjusted to i5.7 and spun at i5.7 to create a stock solution. Is this spinning stock solution sodium hydroxide? lium zoae7t, bow salt g'
o. /L 50C alkaline? Salts? The bath was spun as a coagulating bath, and the following was carried out in the same manner as in Example 11.
f:' Manufactured 3, the performance of the obtained fibers is shown in Table-・2・
To? show. In addition, the 4/7 tl game of the weft was as shown in Figure 7.・Also, this fJv! The performance of the cement board created using ifft is shown in Table 2.・For comparison, one sample was prepared with the coagulation bath changed as follows.
Fibers were produced using the same strips as 21J2, and the performance of the 4-mounted K4LIi support cement board was measured in the same manner as in Example 2.
その桔泌d表−2に示#”imりであった。ヌ.繊維の
横断面G寸第8.9図に示す辿りであった。The cross section G dimension of the fiber was as shown in Figure 8.9.
比較例4:ボウ硝350&/L,水酸化プl・リウム1
5y7t,温度50℃(第8図)
Lt較例5:水fa化f}’)ウム3Ei01/L.(
Fa[20℃実施例3で7ηられた!:’)!14f:
は比較例4.5の繊維K比べ性能(′.1ほとんど変ら
ないが,横断面は異形化され−Cいる。そのためかセメ
ント板の性能は実施例3の方が優f1ていた。Comparative example 4: 350 &/L of sulfur salt, 1 liter of prium hydroxide
5y7t, temperature 50°C (Fig. 8) Lt Comparative Example 5: Water FA f}') Um3Ei01/L. (
Fa [7η was reduced in Example 3 at 20°C! :')! 14f:
Compared to the fiber K of Comparative Example 4.5, the performance ('.1 is almost unchanged, but the cross section is irregularly shaped -C).Perhaps for this reason, the performance of the cement board of Example 3 was superior f1.
実施例4.比較例6〜9
子均重合度1680のI)VAを濃度が16.2’ii
’j.−敞係となるよう水に溶解し,得られた溶液にP
VAに”tt,1.3重量チのホウ酸を添加しl)Hを
5.7に調整してκJi糸原液を作成した。この紡糸原
液を水酸化ナトリウム170.9/t,ボウ硝120f
i/tで50℃のアルカリihLの塩禎浴−を,・疑固
浴として紡出し.以下実施(i’lJ1と全く回様jで
して繊維孕製造し,た。得られた繊K『の性能を表−3
に示す。又,繊維の横断面は第10図に示す通りであっ
た。又,この繊維を用いて作成したセメント板の性能に
表−3に示す通りであった。Example 4. Comparative Examples 6 to 9 I) VA with a molecular polymerization degree of 1680 was used at a concentration of 16.2'ii
'j. - P is dissolved in water so that it becomes a
A κJi yarn stock solution was prepared by adding 1.3 wt.
A salt bath of alkaline IHL at 50°C was spun at I/T as a pseudo-solid bath. Fiber production was carried out in the following manner (I'lJ1 and J).The performance of the obtained fiber K' is shown in Table 3.
Shown below. Further, the cross section of the fiber was as shown in FIG. Furthermore, the performance of the cement board made using this fiber was as shown in Table 3.
比較のため,比較例6,7については凝固浴を以下の通
り変えた他は実施例4と同一条件で,比較ft・り8.
91C−)いては紡糸原液にホウ酸を加えず.かつ凝固
浴及び熱延伸倍率を以下の通り変えた他は実施例4と同
−条件で繊維を製造l2,以下実施例4と同様に繊if
Kl々びセメント板の性能を測定しA−。その結果は氏
−3に示す通りで子)っフコ。又,峨維の{jl断而(
ζ1.¥NI1〜14図に示す通りであった。For comparison, Comparative Examples 6 and 7 were made under the same conditions as Example 4 except that the coagulation bath was changed as follows.
91C-), no boric acid was added to the spinning dope. Fibers were produced under the same conditions as in Example 4, except that the coagulation bath and hot drawing ratio were changed as follows.
Measuring the performance of Klubi cement board A-. The result is as shown in Mr.-3. Also, Awei's {jl discontinuation (
ζ1. It was as shown in ¥NI1-14 figures.
比較例6:ボウ硝350E/t,水酸化ナトリウム15
.9/l,温度50’C(第11図)
比較例7:水酸化ナトリウム350.97/=,温度2
0C.(第12図)
比較例8:ホウ酸無添加PVA原液(PH6’).飽和
ボウ硝浴.熱延伸28倍(第13図)
比較例9ニホウ酸無添加PVA原液(PH6).水酸化
ナトリウム350g/t,温度20℃.熱延伸倍率3.
3倍(?Jfj14図)
実施例4で得られた繊維は比較例6.7の繊維に比べ若
干高いヤング率を示している。又.繊維横断面は異形化
されている。セメント板の性能は朶施例4の方が優れ.
ていた。、
参考例1〜8・.
実施例1,7c得られた繊維をそれぞれ033重ft’
i%.0,5重量チ,..1重量チ,1.5重量チ,2
重i′チ.2.5重量チ,0.1重量チ,3重量.勇と
,バルブ3重量チ及びスペシャルクレイ1.OM量係を
含有し,残部が普通ボルトランドセ/ントから.,ナる
混合物より湿式抄造法にてセメント積層板全成形し,次
いで20℃.湿空中で28日間狡住し積層.板を得た。Comparative example 6: 350E/t of salt, sodium hydroxide 15
.. 9/l, temperature 50'C (Figure 11) Comparative example 7: Sodium hydroxide 350.97/=, temperature 2
0C. (Figure 12) Comparative Example 8: Boric acid-free PVA stock solution (PH6'). Saturated bow glass bath. Hot stretching 28 times (Figure 13) Comparative Example 9 PVA stock solution without diboric acid (PH6). Sodium hydroxide 350g/t, temperature 20℃. Hot stretching ratio 3.
3 times (?Jfj14 figure) The fiber obtained in Example 4 shows a slightly higher Young's modulus than the fiber in Comparative Example 6.7. or. The fiber cross section is deformed. The performance of the cement board was better in Example 4.
was. , Reference Examples 1 to 8. Examples 1 and 7c The obtained fibers were each 033 ft'
i%. 0.5 weight chi,. .. 1 weight chi, 1.5 weight chi, 2
heavy i'chi. 2.5 weight, 0.1 weight, 3 weight. Isamu, Valve 3 weight chi and special clay 1. Contains OM quantity, and the rest is from normal Bolland cent. , a cement laminate was completely formed using a wet paper-making method from the mixture, and then molded at 20°C. Laminated in a humid atmosphere for 28 days. Got the board.
得られた積層板について曲げ強度及びシャルビー@撃強
度を測定した。又,湿式抄造時の繊維の分散性を肉眼に
より観察し,良好(◎).良(○),やや不良(△)で
評価した。それらの結果を表−4に示す。The bending strength and Charby @ impact strength of the obtained laminate were measured. In addition, the dispersibility of fibers during wet papermaking was visually observed and was good (◎). Evaluation was made as good (◯) or slightly poor (△). The results are shown in Table 4.
スレート平板を基準にすると繊維の添加fkld0.3
〜2.5重量チが良く,とくに0.5〜2重量チが良好
であった。Based on slate plate, fiber addition fkld0.3
A weight of ~2.5 weight was good, and a weight of 0.5 to 2 weight was particularly good.
第1図は本発明の凝固浴条件を示すグラフである。第2
1凶.tif.a図,第7図及び第10図はそれぞれ実
施例1〜4で得られた繊維の横断面図を示し,第4図.
第5図,第6図,第8図,第9図,第11図,第12図
,第13図及び第14図はそれぞれ比較例1.〜9で得
られた繊維の横断回図を示す。
67一FIG. 1 is a graph showing the coagulation bath conditions of the present invention. Second
1 evil. tif. Figure a, Figure 7, and Figure 10 respectively show cross-sectional views of the fibers obtained in Examples 1 to 4, and Figure 4.
5, 6, 8, 9, 11, 12, 13, and 14 are Comparative Example 1, respectively. The cross-sectional diagram of the fiber obtained in ~9 is shown. 671
Claims (1)
系紡糸原液をカ性アルカリ濃度(xg/t)及び脱水性
塩類濃度(yg7t)が下記(a)−(b),(c)式
の条件を同時に満足する凝固浴中に紡出1./I1つい
で常法の中和.湿熱処理を行った後,水洗,乾燥し,ジ
’f−FC熱延伸を施すことを特徴とするポリビニルア
ルコール系合成繊維の製造法。 Y≦41.5−1.68X(a) Y≧850−5X(b) Y≧185−0.58X(e)(1) A polyvinyl alcohol-based spinning stock solution to which boric acid or copper salt has been added is prepared under conditions where the caustic alkali concentration (xg/t) and the dehydrating salt concentration (yg7t) are as shown in equations (a)-(b) and (c) below. Spinning into a coagulation bath that simultaneously satisfies 1. /I1 Next, neutralize the conventional method. A method for producing polyvinyl alcohol-based synthetic fibers, which comprises performing wet heat treatment, washing with water, drying, and subjecting to di'f-FC hot stretching. Y≦41.5-1.68X (a) Y≧850-5X (b) Y≧185-0.58X (e)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP14964082A JPS5943112A (en) | 1982-08-27 | 1982-08-27 | Manufacture of polyvinyl alcohol synthetic fiber |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP14964082A JPS5943112A (en) | 1982-08-27 | 1982-08-27 | Manufacture of polyvinyl alcohol synthetic fiber |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS5943112A true JPS5943112A (en) | 1984-03-10 |
Family
ID=15479641
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP14964082A Pending JPS5943112A (en) | 1982-08-27 | 1982-08-27 | Manufacture of polyvinyl alcohol synthetic fiber |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS5943112A (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS61160414A (en) * | 1985-01-08 | 1986-07-21 | Kuraray Co Ltd | Extremely thin yarn of high-strength polyvinyl alcohol type and production thereof |
CN100406621C (en) * | 2006-11-29 | 2008-07-30 | 浙江理工大学 | Process for preparing polytetrafluoroethylene fibre |
CN100422404C (en) * | 2006-07-27 | 2008-10-01 | 中国石化集团资产经营管理有限公司重庆天然气化工分公司 | Anti-wear polyvinyl alcohol aldehyde acetal fiber and its preparing method and use |
CN112226840A (en) * | 2020-08-04 | 2021-01-15 | 东华大学 | High-strength high-modulus PVA fiber and preparation method thereof |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS4912126A (en) * | 1972-05-15 | 1974-02-02 |
-
1982
- 1982-08-27 JP JP14964082A patent/JPS5943112A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS4912126A (en) * | 1972-05-15 | 1974-02-02 |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS61160414A (en) * | 1985-01-08 | 1986-07-21 | Kuraray Co Ltd | Extremely thin yarn of high-strength polyvinyl alcohol type and production thereof |
JPH0235044B2 (en) * | 1985-01-08 | 1990-08-08 | Kuraray Co | |
CN100422404C (en) * | 2006-07-27 | 2008-10-01 | 中国石化集团资产经营管理有限公司重庆天然气化工分公司 | Anti-wear polyvinyl alcohol aldehyde acetal fiber and its preparing method and use |
CN100406621C (en) * | 2006-11-29 | 2008-07-30 | 浙江理工大学 | Process for preparing polytetrafluoroethylene fibre |
CN112226840A (en) * | 2020-08-04 | 2021-01-15 | 东华大学 | High-strength high-modulus PVA fiber and preparation method thereof |
CN112226840B (en) * | 2020-08-04 | 2021-07-23 | 东华大学 | High-strength high-modulus PVA fiber and preparation method thereof |
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