JPH032363B2 - - Google Patents

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Publication number
JPH032363B2
JPH032363B2 JP10534283A JP10534283A JPH032363B2 JP H032363 B2 JPH032363 B2 JP H032363B2 JP 10534283 A JP10534283 A JP 10534283A JP 10534283 A JP10534283 A JP 10534283A JP H032363 B2 JPH032363 B2 JP H032363B2
Authority
JP
Japan
Prior art keywords
coagulating
coagulation
nozzle
latex
thin tube
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.)
Expired
Application number
JP10534283A
Other languages
Japanese (ja)
Other versions
JPS59230004A (en
Inventor
Teruhiko Sugimori
Takayuki Tajiri
Akio Hironaka
Hideaki Habara
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsubishi Chemical Corp
Original Assignee
Mitsubishi Rayon Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Mitsubishi Rayon Co Ltd filed Critical Mitsubishi Rayon Co Ltd
Priority to JP10534283A priority Critical patent/JPS59230004A/en
Publication of JPS59230004A publication Critical patent/JPS59230004A/en
Publication of JPH032363B2 publication Critical patent/JPH032363B2/ja
Granted legal-status Critical Current

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Description

【発明の詳細な説明】 本発明は重合体ラテツクスの凝固方法に関する
ものである。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for coagulating polymer latexes.

化学工業においては凝固性物質、例えば重合体
ラテツクス、ゴムラテツクス等は多量に扱われて
おり、その内一部は接着剤や塗料等として液状の
まま使用されているが、大部分のものは凝固剤に
より凝固した後使用されているのが現状である。
従つて凝固操作はこれらの分野では重要な位置を
占める操作であるにもかかわらず現状では凝固の
方法あるいは凝固装置は従来からの経験により得
られた古い技術に基くものが使用されている。
In the chemical industry, large amounts of coagulable substances such as polymer latex and rubber latex are handled, and some of them are used in liquid form as adhesives and paints, but most of them are used as coagulants. Currently, it is used after being solidified.
Therefore, although the coagulation operation is an important operation in these fields, currently the coagulation methods and coagulation apparatuses are based on old techniques obtained through conventional experience.

ところで樹脂工業に限つて述べるならば、乳化
重合法により製造された重合体ラテツクスから重
合体粉末を製造する場合、一般にはラテツクスと
酸類あるいは無機質の多価塩類からなる凝固剤と
を接触せしめ凝析した後、熱処理等の方法により
重合体を固化せしめ、しかる後に脱水、乾燥等の
操作を経て重合体の乾燥粉末とするのが通常であ
る。しかるに通常採用されている方法によれば得
られる粉末の粒子は不定形をしており、粒度分布
も広く、粗大粒子が含まれる反面微粉末も相当の
量存在する。従つて前記微粉末の飛散に基づく歩
留りの低下、あるいは環境問題、さらには粉末の
低流動性に基づく配管、貯槽出口等での詰り、粉
塵発生による作業環境の悪化、粉塵爆発の危険性
の増大等好ましからざる問題を有している。また
重合体粉末の嵩比重が小さく脱水機における脱水
性が悪いため輸送、貯蔵のコストが高く、しかも
乾燥工程で多大の熱エネルギーを消費しているの
が現状である。
By the way, speaking specifically in the resin industry, when producing polymer powder from polymer latex produced by emulsion polymerization, it is generally coagulated by bringing the latex into contact with a coagulant consisting of acids or inorganic polyvalent salts. After that, the polymer is usually solidified by a method such as heat treatment, and then subjected to operations such as dehydration and drying to form a dry powder of the polymer. However, according to the commonly used method, the powder particles obtained have an irregular shape, have a wide particle size distribution, and contain coarse particles but also a considerable amount of fine powder. Therefore, there is a reduction in yield due to the scattering of the fine powder, or environmental problems, and furthermore, clogging at piping, storage tank outlet, etc. due to the low fluidity of the powder, deterioration of the working environment due to dust generation, and increased risk of dust explosion. It has some undesirable problems. In addition, the bulk specific gravity of the polymer powder is small and dehydration properties in a dehydrator are poor, so transportation and storage costs are high, and moreover, a large amount of thermal energy is consumed in the drying process.

ところで、近年凝固操作の重要性に鑑み重合体
粉体の粉体特性を向上しようとする研究が多く見
られ。これらの研究開発の動向の一つとして従来
の凝固方法あるいは凝固装置の若干の改善、他の
ものとして気相反応を利用した噴霧乾燥や気相凝
固等の方法がある。しかしながらかかる方法は依
然として粉体として低品位なものであつたり、多
大なエネルギーコストと建設コストを強いるもの
であつたりするなど決定的な改善策とはなつてい
ない。
Incidentally, in view of the importance of coagulation operations in recent years, many studies have been conducted to improve the powder properties of polymer powders. One of these trends in research and development is the slight improvement of conventional coagulation methods or coagulation equipment, and other methods include methods such as spray drying and vapor phase coagulation that utilize gas phase reactions. However, such methods still produce low-grade powders, impose large energy costs and construction costs, and have not yet become a definitive solution.

このような状況下において、本発明者らは特定
の条件を満す細管より乳化ラテツクスを凝固液中
に吐出させることにより微粉および粗大粒子を実
質的に含まない高嵩比重粉粒体とし得る発明につ
いて、先に特願昭56−73115号(特開昭57−
187322号)として特許出願した。
Under these circumstances, the present inventors have developed an invention in which a high bulk specific gravity powder or granule substantially free of fine powder and coarse particles can be obtained by discharging emulsified latex into a coagulating liquid from a capillary that satisfies specific conditions. Regarding this, we first filed Japanese Patent Application No. 73115 (1983)
A patent application was filed as (No. 187322).

本発明者らは先の発明に基づき、さらに鋭意検
討した結果、ラテツクス凝固用ノズルとして特定
の構造を有するものを重合体ラテツクスの凝固に
使用することにより粉体特性に極めて優れる重合
体粉粒体とし得ることを見出し本発明に到達し
た。
Based on the previous invention, the inventors of the present invention have conducted extensive studies and found that by using a nozzle with a specific structure as a latex coagulating nozzle for coagulating polymer latex, polymer powder particles with extremely excellent powder properties can be produced. The inventors have discovered that this can be done, and have arrived at the present invention.

本発明は重合体ラテツクスを凝固する際に、ラ
テツクス凝固用ノズルとして基板に設けられた細
管より該ラテツクスの吐出が可能であり、かつ細
管の周囲より凝固液の吐出が可能である構造のも
のを使用することを特徴とする重合体ラテツクス
の凝固方法である。
The present invention uses a latex coagulating nozzle that is capable of discharging the latex from a thin tube provided on a substrate when coagulating a polymer latex, and that also allows the coagulation liquid to be discharged from around the thin tube. A method for coagulating a polymer latex, characterized in that it is used.

本発明において使用するラテツクス凝固用ノズ
ルの一例の構造を図面に基づいて説明する。図面
は本発明において使用するラテツクス凝固用ノズ
ルの一例の断面斜視図であり、図面中1は細管、
2は基板、3はホルダー、4はガスケト、5は締
結具、6は凝固液供給器、7は凝固液導入管、8
は凝固液吐出口である。本ノズルにおいて細管と
基板は直接あるいは接着剤等によつて固着してい
る必要があり、両者間に凝固性物質が漏出する間
隙が存在してはならない。また基板とホルダーを
つなぐガスケツトの部位は完全に密着し凝固性物
質が外部へ漏出しないようにすべきである。同様
に基板と凝固液供給器の結合部位も密着しており
凝固液が外部へ漏出しないようにすべきである。
また凝固液供給器と凝固液導入管は通常の方法、
例えば熔接、接着、ねじ込み等で固着されるか、
あるいは一体物であれば取扱上好ましいものであ
る。
The structure of an example of a nozzle for coagulating latex used in the present invention will be explained based on the drawings. The drawing is a cross-sectional perspective view of an example of a latex coagulating nozzle used in the present invention, and in the drawing 1 is a thin tube;
2 is a substrate, 3 is a holder, 4 is a gasket, 5 is a fastener, 6 is a coagulation liquid supply device, 7 is a coagulation liquid introduction pipe, 8
is a coagulation liquid discharge port. In this nozzle, the thin tube and the substrate must be fixed directly or with an adhesive, and there must be no gap between them from which a coagulable substance may leak. In addition, the gasket connecting the substrate and holder should be in perfect contact to prevent coagulable substances from leaking outside. Similarly, the bonding portion between the substrate and the coagulation liquid supply device should be in close contact with each other to prevent the coagulation liquid from leaking to the outside.
In addition, the coagulation liquid supply device and coagulation liquid introduction pipe are installed using the usual method.
For example, is it fixed by welding, gluing, screwing, etc.
Alternatively, it is preferable to handle it if it is a single piece.

本発明におけるラテツクスの凝固用ノズルの特
徴は、 1 重合体ラテツクス等の凝固性物質が細管より
吐出可能であること、 2 細管の周囲より凝固液の吐出が可能であるこ
と、 であり、細管より吐出した凝固性物質を包み込む
形で凝固液を流し、凝固反応をせしめ得ることを
最大の長所としており、ノズル周辺の水または凝
固液の流れの影響を受け難く、渦流によつて吐出
した凝固性物質が互いに合一しあい粗大塊となる
ようなことがないため、細管の配置は自由に決め
ることが可能である。
The features of the nozzle for coagulating latex according to the present invention are: 1. A coagulable substance such as a polymer latex can be discharged from a capillary. 2. A coagulating liquid can be discharged from around the capillary. The biggest advantage is that the coagulating liquid flows in a manner that envelops the discharged coagulable substance, causing a coagulation reaction.It is not easily affected by the flow of water or coagulating liquid around the nozzle, and the coagulating property discharged by a vortex flow Since the substances do not coalesce together to form a coarse mass, the arrangement of the thin tubes can be freely determined.

本発明におけるラテツクス凝固用ノズルは図面
に示したような如く細管の先端と凝固液の吐出口
が同一平面にある態様にとどまらず、細管が凝固
液供給器より突出している態様、あるいは細管の
先端が凝固液吐出口より基板寄りにある態様であ
つてもよい。しかしながら、細管の先端は凝固液
の細管軸方向流れが存在する領域内にある必要が
あり、該領域は凝固液供給器の形状、あるいは凝
固液吐出口の形状、または凝固液の供給流量等に
よつてある程度調整できる。
The nozzle for latex coagulation according to the present invention is not limited to the embodiment in which the tip of the thin tube and the discharge port of the coagulating liquid are on the same plane as shown in the drawings, but also the embodiment in which the thin tube protrudes from the coagulating liquid supply device, or the tip of the thin tube. may be located closer to the substrate than the coagulation liquid discharge port. However, the tip of the capillary needs to be in a region where the coagulation fluid flows in the capillary axial direction, and this region depends on the shape of the coagulation fluid supply device, the shape of the coagulation fluid discharge port, the supply flow rate of the coagulation fluid, etc. It can be adjusted to some extent.

さらに本発明におけるラテツクス凝固用ノズル
を使用する場合には空気中で使用することは好ま
しくなく、静止した水中または凝固液中、あるい
は静かに流れている水中または凝固液中に設置す
る必要がある。しかる後、凝固性物質をホルダー
より細管に導き、その先端より吐出せしめると同
時に、凝固液を凝固液供給器の凝固液吐出口よ
り、即ち細管の周囲より吐出せしめることによつ
て極めて粉体特性に優れる粉末を製造することが
できる。
Furthermore, when using the latex coagulating nozzle of the present invention, it is not preferable to use it in air, and it is necessary to install it in still water or a coagulating liquid, or in quietly flowing water or a coagulating liquid. After that, the coagulable substance is guided from the holder into the thin tube and discharged from the tip thereof, and at the same time, the coagulated liquid is discharged from the coagulated liquid outlet of the coagulated liquid supply device, that is, from around the thin tube, thereby achieving extremely powder characteristics. It is possible to produce powder with excellent properties.

また本発明におけるラテツクス凝固用ノズルは
細管より吐出される凝固性物質が夫々独立した凝
固液の流れの中で凝固し、糸状凝集体を形成する
ため全体の形状は自由に選択することが可能であ
る。従つてノズル1個当りの細管数については何
ら制約されない。
In addition, in the latex coagulating nozzle of the present invention, the coagulable substances discharged from the thin tubes coagulate in independent coagulating liquid flows to form filamentous aggregates, so the overall shape can be freely selected. be. Therefore, there is no restriction on the number of thin tubes per nozzle.

一方、細管より凝固性物質を凝固液中に吐出せ
しめて糸状凝集体とした後、これを撹拌等の方法
で適度に切断し顆粒状の粉体特性に優れる粉体を
製造する方法において操作上重要なことは凝固液
と凝固性物質の相対流速である。つまり凝固液と
凝固性物質の流速が等し場合、吐出した凝固性物
質は何ら外乱を受けず、そのままの形で凝固す
る。また凝固液の流速に比べて凝固性物質の流速
がある程度速い場合には、吐出した凝固性物質は
吐出直後にゆらぎ現象を生じ凝集体はじゆず状と
なる。さらに凝固性物質の流速を大きくすると吐
出した凝固性物質がつくるジエツト流と凝固液の
境界面で発生する歪応力が凝固しつつある凝固性
物質の機械的強度に打ち勝ち凝固性物質は粉々に
砕けるため良好な顆粒状粉体は得られない。従つ
て細管1本当りの凝固性物質の吐出量を増大しノ
ズルの生産性を向上するためには、凝固液の流速
を増大せしめる必要があるが、凝固液供給器を持
たないノズルにおいてはノズル周囲の凝固液流速
を増大せしめるとノズルの下流に生じる渦域が拡
大するので、渦域の外部に存在する層流域に凝固
性物質を吐出するためには細管をより長くする必
要がある。このことはノズルの製作上あるいは取
扱上好ましくない。しかし図面に示す如きノズル
であれば凝固液供給器に導入する凝固液の流量を
増加させるだけで、吐出する凝固性物質に対する
凝固液の流速は増加することになる。従つて凝固
性物質の流速も増加せしめることが可能となり工
業的に有利となる。加うるに凝固液供給器によつ
て細管は機械的外力より保護されており、ノズル
の取扱上極めて有利である。すなわち、工業的に
最も有利なノズルは凝固性物質が流れる細管の周
囲より凝固液の吐出が可能な構造のノズルであ
る。
On the other hand, in a method of producing a powder with excellent granular powder characteristics by discharging a coagulable substance from a thin tube into a coagulating liquid to form a filamentous aggregate, and then cutting the filament appropriately by a method such as stirring, it is difficult to operate. What is important is the relative flow velocity of the coagulating liquid and the coagulable substance. In other words, when the flow rates of the coagulating liquid and the coagulating substance are equal, the discharged coagulating substance is not subjected to any disturbance and coagulates as it is. Further, if the flow rate of the coagulable substance is faster than the flow rate of the coagulating liquid to a certain extent, the discharged coagulable substance will undergo a fluctuation phenomenon immediately after being discharged, and the aggregates will become watery. Furthermore, when the flow rate of the coagulable substance is increased, the strain stress generated at the interface between the jet flow created by the discharged coagulable substance and the coagulating liquid overcomes the mechanical strength of the coagulable substance that is solidifying, and the coagulable substance breaks into pieces. Therefore, good granular powder cannot be obtained. Therefore, in order to increase the amount of coagulable material discharged per capillary tube and improve nozzle productivity, it is necessary to increase the flow rate of the coagulating liquid. When the flow rate of the surrounding coagulating liquid is increased, the vortex region generated downstream of the nozzle expands, so the thin tube needs to be made longer in order to discharge the coagulable substance into the laminar region that exists outside the vortex region. This is unfavorable in terms of manufacturing or handling of the nozzle. However, if the nozzle is as shown in the drawing, simply increasing the flow rate of the coagulating liquid introduced into the coagulating liquid supply device will increase the flow rate of the coagulating liquid relative to the coagulating substance to be discharged. Therefore, it is possible to increase the flow rate of the coagulable substance, which is industrially advantageous. In addition, the thin tube is protected from external mechanical forces by the coagulating liquid feeder, which is extremely advantageous in handling the nozzle. That is, the industrially most advantageous nozzle is a nozzle having a structure that allows the coagulating liquid to be discharged from around the thin tube through which the coagulable substance flows.

本発明におけるラテツクス凝固用ノズルを構成
する細管は先に出願した特願昭56−73115(特開昭
57−187322号)によつて規定される細管であり、
その管径については特に制約ないが、内径は3mm
以下、外径は5mm以下が好ましい。細管の材質は
ガラス類;無機焼結体;ポリメチルメタリレー
ト、ポリ塩化ビニル、ポリアミド、ポリエステ
ル、ポリカーボネート、ポリプロピレン、ポリエ
チレン、ABS樹脂、ポリアセタール、AS樹脂、
フツ素樹脂等の合成樹脂類;ステンレススチー
ル、銅、白金、金、鉛等に金属類が好ましいが、
これらに限定されず凝固液および凝固性物質に対
し化学的に安定な物質であれば、いかなるもので
も使用可能である。
The thin tube constituting the nozzle for latex coagulation in the present invention is disclosed in Japanese Patent Application No. 56-73115 (Japanese Unexamined Patent Publication No.
57-187322),
There are no particular restrictions on the pipe diameter, but the inner diameter is 3mm.
Hereinafter, the outer diameter is preferably 5 mm or less. The material of the tube is glass; inorganic sintered body; polymethyl methacrylate, polyvinyl chloride, polyamide, polyester, polycarbonate, polypropylene, polyethylene, ABS resin, polyacetal, AS resin,
Synthetic resins such as fluororesins; metals such as stainless steel, copper, platinum, gold, and lead are preferred;
The material is not limited to these, but any material can be used as long as it is chemically stable to coagulating liquids and coagulable substances.

またラテツクス凝固用ノズルを構成する基板の
材質は前記細管を構成する材質を同じく用いるこ
とができ、さらに凝固液および凝固性物質に対し
化学的に安定な物質であればいかなるものでもよ
い。また基板の形状は円形、正方形、矩形、長円
形等任意の形状のものが使用できる。
Further, the material of the substrate constituting the latex coagulation nozzle can be the same as the material constituting the capillary described above, and any material may be used as long as it is chemically stable to the coagulating liquid and the coagulable substance. Further, the shape of the substrate can be any shape such as circular, square, rectangular, oval, etc.

ここで細管と基板は固着している必要があり、
固着の方法としては接着剤による方法、細管と基
板を直接固着する方法、一体物として成形する方
法、ネジ込みによる方法等が考えられる。
Here, the tube and the substrate must be firmly attached.
Possible fixing methods include using an adhesive, directly fixing the thin tube and the substrate, molding them as an integral body, and screwing them together.

接着剤を使用する場合には凝固液および凝固性
物質に対し化学的に安定であつて、細管および基
板を接着せしめる能力を有するものであればいか
なるものも使用することができ、例えばエポキシ
系接着剤、ゴム系接着剤、ホツトメルト型接着剤
等が使用できる。
When using an adhesive, any adhesive can be used as long as it is chemically stable to coagulating liquids and coagulable substances and has the ability to bond the capillary and the substrate, such as epoxy adhesive. Agents, rubber adhesives, hot melt adhesives, etc. can be used.

細管と基板を直接固着する場合には細管を固定
した型の中に基板を形成する重合性物質を流し込
み重合反応せしめることにより基板と細管とを固
着せしめる方法、さらには細管を固定した型の中
に基板を形成する溶融物質を流し込んだ後、冷却
固化せしめることにより基板と細管とを固着せし
める方法が挙げられる。また一体物として成形す
る場合には合成樹脂を用いた射出成形、金属を用
いた鋳込成形等により成形する。
In the case of directly fixing the thin tube and the substrate, there is a method of pouring a polymerizable substance forming the substrate into a mold in which the thin tube is fixed and causing a polymerization reaction, thereby fixing the substrate and the thin tube. An example of this method is to pour a molten substance forming the substrate into the substrate, and then cool and solidify the substance, thereby fixing the substrate and the thin tube. Moreover, when molding as an integral part, injection molding using synthetic resin, casting molding using metal, etc. are used.

ネジ込みによる方法では細管に雄ネジ、基板雌
ネジを切り細管を基板にネジ込んでやればよい。
In the screwing method, it is sufficient to cut a male thread on the thin tube and a female thread on the substrate, and then screw the thin tube into the substrate.

さらにラテツクス凝固用ノズルを構成するホル
ダーは配管より供給される凝固性物質を細管に分
配するためのもので、通常は漏斗状の形状をした
ものが使用できる。このホルダーの材質は前記細
管を構成する材質と同様のものが使用可能であ
る。
Furthermore, the holder constituting the latex coagulating nozzle is for distributing the coagulable substance supplied from the piping into the thin tubes, and usually has a funnel shape. The material for this holder can be the same as the material constituting the thin tube.

基板とホルダーは保守を容易にする目的で、通
常分離できる構造となつていることが好ましい
が、必ずしもこれに限定されるものではない。な
お、分離できる構造とした場合には基板とホルダ
ーはガスケツトを介して締結具で接合される例が
一例として挙げられる。ガスケツトとしてはゴム
板、ポリテトラフルオロエチレン板、O−リング
等が使用できる。また締結具としてはボルト、万
力、締め付けリング等通常の手段が利用できる。
For the purpose of easy maintenance, it is preferable that the substrate and the holder have a structure that allows them to be separated, but the structure is not necessarily limited to this. In the case of a separable structure, for example, the substrate and the holder may be joined with a fastener via a gasket. As the gasket, a rubber plate, a polytetrafluoroethylene plate, an O-ring, etc. can be used. Further, as the fastener, ordinary means such as a bolt, a vise, a tightening ring, etc. can be used.

次に本発明の凝固用ノズルを構成する凝固液供
給器は凝固液導入管を有し、また細管数と同数の
凝固液吐出口を有する。凝固液吐出口に細管が到
達している場合には凝固液供給器と細管の間隙は
3mm以内であるのが好ましいが、必ずしもこれに
限定されるものではない。また凝固液吐出口の長
さは凝固液の流れを整流する必要から上記間隙よ
り長い方が好ましいようである。凝固液供給器は
製作上、組立上、保守上基板と分離できることが
好ましく、この場合には前記基板とホルダーの接
合と同様に同様のガスケツトを介して締結具で接
合される。
Next, the coagulating liquid supply device constituting the coagulating nozzle of the present invention has a coagulating liquid inlet tube and has the same number of coagulating liquid discharge ports as the number of capillary tubes. When the thin tube reaches the coagulation liquid discharge port, the gap between the coagulation liquid supply device and the thin tube is preferably 3 mm or less, but it is not necessarily limited to this. Further, it seems preferable that the length of the coagulation liquid discharge port be longer than the above-mentioned gap since it is necessary to rectify the flow of the coagulation liquid. For manufacturing, assembly, and maintenance reasons, it is preferable that the coagulating liquid supply device be able to be separated from the substrate, and in this case, it is joined with a fastener via a similar gasket as in the case of joining the substrate and holder.

凝固液供給器および凝固液導入管の材質は前記
細管を構成する材質と同様のものが使用可能であ
る。
The material of the coagulation liquid supply device and the coagulation liquid introduction tube may be the same as the material constituting the thin tube.

本発明の凝固方法は使用するノズルが吐出した
凝固性物質を包み込む形で凝固液を流し得るの
で、ノズル周辺の水または凝固液の流れの影響を
受け難く、渦流によつて吐出した凝固性物質が互
いに合一しあい粗大塊となるようなことがない等
優れた効果を奏する。
The coagulating method of the present invention allows the coagulating liquid to flow in a manner that envelops the coagulable substance discharged by the nozzle used, so it is less affected by the flow of water or coagulating liquid around the nozzle, and the coagulating substance discharged by the vortex flow. It has excellent effects such as preventing the particles from coalescing into large lumps.

本発明において使用する重合体ラテツクスは乳
化重合で得られ回収いうる高分子ラテツクスのほ
とんどが適用可能である。特に効果を発揮する重
合体ラテツクスとしては、エチレン性単量体の乳
化重合によつて得られるラテツクス、ゴム状重合
体ラテツクス、ゴム状重合体にエチレン性単量体
をグラフト重合させたラテツクス、エチレン性単
量体の重合体にゴム形成単量体をグラフト重合さ
せたラテツクスおよびこれらの混合ラテツクス等
が挙げられる。
As the polymer latex used in the present invention, most polymer latexes that can be obtained by emulsion polymerization and can be recovered can be used. Particularly effective polymer latexes include latexes obtained by emulsion polymerization of ethylenic monomers, rubbery polymer latexes, latexes obtained by graft polymerizing ethylenic monomers onto rubbery polymers, and ethylene. Latexes obtained by graft-polymerizing a rubber-forming monomer onto a polymer of a rubber-forming monomer, and mixed latexes thereof can be mentioned.

エチレン性単量体としては、スチレン、α−メ
チルスチレン、O−エチルスチレン、O−クロル
スチレン、P−クロルスチレン、ジビニルベンゼ
ンなどのスチレン系単量体、アクリロニトリル、
シアン化ビニリデンなどのアクリロニトリル系単
量体、アクリル酸やアクリル酸メチル、アクリル
酸エチルなどのアクリル酸エステル、メタクリル
酸やメタクリル酸メチル、メタクリル酸エチルな
どのメタクリル酸エステル、酢酸ビニルなどのビ
ニルエステル、塩化ビニリデンなどのビニリデ
ン、塩化ビニルなどのハロゲン化ビニルなどや他
にビニルケトン、アクリル酸アミド、無水マレイ
ン酸などが挙げられ、これらの単量体は単独で、
または混合して使用される。
Examples of ethylenic monomers include styrene monomers such as styrene, α-methylstyrene, O-ethylstyrene, O-chlorostyrene, P-chlorostyrene, and divinylbenzene, acrylonitrile,
Acrylonitrile monomers such as vinylidene cyanide, acrylic acid esters such as acrylic acid, methyl acrylate, and ethyl acrylate, methacrylic acid esters such as methacrylic acid, methyl methacrylate, and ethyl methacrylate, vinyl esters such as vinyl acetate, Examples include vinylidene such as vinylidene chloride, vinyl halides such as vinyl chloride, vinyl ketone, acrylamide, maleic anhydride, etc. These monomers can be used alone,
or used in combination.

ゴム状重合体としては、天然ゴム、ブタジエン
ゴム、スチレン−ブタジエン共重合体、アクリロ
ニトリル−ブタジエン共重合体、イソブレンゴ
ム、クロロブレンゴム、アクリルゴム、エチレン
−酢酸ビニル共重合体などの天然または合成ゴム
状重合体が挙げられる。
Examples of rubbery polymers include natural or synthetic rubbers such as natural rubber, butadiene rubber, styrene-butadiene copolymer, acrylonitrile-butadiene copolymer, isobrene rubber, chloroprene rubber, acrylic rubber, and ethylene-vinyl acetate copolymer. Examples include polymers.

本発明に用いられる高分子ラテツクスの凝固剤
としては、一般に使用される酸または水溶性無機
塩が全て使用可能であり、酸としては、硫酸・塩
酸類の鉱酸、酢酸等の解離定数10-6mol/以上
の有機酸(安息香酸、サルチル酸、ギ酸、酒石酸
を含む)、塩としては硫酸マグネシウム、硫酸ナ
トリウム等の硫酸塩や塩化物、酢酸塩を含み、こ
れらの混合物も使用可能である。
As a coagulant for the polymer latex used in the present invention, all commonly used acids or water-soluble inorganic salts can be used. Examples of acids include mineral acids such as sulfuric acid and hydrochloric acid, and acetic acid, which has a dissociation constant of 10 - 6 mol/or more of organic acids (including benzoic acid, salicylic acid, formic acid, and tartaric acid), salts include sulfates such as magnesium sulfate and sodium sulfate, chlorides, and acetates; mixtures of these can also be used. .

高分子ラテツクスに予め分散剤、滑剤、増粘
剤、界面活性剤、塑剤、酸化防止剤、着色剤、発
泡剤などの公知の添加物を添加することもでき
る。特に分散剤は、凝固して形成された二次粒子
の粒子形状安定性に大きく影響を与える場合もあ
る。分散剤としては乳化重合や懸濁重合の安定剤
として通常使用される無機系分散剤や有機系分散
剤が使用可能である。無機系分散剤としては炭酸
マグネシウム、第三リン酸カルシウムなどが、ま
た有機系分散剤のうち、天然および合成高分子分
散剤としてはデンプン、ゼラチン、アクリルアミ
ド、部分ケン化ポリビニルアルコール、部分ケン
化ポリメタクリル酸メチル、ポリアクリル酸およ
びその塩、セルロース、メチルセルロース、ポリ
アルキレンオキシド、ポリビニルピロドリン、ポ
リビニルイミダゾール、スルフオン化ポリスチレ
ンなどが挙げられ、また低分子分散剤として、例
えばアルキルベンゼンスルフオン酸塩、脂肪酸塩
などの通常の乳化剤も使用可能である。
Known additives such as dispersants, lubricants, thickeners, surfactants, plasticizers, antioxidants, colorants, and blowing agents can also be added to the polymer latex in advance. In particular, the dispersant may greatly affect the particle shape stability of the secondary particles formed by coagulation. As the dispersant, inorganic dispersants and organic dispersants that are commonly used as stabilizers for emulsion polymerization and suspension polymerization can be used. Examples of inorganic dispersants include magnesium carbonate and tribasic calcium phosphate, and among organic dispersants, natural and synthetic polymer dispersants include starch, gelatin, acrylamide, partially saponified polyvinyl alcohol, and partially saponified polymethacrylic acid. Methyl, polyacrylic acid and its salts, cellulose, methylcellulose, polyalkylene oxide, polyvinylpyrodrine, polyvinylimidazole, sulfonated polystyrene, etc., and as low molecular dispersants, for example, alkylbenzene sulfonates, fatty acid salts, etc. Conventional emulsifiers can also be used.

また増粘剤として水あめ、パラフイン等を添加
することにより二次粒子の形成を容易にし、粒子
形状を制御することも可能である。
It is also possible to facilitate the formation of secondary particles and control the particle shape by adding starch syrup, paraffin, etc. as a thickener.

以下、実施例により本発明を具体的に説明す
る。なお実施例、比較例中「部」及び「%」は全
て「重量部」および「重量%」である。
Hereinafter, the present invention will be specifically explained with reference to Examples. In Examples and Comparative Examples, "parts" and "%" are all "parts by weight" and "% by weight."

実施例 1 厚さ6mm、直径150mmのポリメタクリル酸メチ
ル製基板に均等に外径2mm、内径1mm、長さ50mm
のポリメタクリル酸メチル製細管100本を差し込
み両者をエポキシ系接着剤“エピコン”(商品名、
大日本インキ株式会社製)で固着する。別に孔径
4mm、孔の長さ5mmの凝固液吐出口を有する凝固
液供給器および漏斗状のホルダーをポリメタクリ
ル酸メチルで製作し、シリコンゴム板をガスケツ
トとしてこれらを接合し、図面に示す如き凝固ノ
ズルを得た。この凝固ノズルの細管の先端と凝固
液吐出口は同一面にある。
Example 1 An outer diameter of 2 mm, an inner diameter of 1 mm, and a length of 50 mm are evenly distributed on a polymethyl methacrylate substrate with a thickness of 6 mm and a diameter of 150 mm.
Insert 100 thin tubes made of polymethyl methacrylate and glue them together with epoxy adhesive "Epicon" (trade name,
(manufactured by Dainippon Ink Co., Ltd.). Separately, a coagulating liquid supply device and a funnel-shaped holder having a coagulating liquid discharge port with a hole diameter of 4 mm and a hole length of 5 mm were manufactured from polymethyl methacrylate, and these were joined using a silicone rubber plate as a gasket to form a coagulating liquid as shown in the drawing. Got the nozzle. The tip of the thin tube of this coagulation nozzle and the coagulation liquid discharge port are on the same plane.

これを凝固液(1%の硫酸水溶液)が静かに流
れる凝固槽に設置し毎分2の割合でブタジエン
35部、アクリロニトリル19部、スチレン46部から
なる重合体のラテツクス(固形分38%)をホルダ
ーに導入すると同時に毎分3の割合で凝固液
(1%硫酸水溶液)を凝固液供給器に導入した。
その結果細管より重合体ラテツクスが凝固液吐出
口から凝固液がそれぞれ吐出し、両者が接触する
ことによつて重合体ラテツクスはじゆず状の凝集
体となつたので、これを固化槽へ移し重合体の温
度を92℃に昇温した。固化した重合体粒子を取り
出し遠心脱水機(遠心力は600G)によつて遠心
脱水したところ、得られた湿粉中の水分は17.5%
(ドライベース)であつた。本凝固操作を連続し
て100時間続けたが、その間ラテツクスおよび凝
固液の吐出状態は非常に安定しており、ノズルの
閉塞は観測されなかつた。
This was placed in a coagulation tank where a coagulation solution (1% sulfuric acid aqueous solution) was flowing quietly, and butadiene was added at a rate of 2 per minute.
A polymer latex (solid content: 38%) consisting of 35 parts of acrylonitrile, 19 parts of acrylonitrile, and 46 parts of styrene was introduced into the holder, and at the same time a coagulating liquid (1% aqueous sulfuric acid solution) was introduced into a coagulating liquid feeder at a rate of 3 per minute. .
As a result, the polymer latex was discharged from the thin tube and the coagulating liquid was discharged from the coagulating liquid discharge port, and as the two came into contact, the polymer latex became a lily-shaped aggregate, which was transferred to a solidification tank and the polymer was The temperature was raised to 92°C. When the solidified polymer particles were taken out and centrifugally dehydrated using a centrifugal dehydrator (centrifugal force is 600G), the moisture content of the obtained wet powder was 17.5%.
(dry base). This coagulation operation was continued for 100 hours, during which time the discharge conditions of the latex and coagulation liquid were very stable, and no nozzle clogging was observed.

また、得られた重合体湿粉を十分に乾燥した乾
粉の嵩比重は0.45、平均粒径は0.95mm、250メツ
シユ標準篩通過量は全体の0.11%であつた。本実
施例で得られた粉体は後述の比較例3で得られた
粉体とくらべて極めて脱水性がよく、嵩比重が大
きく、且つ平均粒径が大きく、しかも極端に微粉
が少いものであつて、理想的な粉体と言える。
Further, the bulk specific gravity of the dried powder obtained by sufficiently drying the obtained wet polymer powder was 0.45, the average particle size was 0.95 mm, and the amount passing through a 250 mesh standard sieve was 0.11% of the total. Compared to the powder obtained in Comparative Example 3 described later, the powder obtained in this example has extremely good dehydration properties, has a large bulk specific gravity, has a large average particle size, and has an extremely small amount of fine powder. It can be said to be an ideal powder.

実施例 2 厚さ5mm、直径190mmのポリカーボネート製基
板に均等に外径1.26mm、内径0.90mm、長さ50mmの
ステンレススチール製細管を1000本差し込み両者
をエポキシ系接着剤“エピコン”で固着する。別
に孔径2mm、孔の長さ6mmの凝固液吐出口を有す
る凝固液供給器および漏斗状のホルダーをポリカ
ーボネートで製作し、ネオブレンゴム製O−リン
グを介してこれらを接合し、図面に示す如き凝固
ノズルを得た。この凝固ノズルの細管の先端と凝
固液吐出口は同一面にある。
Example 2 1000 stainless steel thin tubes with an outer diameter of 1.26 mm, an inner diameter of 0.90 mm, and a length of 50 mm were evenly inserted into a polycarbonate substrate with a thickness of 5 mm and a diameter of 190 mm, and both were fixed with epoxy adhesive "Epicon". Separately, a coagulating liquid supply device and a funnel-shaped holder having a coagulating liquid discharge port with a hole diameter of 2 mm and a hole length of 6 mm were manufactured from polycarbonate, and these were joined via a neoprene rubber O-ring to form a coagulating nozzle as shown in the drawing. I got it. The tip of the thin tube of this coagulation nozzle and the coagulation liquid discharge port are on the same plane.

これを凝固液(1%硫酸水溶液)が静かに流れ
る凝固槽に設定し、毎分18の割合で実施例1と
同一の重合体ラテツクスをホルダーに導入すると
同時に、毎分3.5の割合で凝固液(1%硫酸水
溶液)を凝固液供給器に導入した。その結果、重
合体ラテツクスは細管より勢いよく吐出しじゆず
状に凝固したので、これを固化槽へ移し重合体の
温度を92℃に昇温し重合体を固化した。次いで固
化槽により固化した重合体粒子を取り出し遠心脱
水機(遠心力は600G)によつて遠心脱水したと
ころ、得られた湿粉中の水分は17.1%(ドライベ
ース)であつた。本凝固操作を連続して8時間続
けたが、その間ラテツクスおよび凝固液の吐出状
態は非常に安定しており、ノズルの閉塞は観測さ
れなかつた。また得られた湿粉を十分乾燥した
後、粉体物性を測つたところ、乾粉の嵩比重は
0.47、平均粒径は0.90mm、250メツシユ標準篩通
過量は全体の0.06%であつた。
This was set in a coagulation tank where a coagulation liquid (1% sulfuric acid aqueous solution) was flowing gently, and the same polymer latex as in Example 1 was introduced into the holder at a rate of 18 per minute, and at the same time, the coagulation liquid was introduced at a rate of 3.5 per minute. (1% aqueous sulfuric acid solution) was introduced into the coagulation liquid feeder. As a result, the polymer latex was vigorously discharged from the thin tube and solidified in the shape of a slow drop, so this was transferred to a solidification tank and the temperature of the polymer was raised to 92°C to solidify the polymer. Next, the solidified polymer particles were taken out from the solidification tank and centrifugally dehydrated using a centrifugal dehydrator (centrifugal force: 600G), and the moisture content of the obtained wet powder was 17.1% (dry base). This coagulation operation was continued for 8 hours, during which time the discharge conditions of the latex and coagulation liquid were very stable, and no nozzle clogging was observed. In addition, after sufficiently drying the obtained wet powder, we measured the powder physical properties and found that the bulk specific gravity of the dry powder was
0.47, the average particle size was 0.90 mm, and the amount passing through a 250-mesh standard sieve was 0.06% of the total.

実施例 3 厚さ6mm、直径150mmのポリメタクリル酸メチ
ル製基板に均等に外径2mm、内径1mm、長さ50mm
のポリメタクリル酸メチル製細管100本を差し込
み、両者をエポキシ系接着剤“エピコン”で固着
する。別に孔径4mm、孔の長さ20mmの凝固液吐出
口を有する凝固液供給器および漏斗状のホルダー
をポリメタクリル酸メチルで製作し、シリコンゴ
ム板をガスケツトとしてこれらを接合し、図面の
如き凝固ノズルを得た。この凝固ノズルの細管の
先端と凝固液吐出口は同一面にある。
Example 3 An outer diameter of 2 mm, an inner diameter of 1 mm, and a length of 50 mm are evenly distributed on a polymethyl methacrylate substrate with a thickness of 6 mm and a diameter of 150 mm.
Insert 100 thin tubes made of polymethyl methacrylate and secure them together with epoxy adhesive "Epicon". Separately, a coagulating liquid supply device with a coagulating liquid discharge port with a hole diameter of 4 mm and a hole length of 20 mm and a funnel-shaped holder were manufactured from polymethyl methacrylate, and these were joined using a silicone rubber plate as a gasket to form a coagulating nozzle as shown in the drawing. I got it. The tip of the thin tube of this coagulation nozzle and the coagulation liquid discharge port are on the same plane.

これを凝固液(1%硫酸水溶液)が静かに流れ
る凝固槽に設置し、毎分4の割合で実施例1と
同一の重合体ラテツクスをホルダーに導入すると
同時に凝固液(1%硫酸水溶液)を毎分25の割
合で凝固液供給器に導入した。その結果ノズルよ
り重合体ラテツクスおよび凝固液がともに勢いよ
く凝固槽に吐出し重合体ラテツクスはじゆず状に
凝固した。次いで凝固した重合体を固化槽へ移し
92℃に加熱して、重合体粒子を固化した後、遠心
脱水機(遠心力は600G)によつて遠心脱水し湿
粉を得た。得られた湿粉中の水分は18.8%(ドラ
イベース)であつた。本凝固操作を連続して30時
間続けてがその間ラテツクスおよび凝固液の吐出
状態は安定しており、ノズルの閉塞は観測されな
かつた。また得られた湿粉を十分乾燥した後、粉
体物性を測定したところ乾粉の嵩比重は0.43、平
均粒径は0.91mm、250メツシユ標準篩通過量は全
体の0.15%であつた。尚、本実施例では実施例1
にくらべて細管1本当りの生産量が2倍に向上し
た。
This was placed in a coagulation tank where the coagulation liquid (1% sulfuric acid aqueous solution) was flowing gently, and the same polymer latex as in Example 1 was introduced into the holder at a rate of 4 per minute, and at the same time the coagulation liquid (1% sulfuric acid aqueous solution) was introduced into the holder. The coagulation liquid was introduced into the coagulation liquid feeder at a rate of 25 per minute. As a result, both the polymer latex and the coagulating liquid were vigorously discharged from the nozzle into the coagulating tank, and the polymer latex coagulated in the shape of a drop. The solidified polymer is then transferred to a solidification tank.
After heating to 92°C to solidify the polymer particles, they were centrifugally dehydrated using a centrifugal dehydrator (centrifugal force: 600G) to obtain wet powder. The moisture content of the obtained wet powder was 18.8% (dry basis). This coagulation operation was continued for 30 hours, during which time the discharge conditions of the latex and coagulation liquid were stable, and no nozzle clogging was observed. Further, after sufficiently drying the obtained wet powder, the physical properties of the powder were measured, and the bulk specific gravity of the dry powder was 0.43, the average particle size was 0.91 mm, and the amount passing through a 250 mesh standard sieve was 0.15% of the total. In this example, Example 1
The production volume per tube has been doubled compared to the previous model.

実施例 4 細管の長さが15mmである以外は実施例1で用い
た凝固ノズルと同一の凝固ノズルを製作した。従
つて、本凝固ノズルの細管は凝固液吐出口より20
mm突出している。これを凝固液(0.2%硫酸アル
ミニウム水溶液)が静かに流れる凝固槽に設置
し、毎分2の割合でブタジエン50部、メタクリ
ル酸メチル20部、スチレン30部からなる重合体の
ラテツクス(固形分40%)をホルダーに導入する
と同時に毎分3の割合で凝固液(0.2%硫酸ア
ルミニウム水溶液)を凝固液供給器に導入した。
その結果、重合体ラテツクスは良好な状態でじゆ
ず状に凝固したので、これを固化槽へ移し85℃に
加熱固化せしめた。固化した重合体粒子を遠心脱
水機(遠心力は600G)で脱水したところ、水分
16.2%(ドライベース)を含む湿粉が得られた。
本凝固操作を連続して64時間続けたがその間ラテ
ツクスおよび凝固液の吐出状態は安定しており、
ノズルの閉塞は観測されなかつた。また得られた
湿粉を十分乾燥後、粉体物性を測定したところ乾
粉の嵩比重は0.45、平均粒径は1.06mm、250メツ
シユ標準篩通過量は全体の0.03%であつた。
Example 4 A coagulation nozzle identical to that used in Example 1 was manufactured except that the length of the capillary was 15 mm. Therefore, the thin tube of this coagulation nozzle is 20 mm from the coagulation liquid outlet.
mm protrudes. This was placed in a coagulation tank where a coagulation liquid (0.2% aluminum sulfate aqueous solution) was flowing gently, and a polymer latex (solid content 40 %) was introduced into the holder, and at the same time, coagulation liquid (0.2% aluminum sulfate aqueous solution) was introduced into the coagulation liquid supply device at a rate of 3 per minute.
As a result, the polymer latex was solidified in a good condition in a succulent shape, so it was transferred to a solidification tank and solidified by heating at 85°C. When the solidified polymer particles were dehydrated using a centrifugal dehydrator (centrifugal force is 600G), water was removed.
A wet flour containing 16.2% (dry basis) was obtained.
This coagulation operation was continued for 64 hours, during which time the discharge conditions of the latex and coagulation liquid remained stable.
No nozzle blockage was observed. Further, after sufficiently drying the obtained wet powder, the physical properties of the powder were measured, and the bulk specific gravity of the dry powder was 0.45, the average particle size was 1.06 mm, and the amount passing through a 250 mesh standard sieve was 0.03% of the total.

実施例 5 細管の長さが43mmである以外は実施例1で用い
た凝固ノズルと同一の凝固ノズルを製作した。従
つて、本凝固ノズルの細管の先端と凝固液供給器
の内面の間隙は2mmである。これを凝固液(0.5
%硫酸マグネシウム水溶液)が静かに流れる凝固
槽に設置し、毎分2の割合でブタジエン60部、
メタクリル酸メチル13部、スチレン23部、アクリ
ル酸ブチル4部からなる重合体のラテツクス(固
形分35%)をホルダーに導入すると同時に毎分3
の割合で凝固液(0.5%硫酸マゲネシウム水溶
液)を凝固液供給器に導入した。その結果、細管
より吐出した重合体ラテツクスは凝固液供給器の
中で凝固液の流れに搬送され凝固液吐出口へ吸い
込まれるように流れ、該吐出口より凝固液と共に
じゆず状に凝固して吐出した。これを固化槽へ移
し重合体粒子を90℃加熱固化した後、遠心脱水機
(遠心力は600G)で脱水し、水分18.0%(ドライ
ベース)を含む湿粉を得た。本凝固操作を連続し
て48時間続けたが、その間ラテツクスおよび凝固
液の吐出状態は安定しておりノズルの閉塞は観測
されなかつた。また得られた湿粉を十分乾燥後粉
体物性を測定したところ乾粉の嵩比重は0.47、平
均粒径は1.12mm、250メツシユ標準篩通過量は全
体の0.01%以下であつた。
Example 5 A coagulation nozzle identical to that used in Example 1 was manufactured except that the length of the capillary was 43 mm. Therefore, the gap between the tip of the thin tube of this coagulation nozzle and the inner surface of the coagulation liquid supply device was 2 mm. Add this to the coagulation liquid (0.5
% magnesium sulfate aqueous solution) was placed in a coagulation tank where it was gently flowing, and 60 parts of butadiene was added at a rate of 2/min.
A polymer latex (35% solids) consisting of 13 parts of methyl methacrylate, 23 parts of styrene, and 4 parts of butyl acrylate was introduced into the holder at a rate of 3 parts per minute at the same time.
A coagulating liquid (0.5% magnesium sulfate aqueous solution) was introduced into the coagulating liquid supply device at a ratio of . As a result, the polymer latex discharged from the thin tube is carried by the flow of the coagulating liquid in the coagulating liquid supply device and flows as if being sucked into the coagulating liquid outlet, where it coagulates in a slow-flowing manner along with the coagulating liquid from the outlet. I spat it out. This was transferred to a solidification tank and the polymer particles were solidified by heating at 90°C, and then dehydrated using a centrifugal dehydrator (centrifugal force: 600G) to obtain a wet powder containing 18.0% moisture (dry base). This coagulation operation was continued for 48 hours, during which time the discharge conditions of the latex and coagulation liquid were stable and no nozzle clogging was observed. Further, after thoroughly drying the obtained wet powder, the physical properties of the powder were measured, and the bulk specific gravity of the dry powder was 0.47, the average particle size was 1.12 mm, and the amount passing through a 250-mesh standard sieve was less than 0.01% of the total.

比較例 1 実施例2で用いたノズルより凝固液供給器を取
り外し、細管の周囲より凝固液の供給が無いよう
にした他は実施例2と同一の凝固操作を行つた。
その結果、重合体ラテツクスをホルダーに導入し
て30秒経過したとき凝固した重合体の粗大塊が観
測され、その後連続的に該粗大塊が発生し、良好
な凝固操作は行えなかつた。また運転終了後ノズ
ルを調べたところ大部分の細管が閉塞していた。
Comparative Example 1 The same coagulation operation as in Example 2 was performed except that the coagulation liquid supply device was removed from the nozzle used in Example 2 so that no coagulation liquid was supplied from around the thin tube.
As a result, coarse lumps of the coagulated polymer were observed 30 seconds after the polymer latex was introduced into the holder, and the coarse lumps continued to occur thereafter, making it impossible to perform a good coagulation operation. Furthermore, when the nozzle was examined after the operation was completed, most of the capillaries were blocked.

比較例 2 実施例3で用いたノズルより凝固液供給器を取
り外し、細管の周囲より凝固液の供給が無いよう
にした他は、実施例3と同一の凝固操作を行つ
た。その結果、ホルダーに導入した重合体ラテツ
クスは細管より極めて勢いよく吐出し、該ラテツ
クスは粉状に凝固したのでこれを固化槽へ移し92
℃に加熱し重合体を固化した。得られた重合体の
スラリーを遠心脱水機(遠心力は600G)で脱水
し、水分31.7%(ドライベース)を含む湿粉を得
た。さらに該湿粉を十分乾燥した後粉体物性を測
定したところ嵩比重は0.29、平均粒径は0.21mm、
250メツシユ標準篩通過量は全体の2.26%であつ
た。本凝固操作は連続して3時間続けられ、その
間ノズルの閉塞は観測されなかつたものの、粉体
物性に優れる粉は得られなかつた。
Comparative Example 2 The same coagulation operation as in Example 3 was performed except that the coagulation liquid supply device was removed from the nozzle used in Example 3 so that no coagulation liquid was supplied from around the thin tube. As a result, the polymer latex introduced into the holder was expelled extremely vigorously from the thin tube, and the latex solidified into powder, which was transferred to a solidification tank92.
The polymer was solidified by heating to .degree. The obtained polymer slurry was dehydrated using a centrifugal dehydrator (centrifugal force: 600 G) to obtain a wet powder containing 31.7% water (dry base). Furthermore, after sufficiently drying the wet powder, the physical properties of the powder were measured, and the bulk specific gravity was 0.29, the average particle size was 0.21 mm,
The amount passing through the 250 mesh standard sieve was 2.26% of the total. This coagulation operation was continued continuously for 3 hours, and although no nozzle clogging was observed during this period, no powder with excellent powder properties was obtained.

比較例 3 80の容器に1%の硫酸水溶液を30入れ、こ
れを撹拌しながら、さらに実施例1と同一の重合
体ラテツクス20を注ぎ凝析スラリーをつくる。
この方法は従来より広く一般的に行なわれてきた
凝固方法である。該スラリーを92℃に昇温せしめ
て重合体粒子を固化した後遠心脱水機(遠心力は
600G)で脱水した。得られた湿粉の水分は34%
(ドライベース)であり乾燥後の粉体の嵩比重は
0.32、平均粒径は0.26mm、250メツシユ標準篩通
過量は全体の2.12%であつた。
Comparative Example 3 30g of a 1% aqueous sulfuric acid solution was put into an 80m2 container, and while stirring, 20g of the same polymer latex as in Example 1 was poured to prepare a coagulated slurry.
This method is a coagulation method that has been widely used in the past. After heating the slurry to 92°C to solidify the polymer particles, it was heated to a centrifugal dehydrator (the centrifugal force
600G). The moisture content of the obtained wet powder is 34%
(dry base), and the bulk specific gravity of the powder after drying is
0.32, the average particle size was 0.26 mm, and the amount passing through a 250-mesh standard sieve was 2.12% of the total.

【図面の簡単な説明】[Brief explanation of drawings]

図面は本発明で使用するラテツクス凝固用ノズ
ルの一例の断面斜視図である。 1……細管、2……基板、3……ホルダー、4
……ガスケツト、5……締結具、6……凝固液供
給器、7……凝固液導入管、8……凝固液吐出
口。
The drawing is a cross-sectional perspective view of an example of a latex coagulating nozzle used in the present invention. 1...Thin tube, 2...Substrate, 3...Holder, 4
. . . gasket, 5 . . . fastener, 6 . . . coagulation liquid supply device, 7 .

Claims (1)

【特許請求の範囲】 1 重合体ラテツクスを凝固する際に、ラテツク
ス凝固用ノズルとして基板に設けられた細管より
該ラテツクスの吐出が可能であり、かつ細管の周
囲より凝固液の吐出が可能である構造のものを使
用することを特徴とする重合体ラテツクスの凝固
方法。 2 基板と細管が接着剤により固着されたラテツ
クス凝固用ノズルであることを特徴とする特許請
求の範囲第1項記載の重合体ラテツクスの凝固方
法。 3 基板と細管が一体成形により固着されたラテ
ツクス凝固用ノズルであることを特徴とする特許
請求の範囲第1項記載の重合体ラテツクスの凝固
方法。 4 基板と細管が重合反応により固着されラテツ
クス凝固用ノズルであることを特徴とする特許請
求の範囲第1項記載の重合体ラテツクスの凝固方
法。 5 基板と細管が、基板を形成する溶融物質を冷
却固化することによつて固着されたラテツクス凝
固用ノズルであることを特徴とする特許請求の範
囲第1項記載の重合体ラテツクスの凝固方法。
[Scope of Claims] 1. When coagulating polymer latex, the latex can be discharged from a thin tube provided on the substrate as a nozzle for coagulating latex, and the coagulating liquid can be discharged from around the thin tube. A method for coagulating a polymer latex characterized by using a polymer latex having a structure. 2. The method for coagulating polymer latex according to claim 1, wherein the nozzle is a latex coagulating nozzle in which a substrate and a thin tube are fixed with an adhesive. 3. The method for coagulating polymer latex according to claim 1, wherein the nozzle is a latex coagulating nozzle in which a substrate and a thin tube are fixed by integral molding. 4. The method for coagulating polymer latex according to claim 1, wherein the substrate and the thin tube are fixed together by a polymerization reaction to form a nozzle for coagulating latex. 5. The method for solidifying a polymer latex according to claim 1, wherein the substrate and the thin tube are fixed to each other by cooling and solidifying the molten substance forming the substrate.
JP10534283A 1983-06-13 1983-06-13 Method of coagulating polymer latex Granted JPS59230004A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP10534283A JPS59230004A (en) 1983-06-13 1983-06-13 Method of coagulating polymer latex

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP10534283A JPS59230004A (en) 1983-06-13 1983-06-13 Method of coagulating polymer latex

Publications (2)

Publication Number Publication Date
JPS59230004A JPS59230004A (en) 1984-12-24
JPH032363B2 true JPH032363B2 (en) 1991-01-14

Family

ID=14405059

Family Applications (1)

Application Number Title Priority Date Filing Date
JP10534283A Granted JPS59230004A (en) 1983-06-13 1983-06-13 Method of coagulating polymer latex

Country Status (1)

Country Link
JP (1) JPS59230004A (en)

Also Published As

Publication number Publication date
JPS59230004A (en) 1984-12-24

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