JPS6297990A - Fluorescent colorant for raw liquid dyed viscose rayon - Google Patents
Fluorescent colorant for raw liquid dyed viscose rayonInfo
- Publication number
- JPS6297990A JPS6297990A JP61253627A JP25362786A JPS6297990A JP S6297990 A JPS6297990 A JP S6297990A JP 61253627 A JP61253627 A JP 61253627A JP 25362786 A JP25362786 A JP 25362786A JP S6297990 A JPS6297990 A JP S6297990A
- Authority
- JP
- Japan
- Prior art keywords
- viscose
- fluorescent
- rayon
- solution
- fine particles
- 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.)
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Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
(産業上の利用分野)
本発明はごスコースへの分散性や紡糸性に優れ、かつ良
好な光沢と鮮明な蛍光色調を有するレーヨン糸を与える
原液染ビスコースレーヨン用蛍光着色剤に関する。Detailed Description of the Invention (Industrial Field of Application) The present invention is a solution-dyed fluorescent material for solution-dyed viscose rayon that provides rayon yarn with excellent dispersibility in scose and spinnability, as well as good gloss and clear fluorescent color tone. Regarding colorants.
(従来の技術)
従来ビスコースレーヨンの製造法として、原液染と称す
る方法、即ちビスコース等の紡糸原液中に予め顔料、硫
化染料、建染染料等の着色剤を混合分散あるいは溶解し
てから紡糸して、着色レーヨン糸を製造する方法が広く
行なわれている。(Prior art) The conventional method for producing viscose rayon is a method called dope dyeing, in which coloring agents such as pigments, sulfur dyes, vat dyes, etc. are mixed and dispersed or dissolved in a spinning solution of viscose etc. in advance. A method of producing colored rayon yarn by spinning is widely used.
中でも、この場合の着色剤としては、水に不溶性の顔料
を用いることが多く、従って、紡糸性や得られるレーヨ
ン糸の光沢あるいは色調を向上させるため、紡糸原液中
に顔料を均一に分散させることが強く要求される。一方
、ビスコースレーヨンの紡糸に際しては、比較的高濃度
の硫酸や硫酸亜鉛、硫酸ソーダ等の塩を含んだ紡糸浴が
使用されており、紡糸時にこれら高酸高地の浴にビスコ
ースが接触する結果、ビスコース中に分散していた顔料
が凝集を起こして粗大粒子を形成し、糸切れの多発や場
合によっては吐出孔の閉塞という紡糸性の低下をまねく
ことが指摘されている。Among these, water-insoluble pigments are often used as colorants in this case, and therefore, in order to improve spinnability and the gloss or color tone of the resulting rayon yarn, it is necessary to uniformly disperse the pigment in the spinning stock solution. is strongly required. On the other hand, when spinning viscose rayon, a spinning bath containing relatively high concentrations of sulfuric acid, zinc sulfate, sodium sulfate, and other salts is used, and the viscose comes into contact with these highly acidic baths during spinning. As a result, it has been pointed out that the pigments dispersed in the viscose agglomerate to form coarse particles, leading to frequent thread breakage and, in some cases, a decrease in spinnability such as blockage of the discharge holes.
また、着色剤として硫化染料や建染染料等を使用する場
合、染料と回帰もしくはそれ以上の還元剤を加えて染料
を可溶化してからビスコースに添加するが、これら染料
の多くは溶解安定性に乏しく粗大粒子を形成する結果、
紡糸性の低下をまねくという欠点がある。In addition, when using sulfur dyes or vat dyes as colorants, the dye is solubilized by adding a reducing agent or more to the dye and then added to the viscose, but many of these dyes are stable in solution. As a result of forming coarse particles with poor properties,
This has the disadvantage of causing a decrease in spinnability.
(発明が解決しようとする問題点)
このように、原液染ビスコースレーヨン用の着色剤は、
苛酷な条件にも耐える分散・安定性が要求されるために
、市販されている顔料、染料の中でも、良好に使用でき
るものの数は少なく制限さ系
れている。特に、鮮明な蛍光色調のレーヨン会を得よう
として、蛍光染料、例えばローダミン系の塩基性染料や
酸性染料を使用しようとしても、ビスコース中への溶解
性が不充分で蛍光染料本来の鮮明な色調が得られなかっ
たり、高酸高塩の紡糸浴のために色調が変化するという
欠点がある。(Problems to be solved by the invention) In this way, the colorant for solution-dyed viscose rayon is
Since dispersion and stability that can withstand harsh conditions are required, the number of pigments and dyes that can be used satisfactorily among commercially available pigments and dyes is limited. In particular, even if fluorescent dyes such as rhodamine-based basic dyes or acidic dyes are used in an attempt to obtain a rayon dye with a clear fluorescent color, the solubility in viscose is insufficient and the original brightness of the fluorescent dye is lost. There are disadvantages in that the color tone cannot be obtained or the color tone changes due to the high acid and high salt spinning bath.
したがって、希望の色調の原液染ビスコースレーヨン用
の着色剤を得ることは非常に難しく、特に鮮明な蛍光色
調を有する原液染ビスコースレーヨン糸を与える着色剤
はいまだ得られていないのが実情である。Therefore, it is very difficult to obtain a coloring agent for solution-dyed viscose rayon yarn with a desired color tone, and the current situation is that a colorant that can produce solution-dyed viscose rayon yarn with a particularly vivid fluorescent tone has not yet been obtained. be.
本発明は、原液染ビスコースレーヨン用の着色剤に関す
る航記問題点を解消するものである。The present invention overcomes the navigational problems associated with colorants for solution-dyed viscose rayon.
従って、本発明の目的は、ビスコース中への分散性が良
好で高酸高塩の紡糸浴に耐え、良好な光沢と鮮明な蛍光
色調を有するレーヨン糸を与える原液染ごスコースレー
ヨン用蛍光着色剤を提供することにある。Therefore, it is an object of the present invention to develop a solution-dyed scone for rayon that provides rayon yarns that have good dispersibility in viscose, withstand high-acid, high-salt spinning baths, and have good gloss and bright fluorescent color tones. The purpose is to provide a coloring agent.
(問題点を解決するための手段および作用)本発明は、
蛍光染料を0.2〜4重量%含有し平均粒子径が0.1
〜10ミクDンであるアミノ樹脂の硬化球状微粒子より
なる原液染ビスコースレーヨン用蛍光着色剤に関する。(Means and effects for solving the problems) The present invention has the following features:
Contains 0.2 to 4% by weight of fluorescent dye and has an average particle size of 0.1
This invention relates to a fluorescent colorant for solution-dyed viscose rayon made of hardened spherical fine particles of amino resin having a particle size of ~10 mic D.
アミノ樹脂とは、メラミン、尿素、ベンゾグアナミン、
アセトグアナミン等のアミノ基を含む化合物とホルムア
ルデヒドに代表されるアルデヒド類との綜合反応によっ
て得られる樹脂の総称であり、いずれの組合わせのもの
であっても、本発明に用いることができる。中でも、後
述する如き蛍光染料の発色性を考慮すれば、ベンゾグア
ナミン−ホルムアルデヒド樹脂またはベンゾグアナミン
・メラミン−ホルムアルデヒド樹脂が好ましい。Amino resins include melamine, urea, benzoguanamine,
It is a general term for resins obtained by a synthetic reaction between a compound containing an amino group such as acetoguanamine and an aldehyde represented by formaldehyde, and any combination can be used in the present invention. Among these, benzoguanamine-formaldehyde resin or benzoguanamine-melamine-formaldehyde resin is preferable in consideration of the coloring properties of fluorescent dyes as described below.
これらベンゾグアナミンを必須成分とするアミノ樹脂は
蛍光染料によって均一に着色され、蛍光染料本来の鮮明
な色調を発色性良く発現することができる。These amino resins containing benzoguanamine as an essential component are uniformly colored with fluorescent dyes, and can express the vivid color tones inherent to fluorescent dyes with good color development.
本発明においては、アミノ樹脂は蛍光染料を0.2〜4
ffiffi%含有することにより着色されていること
が必須であり、種々の蛍光染料の中から希望する色調の
ものを選択して使用することができる。使用する蛍光染
料としては、着色されたアミノ樹脂に蛍光染料本来の鮮
明な色調が発色性良く発現できるものであれば、特に制
限はなく、例えばローダミン系やチオフラビン系の塩基
性染料、フルオレセイン・エオシン系の酸性染料、ジア
ミノスチルベン系の蛍光増白剤や油溶性蛍光染料などを
挙げることができ、目的とする色調や堅牢特性に応じ適
当に選んで使用することができる。In the present invention, the amino resin contains 0.2 to 4 fluorescent dyes.
It is essential that the dye be colored by containing ffiffi%, and a desired color tone can be selected from various fluorescent dyes and used. The fluorescent dye to be used is not particularly limited as long as it can express the vivid color tone inherent to the fluorescent dye on the colored amino resin with good color development, such as basic dyes such as rhodamine and thioflavin, fluorescein and eosin. Examples include acid dyes based on diaminostilbene, fluorescent whitening agents based on diaminostilbene, and oil-soluble fluorescent dyes, which can be appropriately selected and used depending on the desired color tone and fastness characteristics.
アミノ樹脂を着色するために使用される蛍光染料の吊は
、アミノ樹脂に対して0.2〜4重量%の範囲、より好
ましくは0.5〜3重量%の範囲である。0.2重量%
未満の俊足では、アミノ樹脂の着色が不十分であり、着
色剤のビスコースへの添加に際し多量の添加を必要とし
、着色剤の均一分散が得られにくくなる。また、4重量
%を越える多量では、蛍光染料で着色する際に独特の濃
度消光現象が発現するために、蛍光染料本来の鮮明な蛍
光色調を有する着色剤が得られなくなる。逆に、アミノ
樹脂中に含有される多量の蛍光染料のために、アミノ樹
脂の硬化球状微粒子を製造づる過程で10ミクロンを越
える粗大粒子が生成しやすくなる。The amount of fluorescent dye used to color the amino resin ranges from 0.2 to 4% by weight, more preferably from 0.5 to 3% by weight, based on the amino resin. 0.2% by weight
If the amount is less than 1, the coloring of the amino resin will be insufficient, and a large amount of colorant will need to be added to viscose, making it difficult to obtain uniform dispersion of the colorant. Furthermore, if the amount exceeds 4% by weight, a unique concentration quenching phenomenon occurs when coloring with the fluorescent dye, making it impossible to obtain a coloring agent having the clear fluorescent color tone inherent to the fluorescent dye. On the other hand, due to the large amount of fluorescent dye contained in the amino resin, coarse particles exceeding 10 microns are likely to be produced in the process of producing cured spherical fine particles of the amino resin.
本発明の原液染ビスコースレーヨン用蛍光着色剤として
用いられる蛍光染料で着色されたアミノ樹脂の硬化球状
微粒子(以下、着色樹脂硬化球状微粒子という。)は、
形状が球形で微粒子表面に突起がなく、粒子径がぼり均
一にそろっているものであり、二次凝集がおこりにくく
、ビスコースとの親和性も高いため、ビスコース中への
分散性が優れている。また、着色樹脂硬化球状微粒子は
不溶不融の樹脂からなるため、耐熱性、耐溶剤性、耐酸
性、耐アルカリ性、耐色移行性に優れており、高酸高温
の紡糸浴や、高温の操作を含むビスコースレーヨン製造
工程に充分耐え得るものである。The cured spherical fine particles of amino resin colored with a fluorescent dye (hereinafter referred to as colored resin cured spherical fine particles) used as the fluorescent colorant for solution-dyed viscose rayon of the present invention are:
It has a spherical shape with no protrusions on the particle surface, and the particle size is large and uniform. Secondary aggregation is difficult to occur and it has a high affinity with viscose, so it has excellent dispersibility in viscose. ing. In addition, because colored resin cured spherical fine particles are made of insoluble and infusible resin, they have excellent heat resistance, solvent resistance, acid resistance, alkali resistance, and color migration resistance, and can be used in high-acid, high-temperature spinning baths, and in high-temperature operations. It can fully withstand viscose rayon manufacturing processes including.
上記の如き優れた特性を有する着色樹脂硬化球状微粒子
は、公知の製造方法により得られるものを用いることが
できる。このような製造方法としては、例えば特公昭5
2−27679、特公昭58−5924、特公昭59−
48007、特公昭58−24444に開示の方法を挙
げることができる。これらに開示されている方法に基け
ば、耐熱性、耐溶剤性、耐酸性、耐アルカリ性、耐色移
行性に優れ、球形で粒子径かほず均一であり、且つ任意
の粒子径の着色樹脂硬化球状微粒子が得られる。The colored resin-cured spherical fine particles having the above-mentioned excellent properties can be obtained by a known manufacturing method. As such a manufacturing method, for example,
2-27679, Special Publication No. 58-5924, Special Publication No. 59-
48007, and the method disclosed in Japanese Patent Publication No. 58-24444. Based on the methods disclosed in these documents, colored resins with excellent heat resistance, solvent resistance, acid resistance, alkali resistance, and color migration resistance, spherical shape and fairly uniform particle size, and arbitrary particle size can be produced. Hardened spherical fine particles are obtained.
本発明に用いられる着色樹脂硬化球状微粒子の平均粒子
径は、単糸5デニールのレーヨン糸を紡糸する場合、ビ
スコース吐出孔が80ミクロン程度であることやビスコ
ースへの分散性を考慮すれば、0.1〜10ミクロン、
より好ましくは0.1〜2ミクロンの範囲である。前記
した着色樹脂硬化球状微粒子の公知の製造方法によれば
、0.1〜10ミクロンの平均粒子径のものを容易に得
ることができるが、適宜製造条件を選択して、より好ま
しい平均粒子径範囲のものを得ることも可能である。The average particle diameter of the colored resin cured spherical fine particles used in the present invention is determined by considering that when spinning a single 5-denier rayon yarn, the viscose discharge hole is approximately 80 microns and the dispersibility in viscose is determined. , 0.1-10 microns,
More preferably, it is in the range of 0.1 to 2 microns. According to the known manufacturing method of the colored resin-cured spherical fine particles described above, particles with an average particle size of 0.1 to 10 microns can be easily obtained, but by appropriately selecting manufacturing conditions, a more preferable average particle size can be obtained. It is also possible to obtain a range.
着色樹脂硬化球状微粒子は、本発明の原液染ビスコース
レーヨン用蛍光着色剤として、ビスコースあるいはアル
カリセルロースに添加、混合して使用される。混合に際
しては、特殊な混合・混線装置は必要なく、極めて簡易
な混合装2で充分である。また、本発明の着色剤の対象
となるビスコースやビスコースを紡糸する際の紡糸浴の
組成についても特に制限はない。The colored resin cured spherical fine particles are used as a fluorescent colorant for solution-dyed viscose rayon of the present invention by being added to and mixed with viscose or alkali cellulose. For mixing, no special mixing/crossing device is required, and an extremely simple mixing device 2 is sufficient. Furthermore, there are no particular limitations on the composition of viscose to be used as the colorant of the present invention or the spinning bath used when spinning viscose.
本発明の原液染ビスコースレーヨン用蛍光着色剤の添加
量は、ビスコース100重重部に対して0、1〜10重
量部、好ましくは0.3〜3重量部である。また、本発
明の着色剤をビスコースに添加使用するに際し、他の顔
料や染料などの着色剤や着色剤の分散を助けるための界
面活性剤を併用することもできる。The amount of the fluorescent colorant for solution-dyed viscose rayon of the present invention added is 0.1 to 10 parts by weight, preferably 0.3 to 3 parts by weight, per 100 parts by weight of viscose. Furthermore, when the colorant of the present invention is added to viscose, other colorants such as pigments and dyes, and surfactants for aiding the dispersion of the colorant can also be used together.
(発明の効果)
本発明の原液染ビスコースレーヨン用蛍光着色剤は、粒
子径がほぼ均一で、ビスコースと親和性が高くしかも不
溶不融のアミノ樹脂の硬化球状微粒子からなるため、ご
スコ〜スへの分散性や紡糸性に優れており、特に単糸5
デニール以下の絹物を紡糸する時でも、糸切れなく安定
に紡糸することができる。(Effects of the Invention) The fluorescent colorant for solution-dyed viscose rayon of the present invention is composed of hardened spherical fine particles of an insoluble and infusible amino resin with a substantially uniform particle size and a high affinity for viscose. It has excellent dispersibility in ~ and spinnability, especially for single yarn 5.
Even when spinning silk of denier or less, it can be stably spun without thread breakage.
また、種々の蛍光染料の中から希望する色調のものを選
択してアミノ樹脂を着色し、本発明の着色剤とすること
ができるため、従来の原液染ビスコースレーヨン用着色
剤では得られない鮮明な蛍光色調を有するレーヨン糸あ
るいはレーヨンステーブルが容易に得られるという効果
もある。In addition, it is possible to select a desired color from among various fluorescent dyes to color the amino resin and use it as the colorant of the present invention, which cannot be obtained with conventional colorants for solution-dyed viscose rayon. Another advantage is that rayon yarn or rayon stable having a clear fluorescent color tone can be easily obtained.
更に、本発明の原液染ビスコースレーヨン用蛍光着色剤
を使用すると、レーヨン糸中のアミノ樹脂の硬化球状微
粒子の光散乱によって、ビスコースレーヨン独特の強烈
な光沢が弱められ、非常に好ましいソフトな光沢を有す
る美麗なレーヨン糸を得ることができる。Furthermore, when the fluorescent colorant for solution-dyed viscose rayon of the present invention is used, the intense luster unique to viscose rayon is weakened by the light scattering of the hardened spherical fine particles of the amino resin in the rayon thread, resulting in a very desirable soft color. A beautiful rayon yarn with luster can be obtained.
以下、実施例により本発明を説明するが、この実施例に
より本発明の範囲が何ら制限を受けるものではない。The present invention will be explained below with reference to Examples, but the scope of the present invention is not limited in any way by these Examples.
参考例 1
撹拌機、還流冷却器、温度計を備えた四つ目フラスコに
ベンゾグアナミン240g(1,3モル)、メラミン6
0Q(0,5モル)、濃度37%のホルマリン323.
4c+(4,0モル)および濃度10%の炭酸ナトリウ
ム水溶液1.30 Gを仕込み、撹拌しながら94〜9
5℃の温度で5時間反応させた。Reference Example 1 240 g (1.3 mol) of benzoguanamine and melamine 6 were placed in a four-eye flask equipped with a stirrer, reflux condenser, and thermometer.
0Q (0.5 mol), formalin 323. with a concentration of 37%.
4c+ (4.0 mol) and 1.30 G of a 10% concentration sodium carbonate aqueous solution, and while stirring, 94-9
The reaction was carried out at a temperature of 5° C. for 5 hours.
反応生成物は、疎水性となり、白濁した。The reaction product became hydrophobic and cloudy.
ポリビニルアルコール(■クラレ製品・PVA205)
42.0gを水521.OQに溶解して得た水溶液に、
ホモミキサーで激しく撹拌しながら上記の反応生成物を
含む溶液を加え乳化させた。乳化物を30℃まで冷却し
た後、ローダミンB1.5qとローダミン6GCP1.
5gを加えて15分間撹拌し、ついでドデシルベンゼン
スルホン酸4.620を加え、40℃、50℃、70℃
、90℃の各温度で順次2時間ずつ加熱撹拌し、乳化状
態で重合硬化させた。Polyvinyl alcohol (Kuraray products/PVA205)
42.0g to 521.0g of water. In the aqueous solution obtained by dissolving in OQ,
While vigorously stirring with a homomixer, the solution containing the above reaction product was added and emulsified. After cooling the emulsion to 30°C, rhodamine B1.5q and rhodamine 6GCP1.
5g was added and stirred for 15 minutes, then 4.620% of dodecylbenzenesulfonic acid was added, and the mixture was heated at 40°C, 50°C, and 70°C.
, and 90° C. for 2 hours at a time to polymerize and harden the emulsified state.
重合硬化後の乳化物を炉別して得たフィルターケーキを
100℃で乾燥し、150℃で3時間加熱処理した後、
粉砕して、着色されたベンゾグアナミン・メラミン−ホ
ルムアルデヒド樹脂の硬化球状微粒子392gを得た。After drying the filter cake obtained by furnace-separating the emulsion after polymerization and hardening at 100°C, and heat-treating it at 150°C for 3 hours,
The mixture was crushed to obtain 392 g of hardened spherical fine particles of colored benzoguanamine-melamine-formaldehyde resin.
このようにして得た球状微粒子は平均粒子径0.5ミク
ロンのピンクの蛍光色を持つ樹脂硬化物からなり、軟化
点は300℃以上であった。The thus obtained spherical fine particles were composed of a cured resin having an average particle diameter of 0.5 microns and a pink fluorescent color, and had a softening point of 300° C. or higher.
参考例 2
参考例1で使用したのと同じフラスコにベンゾグアナミ
ン15C1(0,8モル)、濃度37%のホルマリン1
62a(2,0モル)および濃度10%の炭酸ナトリウ
ム水溶液0.650を仕込み、撹拌しながら94〜95
℃の温度で4時間反応させた。その後、蛍光増白剤のL
JVITEX’OB(チバ・ガイギー社M)1.5qを
加え、94〜95℃に保ち60分間撹拌し、反応生成物
を着色した。Reference Example 2 In the same flask as used in Reference Example 1, benzoguanamine 15C1 (0.8 mol) and formalin 1 with a concentration of 37% were added.
62a (2.0 mol) and 0.650 aqueous sodium carbonate solution with a concentration of 10%, and while stirring,
The reaction was carried out for 4 hours at a temperature of .degree. After that, L of optical brightener
1.5 q of JVITEX'OB (Ciba Geigy M) was added, and the mixture was stirred for 60 minutes while being maintained at 94 to 95°C, thereby coloring the reaction product.
ポリビニルアルコール(■クラレ製品・PVA205)
10.5qを水145gに溶解して得た水溶液に、ホモ
ミキサーを用いて激しく撹拌しながら上記の反応生成物
を含む溶液を加え乳化させた後、ドデシルベンゼンスル
ホンM2.1clを加え、50℃、70℃、80℃、9
0℃の各温度で順次2時間ずつ加熱撹拌し、乳化状態で
重合硬化させた。Polyvinyl alcohol (Kuraray products/PVA205)
To an aqueous solution obtained by dissolving 10.5q in 145 g of water, a solution containing the above reaction product was added and emulsified while vigorously stirring using a homomixer, and then 2.1 cl of dodecylbenzenesulfone M was added and the mixture was heated at 50°C. , 70℃, 80℃, 9
The mixture was heated and stirred for 2 hours at each temperature of 0° C. to polymerize and harden the emulsified state.
重合硬化後の乳化物をン戸別して得たフィルターケーキ
を参考例1と同様に乾燥、加熱処理、粉砕して、着色さ
れたベンゾグアナミン−ホルムアルデヒド樹脂の硬化球
状微粒子1800@得た。The filter cake obtained by separating the emulsion after polymerization and hardening was dried, heat treated, and crushed in the same manner as in Reference Example 1 to obtain 1800 hardened spherical fine particles of colored benzoguanamine-formaldehyde resin.
このようにして得た球状微粒子は平均粒子径0、5ミク
ロンの白皮の高い樹脂硬化物からなり、軟化点は300
℃以上であった。The spherical fine particles obtained in this way are made of a hardened resin with a high white skin of an average particle size of 0.5 microns, and have a softening point of 300.
It was above ℃.
参考例 3
参考例1において使用した蛍光染料の量をローダミンB
10.5 gおよびローダミン6 G CP 10゜
5gとした以外は、参考例1と全く同様にして、着色さ
れたベンゾグアナミン・メラミン−ホルムアルデヒド樹
脂の硬化球状微粒子410Qを得た。Reference Example 3 The amount of fluorescent dye used in Reference Example 1 was changed to Rhodamine B.
Colored cured spherical fine particles 410Q of benzoguanamine-melamine-formaldehyde resin were obtained in exactly the same manner as in Reference Example 1, except that 10.5 g of Rhodamine 6 G CP and 10.5 g of Rhodamine 6 G CP were used.
このようにして得た球状微粒子は平均粒子径0、8ミク
ロンの蛍光のほとんどない黒赤色の樹脂硬化物からなり
、軟化点は300℃以上であった。The thus obtained spherical fine particles were composed of a black-red resin cured product with an average particle diameter of 0.8 microns and almost no fluorescence, and had a softening point of 300° C. or higher.
実施例 1
ビスコース組成がセルロース8.5重量%、全アルカリ
6.0重j%、ホラテンロート価11.8のビスコース
100重8部に、参考例1で得た着色されたベンゾグア
ナミン・メラミン−ホルムアルデヒド樹脂の硬化球状微
粒子1重合部を添加しよく混合して、着色ビスコース組
成物を調製した。この組成物を用いて、組成が硫M15
0q/i硫酸ソーダ345 Q/Jl 、硫酸亜鉛15
0/j!で温度60℃の紡糸浴中へ紡糸速度90m/分
、浸漬長60αで紡糸し、50デニール/20フイラメ
ントのレーヨン糸を得た。得られたレーヨン糸は、ソフ
トな好ましい光沢があり、ピンクの蛍光色の鮮明な美麗
な糸であった。また紡糸中、糸切れやビスコース吐出口
の閉塞というトラブルの発生は皆無であった。Example 1 The colored benzoguanamine/melamine obtained in Reference Example 1 was added to 100 parts by weight of viscose whose composition was 8.5% by weight of cellulose, 6.0% by weight of total alkali, and 11.8% by weight of viscose. One polymerized part of cured spherical fine particles of formaldehyde resin was added and mixed thoroughly to prepare a colored viscose composition. Using this composition, the composition is sulfur M15.
0q/i Sodium Sulfate 345 Q/Jl, Zinc Sulfate 15
0/j! The fibers were spun into a spinning bath at a temperature of 60° C. at a spinning speed of 90 m/min and a dipping length of 60 α to obtain a rayon yarn of 50 denier/20 filaments. The obtained rayon yarn was a beautiful yarn with a soft and desirable luster and a bright pink fluorescent color. Furthermore, during spinning, there were no problems such as yarn breakage or clogging of the viscose discharge port.
実施例 2
実施例1で用いたのと同様のごスコース100重最部に
参考例2で得た着色されたベンゾグアナミン−ホルムア
ルデヒド樹脂の硬化球状微粒子1重量部を添加しよく混
合して、着色ビスコース組成物を調製した。この組成物
を用いて、組成が硫W1100g/l、硫酸ソーダ35
0g/j!、硫酸亜鉛20 CJ/1で温度40℃の第
1凝固浴中に紡糸した。Example 2 1 part by weight of cured spherical fine particles of colored benzoguanamine-formaldehyde resin obtained in Reference Example 2 was added to the 100-weight part of the same scose used in Example 1, and mixed well to form a colored biscoat. A course composition was prepared. Using this composition, the composition was 1100 g/l of sulfur W and 35 g/l of sodium sulfate.
0g/j! , zinc sulfate 20 CJ/1 in a first coagulation bath at a temperature of 40°C.
続いて硫酸10g/j!よりなる湿度90℃の第2浴中
に導き延伸をかけながら再生を完了した。Next, sulfuric acid 10g/j! The regeneration was completed while the film was introduced into a second bath with a humidity of 90° C. and stretched.
得られたレーヨン糸を50順に切断後、乾燥して、レー
ヨン・ステーブルを得た。The obtained rayon yarn was cut into 50 pieces and dried to obtain a rayon stable.
得られたレーヨン・ステーブルは5デニールの非常に白
皮の高いものであった。また、紡糸中、糸切れやごスコ
ース吐出口の閉塞というトラブルの発生は皆無であった
。The resulting rayon stable had a very white skin of 5 denier. Furthermore, during spinning, there were no problems such as yarn breakage or blockage of the scose discharge port.
比較例 1
実施例1で用いたのと同様のビスコース100tfif
fi部に、参考例3で得た着色されたベンゾグアナミン
・メラミン−ホルムアルデヒド樹脂の硬化球状微粒子1
重量部を添加しよく混合して、比較用の着色どスコース
組成物を調製した。この比較用の組成物を用いて、実施
例1と同様にして紡糸し、50デニール/20フイラメ
ントのレーヨン糸を得た。Comparative Example 1 Viscose 100tfif similar to that used in Example 1
In part fi, hardened spherical fine particles 1 of colored benzoguanamine-melamine-formaldehyde resin obtained in Reference Example 3 are added.
A colored scose composition for comparison was prepared by adding parts by weight and mixing well. Using this comparative composition, spinning was carried out in the same manner as in Example 1 to obtain a 50 denier/20 filament rayon yarn.
得られたレーヨン糸は、ピンクの蛍光色のほとんどない
鮮明さに欠けたものであった。また、レーヨン糸中のと
ころどころに赤色の粗大粒子が混入していることが顕微
鏡観察で認められた。The obtained rayon yarn lacked sharpness with almost no pink fluorescent color. Furthermore, microscopic observation revealed that red coarse particles were mixed in some places in the rayon yarn.
Claims (1)
.1〜10ミクロンであるアミノ樹脂の硬化球状微粒子
よりなる原液染ビスコースレーヨン用蛍光着色剤。 2、アミノ樹脂がベンゾグアナミン−ホルムアルデヒド
樹脂またはベンゾグアナミン・メラミン−ホルムアルデ
ヒド樹脂である特許請求の範囲第1項記載の原液染ビス
コースレーヨン用蛍光着色剤。[Claims] 1. Contains 0.2 to 4% by weight of fluorescent dye and has an average particle size of 0.
.. A fluorescent colorant for solution-dyed viscose rayon consisting of hardened spherical fine particles of amino resin having a size of 1 to 10 microns. 2. The fluorescent colorant for solution-dyed viscose rayon according to claim 1, wherein the amino resin is benzoguanamine-formaldehyde resin or benzoguanamine-melamine-formaldehyde resin.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP61253627A JPS6297990A (en) | 1986-10-27 | 1986-10-27 | Fluorescent colorant for raw liquid dyed viscose rayon |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP61253627A JPS6297990A (en) | 1986-10-27 | 1986-10-27 | Fluorescent colorant for raw liquid dyed viscose rayon |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS6297990A true JPS6297990A (en) | 1987-05-07 |
Family
ID=17253974
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP61253627A Pending JPS6297990A (en) | 1986-10-27 | 1986-10-27 | Fluorescent colorant for raw liquid dyed viscose rayon |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS6297990A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101974797A (en) * | 2010-10-02 | 2011-02-16 | 山东海龙股份有限公司 | Method for preparing totally chlorine-free high-whiteness cellulose fiber |
JP2013537588A (en) * | 2010-07-27 | 2013-10-03 | レンツィング アクチェンゲゼルシャフト | Fluorescent fibers and their use |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3458271A (en) * | 1966-12-22 | 1969-07-29 | Asahi Chemical Ind | Simultaneous aminoplast impregnation and direct dyeing by the pad dwell process followed by hot curing of the aminoplast |
JPS498835A (en) * | 1972-05-22 | 1974-01-25 | ||
JPS50105743A (en) * | 1973-11-23 | 1975-08-20 | ||
JPS5227197A (en) * | 1975-08-28 | 1977-03-01 | Nippon Hakuyo Kiki Kaihatsu Kyokai | Device for automatically operating underwater walking machine |
JPS5227679A (en) * | 1975-08-27 | 1977-03-02 | Audio Technica Corp | Horizontal force detecting device |
JPS61160411A (en) * | 1984-12-27 | 1986-07-21 | Kuraray Co Ltd | Production of colored yarn of wet spinning |
JPS6241310A (en) * | 1985-08-14 | 1987-02-23 | Kohjin Co Ltd | Rayon fiber having excellent light fastness |
-
1986
- 1986-10-27 JP JP61253627A patent/JPS6297990A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3458271A (en) * | 1966-12-22 | 1969-07-29 | Asahi Chemical Ind | Simultaneous aminoplast impregnation and direct dyeing by the pad dwell process followed by hot curing of the aminoplast |
JPS498835A (en) * | 1972-05-22 | 1974-01-25 | ||
JPS50105743A (en) * | 1973-11-23 | 1975-08-20 | ||
JPS5227679A (en) * | 1975-08-27 | 1977-03-02 | Audio Technica Corp | Horizontal force detecting device |
JPS5227197A (en) * | 1975-08-28 | 1977-03-01 | Nippon Hakuyo Kiki Kaihatsu Kyokai | Device for automatically operating underwater walking machine |
JPS61160411A (en) * | 1984-12-27 | 1986-07-21 | Kuraray Co Ltd | Production of colored yarn of wet spinning |
JPS6241310A (en) * | 1985-08-14 | 1987-02-23 | Kohjin Co Ltd | Rayon fiber having excellent light fastness |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2013537588A (en) * | 2010-07-27 | 2013-10-03 | レンツィング アクチェンゲゼルシャフト | Fluorescent fibers and their use |
CN101974797A (en) * | 2010-10-02 | 2011-02-16 | 山东海龙股份有限公司 | Method for preparing totally chlorine-free high-whiteness cellulose fiber |
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