JPS63236608A - Apparatus for coagulation and granulation - Google Patents
Apparatus for coagulation and granulationInfo
- Publication number
- JPS63236608A JPS63236608A JP7017587A JP7017587A JPS63236608A JP S63236608 A JPS63236608 A JP S63236608A JP 7017587 A JP7017587 A JP 7017587A JP 7017587 A JP7017587 A JP 7017587A JP S63236608 A JPS63236608 A JP S63236608A
- Authority
- JP
- Japan
- Prior art keywords
- liquid
- granules
- liquid film
- coagulation
- coagulating
- 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
- 238000005469 granulation Methods 0.000 title claims description 34
- 230000003179 granulation Effects 0.000 title claims description 34
- 238000005345 coagulation Methods 0.000 title claims description 27
- 230000015271 coagulation Effects 0.000 title claims description 27
- 239000007788 liquid Substances 0.000 claims abstract description 123
- 239000008187 granular material Substances 0.000 claims abstract description 33
- 230000001112 coagulating effect Effects 0.000 claims abstract description 31
- 239000000126 substance Substances 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims description 2
- 239000011550 stock solution Substances 0.000 abstract description 15
- 238000001035 drying Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 239000000701 coagulant Substances 0.000 abstract 6
- 238000007599 discharging Methods 0.000 abstract 1
- 238000011282 treatment Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 description 20
- 229920000642 polymer Polymers 0.000 description 15
- 239000002245 particle Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 238000012432 intermediate storage Methods 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000000747 cardiac effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229920006158 high molecular weight polymer Polymers 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
Landscapes
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、高分子重合体中に粉粒体が分散、担持された
粒状物等を製造するための凝固造粒装置に関するもので
ある。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a coagulation granulation device for producing granules in which powder particles are dispersed and supported in a high molecular weight polymer.
微粉粒体からの造粒に関しては、目的，材料の種類等に
よって多くの造粒方法並びに造粒装置が知られている。Regarding granulation from fine powder, many granulation methods and granulation devices are known depending on the purpose, type of material, etc.
本発明は、液状物質を液中硬化被覆法によって造粒する
ことを目的とするものであるが、この種の造粒作業につ
いても種々の装置が従業されている。そして前記の液中
硬化被覆法は、微粉粒体の心物質をポリマー溶液中に乳
化分散させた粘稠な液を重力，圧力あるいは遠心力等に
よって適宜の大きさの液滴として、硬化剤浴中に投入す
る方法が造粒の原理であるが、この方法では、出発点か
ら完成されたポリマーが使用され、該完成ポリマは通常
は液溶性である。従って、微粉粒体の心物質を乳化分散
したポリマー溶液の液滴は、硬化剤によって速かに不溶
化し硬化膜を形成して粒状に凝固する性質を有する。The object of the present invention is to granulate a liquid substance by an in-liquid curing coating method, and various apparatuses are used for this type of granulation work. In the liquid-curing coating method, a viscous liquid obtained by emulsifying and dispersing finely divided core substances in a polymer solution is formed into droplets of an appropriate size by gravity, pressure, centrifugal force, etc., and then placed in a curing agent bath. The principle of granulation is the granulation method, in which a finished polymer is used from the starting point, and the finished polymer is usually liquid-soluble. Therefore, the droplets of the polymer solution emulsifying and dispersing the core substance of fine powder particles have the property of being quickly insolubilized by the hardening agent, forming a hardened film, and coagulating into particles.
上記した性質を利用して造粒する場合、液滴化には通常
は回転円盤あるいは該回転円盤を改良したアトマイザ−
カップ等が使用される。そして、凝固造粒体の製造量や
粒径は、回転円盤あるいはアトマイザ−カップの回転速
度と心物質が分散されたポリマー溶液の供給量との相互
の関係によって決定される。When granulating using the above properties, droplets are usually produced using a rotating disk or an atomizer that is an improved version of the rotating disk.
Cups etc. are used. The production amount and particle size of the coagulated granules are determined by the mutual relationship between the rotational speed of the rotating disk or atomizer cup and the supply amount of the polymer solution in which the core substance is dispersed.
前記した回転円盤あるいはアトマイザ−カップの回転速
度が低速から高速になるにつれてポリマー溶液が順次膜
状***、紐状***９滴状***となり、最終的に得られる
液滴の大きさも変化することが知られている。したがっ
て、通常ポリマー溶液を液滴に***させる場合、回転円
盤あるいはアトマイザ−カップは相当の高速で回転され
るのが一般的である。It is known that as the rotational speed of the above-mentioned rotating disk or atomizer cup increases from low to high speed, the polymer solution sequentially splits into films, strings, and 9 droplets, and the size of the final droplets also changes. It is being Therefore, when breaking up a polymer solution into droplets, the rotating disk or atomizer cup is typically rotated at a fairly high speed.
上記のように高速回転によって***された液滴は、飛散
速度が大きいために、硬化剤（凝固液）槽が水平面であ
る場合には広い範囲に飛散するので、その設置には大き
な面積を必要とし、また、液滴の落下位置が限られた範
囲になるため凝固粉が重なりあった固着団塊が生成し易
く、そのため凝固造粒体の連続捕集が困難であった。As mentioned above, the droplets split by high-speed rotation have a high scattering speed, so if the curing agent (coagulating liquid) tank is on a horizontal surface, they will scatter over a wide area, so a large area is required for installation. In addition, since the falling position of the droplets is limited to a limited range, it is easy to form stuck lumps in which the coagulated powder overlaps, making it difficult to continuously collect the coagulated granules.
また、壁面流下式硬化剤槽を使用した場合は、装置面積
は小さくすることができるが、液滴が壁面に衝突するた
めに、造粒体の形状並びに大きさが不揃いとなり、使用
目的に添わないこともある。In addition, when using a wall-flow type curing agent tank, the equipment area can be reduced, but since the droplets collide with the wall, the shape and size of the granules may be irregular, making it difficult to meet the intended use. Sometimes there isn't.
更に、前記したポリマーの溶剤は、蒸気あるいは揮発物
質が作業環境を汚染するものが多いので、前記の如き開
放型の硬化側槽を使用した場合には、汚染物質の環境へ
の散逸も考えられるので、これを防止するには装置を密
閉型とすることで解決が可能ではあるが、−ｉ的に粘稠
液を遠心力によって液滴とする造粒法においては、ポリ
マー溶液の***状態の監視や、回転円盤等の定期的な整
備点検を必要とするために密閉型とすることは好ましく
ない。Furthermore, since many of the polymer solvents mentioned above contaminate the working environment with vapor or volatile substances, when an open curing side tank like the one mentioned above is used, there is a possibility that the contaminants may be dissipated into the environment. Therefore, it is possible to prevent this by making the device a closed type, but in the granulation method in which a viscous liquid is made into droplets by centrifugal force, It is not preferable to use a closed type because it requires monitoring and periodic maintenance and inspection of the rotating disk, etc.
本発明は、液状物質の凝固造粒装置において、前述した
問題点を解決し、装置の小型化を図るとともに、造粒原
液の液滴と凝固液（硬化剤）とを効率良く接触させ、造
粒体と凝固液との分離回収が容易に行うことができ、し
かも生産量をも自由に調節可能となすことを目的とする
ものである。The present invention solves the above-mentioned problems in a coagulation granulation apparatus for liquid substances, aims to downsize the apparatus, and efficiently brings droplets of a granulation stock solution into contact with a coagulation liquid (curing agent) to form a liquid substance. The object of this invention is to enable easy separation and recovery of granules and coagulated liquid, and to freely adjust the production amount.
ｃ問題点を解決するための手段・作用〕本発明の凝固造
粒装置は、前記の目的を達成するために、凝固液を装置
の上部に配設した液膜発生器内に供給し、該液膜発生器
より前記凝固液を装置内に流下せしめ、該凝固液と接触
することにより凝固する性質を有する液状物質を遠心力
によって液滴化し、該液滴と前記の凝固液とを接触せし
めて固体状粒状物とすることをその特徴とするものであ
る。c Means/effect for solving the problem] In order to achieve the above-mentioned object, the coagulation granulation device of the present invention supplies the coagulation liquid into a liquid film generator disposed at the upper part of the device, and The coagulating liquid is caused to flow into the apparatus from a liquid film generator, a liquid substance having the property of solidifying upon contact with the coagulating liquid is turned into droplets by centrifugal force, and the droplets are brought into contact with the coagulating liquid. It is characterized by the fact that it is made into solid granules.
そして、前記したように凝固液を流下させることにより
、造粒原液の液滴は流下する凝固液の中心部位より飛来
させるものであるので前記の流下する凝固液の内面に接
触した際に表面全体が凝固液で瞬間的に包み込まれて凝
固されるものである。By flowing the coagulating liquid as described above, droplets of the granulation stock solution are made to fly from the center of the flowing coagulating liquid, so when they come into contact with the inner surface of the flowing coagulating liquid, they cover the entire surface. is instantaneously wrapped in a coagulating liquid and coagulated.
本発明の実施例を図面に基いて説明する。 Embodiments of the present invention will be described based on the drawings.
第１図は本発明の第一の実施例であり、図において１は
中央部が開口２された器体でその下部はホッパー状の傾
斜底板３とされる。４は前記器体の中央開口部２に配装
された液膜発生器であり、該液膜発生器４は、円筒状の
内外側壁５．６と、凝固液導入管７が接続される頂板８
と、円筒状の外側壁６の下端と小間隙を設けて吐出口９
を形成する円筒状の内側壁５の下端に固定された底板１
０とより円形状の空室とされた流下液膜形成用調圧室１
１より成っている。FIG. 1 shows a first embodiment of the present invention. In the figure, reference numeral 1 denotes a container body with an opening 2 in the center, and a hopper-shaped inclined bottom plate 3 at the bottom thereof. 4 is a liquid film generator disposed in the central opening 2 of the container body, and the liquid film generator 4 has cylindrical inner and outer walls 5.6 and a top plate to which a coagulation liquid introduction pipe 7 is connected. 8
A discharge port 9 is provided with a small gap between the lower end of the cylindrical outer wall 6 and the lower end of the cylindrical outer wall 6.
A bottom plate 1 fixed to the lower end of a cylindrical inner wall 5 forming a
0 and pressure regulating chamber 1 for forming a falling liquid film, which is a circular empty chamber.
It consists of 1.
１２は前記した器体１内の略中央部に配設されたアトマ
イザ−カップであり、該アトマイザ−カップ１２は器体
１の外部より回転軸１３によって回転せしめられる。１
４は前記のアトマイザ−カップ１２に造粒原液を供給す
る造粒原液供給管であり、１５は前記した器体１のホッ
パー状傾斜底板３の下部出口に連接された取出管である
。Reference numeral 12 denotes an atomizer cup disposed approximately at the center of the container 1, and the atomizer cup 12 is rotated by a rotating shaft 13 from the outside of the container 1. 1
Reference numeral 4 denotes a granulation stock solution supply pipe for supplying the granulation stock solution to the atomizer cup 12, and 15 is a take-out pipe connected to the lower outlet of the hopper-shaped inclined bottom plate 3 of the container 1.
なお、造粒原液は水、アルコール等の液体と接触するこ
とにより凝固する性質を有する液状物質にして、例えば
ポリマー溶液であって、粉粒状を心動質として混入され
ていることが望ましい。The granulation stock solution is preferably a liquid substance that solidifies when it comes into contact with a liquid such as water or alcohol, such as a polymer solution, and is preferably mixed with powder or granules as cardiac fluid.
本発明の第一実施例は上記のように構成されるので、凝
固液導入管７より凝固液を所定の供給速度で液膜発生器
４の流下液膜形成用調圧室（以下単に調圧室というＨ１
内に導入すると、凝固液は前記の調圧室１１の外側壁６
の下端周縁に形成された小間隙の吐出口９より押し出さ
れ、凝固液は器体１内に早鐘状に流下する液膜１６を形
成する。Since the first embodiment of the present invention is configured as described above, the coagulating liquid is supplied from the coagulating liquid introduction pipe 7 at a predetermined rate to the liquid film generator 4 in a pressure regulating chamber (hereinafter simply referred to as pressure regulating chamber) for forming a flowing liquid film. H1 called room
When the coagulating liquid is introduced into the pressure regulating chamber 11, the outer wall 6 of the pressure regulating chamber 11
The coagulating liquid is pushed out from the discharge port 9 in a small gap formed at the lower edge of the container 1, and forms a liquid film 16 that flows down into the vessel body 1 in a bell-like manner.
一方、造粒原液供給管１４から器体１の略中央に配装さ
れるアトマイザ−カップ１２内に供給された造粒原液は
、前記アトマイザ−カップ１２の回転によって遠心力に
よって飛ばされて液滴化１７．１７゜１７、・・・・・
・され、前記早鐘状に流下する凝固液の液膜１６の内面
に接触して凝固造粒体１８．１８．１８．・・・・・・
となり、凝固した造粒体１８．１８．１８．・・・・・
・並びに膜状で流下した凝固液は器体１のホブパー状傾
斜底板３に沿って下部中央に集められ、前記の傾斜底板
３に連接される取出管１５より系外に抜き出される。On the other hand, the granulation stock solution supplied from the granulation stock solution supply pipe 14 into the atomizer cup 12 arranged approximately in the center of the container 1 is blown off by centrifugal force due to the rotation of the atomizer cup 12, and drops into droplets. 17.17゜17,...
- The solidified granules 18.18.18.・・・・・・
The solidified granules 18.18.18.・・・・・・
- The coagulated liquid that has flowed down in a film form is collected at the center of the lower part along the hobber-shaped inclined bottom plate 3 of the container body 1, and is extracted out of the system through the take-out pipe 15 connected to the inclined bottom plate 3.
系外に抜き出された造粒体と凝固液とはそれ自体公知の
手段によって分離され、造粒体は目的に応じて分級、熱
処理、乾燥等の処理加工に供される。The granules and coagulation liquid extracted from the system are separated by means known per se, and the granules are subjected to processing such as classification, heat treatment, drying, etc. depending on the purpose.
また、系外に取り出された凝固液はポリマー溶剤が混入
蓄積してくるので、凝固に対してポリマー溶剤の濃度が
許される範囲で中間貯槽において濃度を管理調整し、し
かる後に循環使用するために凝固液導入管７に導くよう
にする。In addition, since the coagulation liquid taken out of the system is contaminated with polymer solvent and accumulates, the concentration of the polymer solvent is controlled and adjusted in an intermediate storage tank within a range that allows for coagulation, and then recycled. It is made to lead to the coagulation liquid introduction pipe 7.
なお、回転せしめて遠心力によって造粒原液を飛ばして
液滴化するのに、第一実施例（後記する第二実施例にお
いても同様）ではアトマイザ−カップを用いることで説
明したが、前記のアトマイザ−カップの代りに回転円盤
としてもよいものである。In addition, in the first embodiment (the same applies to the second embodiment described later), an atomizer cup is used to spray the granulation stock solution by centrifugal force and turn it into droplets. A rotating disk may be used instead of the atomizer cup.
前記した調圧室１１の外周縁に設けられた吐出口９より
該固液を流下せしめて早鐘状の液膜１６を形成するが、
前記凝固液によって形成される早鐘状液膜１６の直径が
大きいものが要求される場合には、吐出される凝固液の
圧力が同じであれば、調圧室１１を構成する円筒状の外
側壁６の下端部より小間隙を有して内側壁５に固設され
た底板１０の先端部を突出せしめたものを用意すればよ
く、また、前記した液膜１６の半径が小さいものが要求
される場合には、前記の底板１０と円筒状外側壁６との
同一の高さとする等として吐出方向を変えるようにする
とよい。The solid liquid is caused to flow down from the discharge port 9 provided at the outer peripheral edge of the pressure regulating chamber 11 described above to form a bell-shaped liquid film 16.
If the bell-shaped liquid film 16 formed by the coagulating liquid is required to have a large diameter, the cylindrical outer wall constituting the pressure regulating chamber 11 may be It is sufficient to prepare a base plate 10 which has a tip portion protruding from the lower end of the bottom plate 10 fixedly attached to the inner wall 5 with a small gap, and also requires a liquid film 16 having a small radius. In this case, it is preferable to change the discharge direction by, for example, making the bottom plate 10 and the cylindrical outer wall 6 the same height.
次に、本発明の第二の実施例を第２図に基いて説明する
が、前述した第一実施例と同−又は均等の構成部材は同
一の符号で示すこととする。Next, a second embodiment of the present invention will be described with reference to FIG. 2, in which constituent members that are the same or equivalent to those of the first embodiment described above are designated by the same reference numerals.
第二実施例は第一実施例で説明した液膜発生器４を構成
する調圧室１１を複数重合して設けたものであり、その
他の構成については、第一実施例と同様である。The second embodiment is provided by superposing a plurality of pressure regulating chambers 11 constituting the liquid film generator 4 described in the first embodiment, and the other configurations are the same as those of the first embodiment.
そして、前記した複数の調圧室を形成するには、この第
二実施例においては、短かい円筒状外側壁６と稍長い円
筒状の中間側壁６′と凝固液導入管７が接続された頂板
８と外側壁６の下端と小間隙を隔てて吐出口９を形成す
る中間側壁６′の途中より突設された底板１０とより第
一調圧室１１′を構成し、更に、前記の円筒状中間側壁
６′と円筒状の内側壁５と凝固液導入管７′が接続され
た頂板８′と、中間側壁６′の下端と小間隙を隔てて吐
出口９′を形成する内側壁下端に固定された底板１０′
とより第二調圧室１１′を構成する。したがって、第
二実施例においては、凝固液導入管７及び７′より凝固
液を所定の供給速度で液膜発生器４の重合された第一調
圧室１１′及び第二調圧室１１″内に各別に導入すると
、凝固液は第−及び第二調圧室１１’及び１１＃にて均
一な圧力とされ、それぞれの調圧室１１’ 、 １１″
の下部外周縁に形成されている小間隙の吐出口９及び９
′より器体ｌ内に押し出されるが、前記第一調圧室１１
′の吐出口９より押し出される凝固液は流下して早鐘状
の外側の液膜１６となり、前記した第一調圧室１１の内
側に形成される第二調圧室１１“の吐出口９′より押し
出される凝固液は流下して前記の外側の早鐘状液膜１６
の内側に小径の早鐘状液膜１６′が形成されることにな
る。In order to form the plurality of pressure regulating chambers described above, in this second embodiment, the short cylindrical outer wall 6, the slightly elongated cylindrical intermediate side wall 6', and the coagulation liquid introduction pipe 7 are connected. The top plate 8 and the bottom plate 10 protruding from the middle of the intermediate side wall 6' which forms the discharge port 9 with a small gap from the lower end of the outer wall 6 constitute a first pressure regulating chamber 11'. A cylindrical intermediate side wall 6', a cylindrical inner wall 5, a top plate 8' to which the coagulating liquid introduction pipe 7' is connected, and an inner wall forming a discharge port 9' with a small gap from the lower end of the intermediate side wall 6'. Bottom plate 10' fixed at the lower end
This constitutes a second pressure regulating chamber 11'. Therefore, in the second embodiment, the coagulating liquid is supplied from the coagulating liquid introduction pipes 7 and 7' at a predetermined rate to the first pressure regulating chamber 11' and the second pressure regulating chamber 11'' where the coagulating liquid is polymerized in the liquid film generator 4. When the coagulating liquid is introduced separately into the pressure regulating chambers 11' and 11#, the pressure of the coagulating liquid is made uniform in the pressure regulating chambers 11' and 11'', respectively.
Small gap discharge ports 9 and 9 formed at the lower outer peripheral edge of the
', but the first pressure regulating chamber 11
The coagulated liquid pushed out from the discharge port 9' flows down to form a bell-shaped outer liquid film 16, and the coagulated liquid is discharged from the discharge port 9' of the second pressure regulation chamber 11'' formed inside the first pressure regulation chamber 11 described above. The coagulated liquid pushed out flows down and forms the outer bell-shaped liquid film 16.
A bell-shaped liquid film 16' having a small diameter is formed on the inside of the tube.
このように、液膜を複数層とするのは、生産量を増大さ
せる一つの手段であり、生産量の増大を図るために回転
円盤やアトマイザ−カップへの造粒原液の供給量を増加
させて、回転円盤やアトマイザ−カップを高速回転せし
めて遠心力を大きくするが、遠心力が大きくなると***
液滴の飛散速度並びに推進慣性力が大きくなるので、液
滴が液膜を貫通する場合も生じ、造粒効率が低下する。In this way, creating multiple layers of liquid film is one way to increase production volume, and in order to increase production volume, the amount of granulation stock solution supplied to the rotating disk or atomizer cup is increased. The centrifugal force is increased by rotating the rotating disk or atomizer cup at high speed, but as the centrifugal force increases, the scattering speed of the split droplets and the propulsion inertia increase, so the droplets may penetrate the liquid film. granulation efficiency decreases.
しかし、液滴は流下する液膜を通過することにより飛散
速度並びに推進慣性力は著しく小さくなるために、外側
の液膜によって捕捉されることになる。更に、液膜を通
過するものがあっても今一つの外膜によって捕捉する仕
組となっているので、液膜を複数層有することによって
飛散液膜を完全に凝固造粒体として捕捉することが可能
である。However, as the droplets pass through the falling liquid film, their scattering speed and propulsion inertia are significantly reduced, so they are captured by the outer liquid film. Furthermore, even if something passes through the liquid film, it is captured by another outer membrane, so by having multiple layers of liquid films, it is possible to completely capture the scattered liquid film as solidified granules. It is.
そして、第一、第二実施例による液膜を早鐘状とするの
は凝固造粒装置を小型化でき、液膜の中心部位より飛来
する液滴を膜の内面で受けるため造粒原液中のポリマー
溶剤などの揮発蒸気の散逸を防止することができるもの
である。The reason why the liquid film according to the first and second embodiments is bell-shaped is that the coagulation and granulation device can be made smaller, and the inner surface of the film receives the droplets that fly from the center of the liquid film. It is possible to prevent the dissipation of volatile vapors such as polymer solvents.
具体例−１
ポリアクリルニトリルのＮ−Ｎジメチルホルムアミド溶
液にチタン酸を混入させた造粒原液を１５２／１１ｒ及
び２０１ ／Ｈｒの速度で、１２００ｒｐｎ＋で回転し
ている５ｃｍφのアトマイザ−カップに供給し液滴化さ
せた。Specific Example-1 A granulation stock solution in which titanic acid was mixed into an N-N dimethylformamide solution of polyacrylonitrile was supplied at a speed of 152/11r and 201/Hr to a 5cmφ atomizer cup rotating at 1200 rpm+. It was made into droplets.
凝固液である水を７０４！ ／ｗｉｎの速度で液膜発生
器に供給し早鐘状の液膜を形成させた。このときの早鐘
状液膜の大きさは、落下終端部で４０ｃｍφであった。Water, which is a coagulating liquid, is 704! The liquid was supplied to a liquid film generator at a speed of /win to form a bell-shaped liquid film. The size of the bell-shaped liquid film at this time was 40 cmφ at the end of the fall.
飛散する造粒原液の液滴を早鐘状液膜凝固液の内面に接
触させたところ、液滴は完全に捕捉され液膜とともに流
下し、次いで底部傾斜板に沿って取出管部へ集められた
。When the scattered droplets of the granulation stock solution were brought into contact with the inner surface of the bell-shaped liquid film solidified liquid, the droplets were completely captured and flowed down together with the liquid film, and were then collected along the bottom inclined plate into the take-out pipe section. .
捕捉された凝固造粒体の平均粒径は、原液供給速度が１
５１ ／Ｈｒのとき０．６６ｍｍφ、 ２０１ ／Ｈｒ
のとき０．７１ｍｍφであった。このときの造粒体の粒
度構成は第３図に記載のとおりであった。The average particle size of the captured coagulated granules is
0.66mmφ when 51/Hr, 201/Hr
At that time, the diameter was 0.71 mm. The particle size structure of the granules at this time was as shown in FIG.
具体例−２
具体例−１と同様の造粒原液を１５１ ／Ｈｒ、 ２０
１ ／Ｈｒ。Specific example-2 The same granulation stock solution as in specific example-1 was heated at 151/Hr, 20
1/Hr.
３０１ ／Ｈｒ及び４０１ ／Ｈｒの供給速度で１５０
Ｏｒｐｍで回転している５ ａｍφのアトマイザ−カッ
プに供給し液滴化させた。凝固液である水を第二実施例
に示す第二調圧室１１“には７０１ ／ｍｉｎで、第一
調圧室１１′には１００１！ ／ｍｉｎで供給し二層の
早鐘状の液膜を形成させた。このときの早鐘状液膜の大
きさは落下終端部で第二調圧室１１＃による内側液膜が
４０ｃｍφ。150 at feed rates of 301/Hr and 401/Hr
The mixture was supplied to an atomizer cup of 5 amφ rotating at 100 rpm to form droplets. Water, which is a coagulating liquid, is supplied to the second pressure regulating chamber 11'' shown in the second embodiment at a rate of 701/min and to the first pressure regulating chamber 11' at a rate of 1001!/min to form a two-layer bell-shaped liquid film. At this time, the size of the bell-shaped liquid film was 40 cmφ at the end of the fall, and the inner liquid film formed by the second pressure regulating chamber 11# was 40 cm in diameter.
第一調圧室１１’による外側液膜で５０ＣＩｌφであっ
た。The outer liquid film formed by the first pressure regulating chamber 11' was 50 CIlφ.
飛散する造粒原液の液滴を内側の液膜凝固液の内面に接
触させたところ、供給速度１５１ ／Ｈｒ並びに２０１
／Ｈｒの場合は液滴は完全に捕捉された。When the scattered droplets of the granulation stock solution were brought into contact with the inner surface of the inner liquid film coagulating liquid, the supply rate was 151/Hr and 201/Hr.
/Hr, the droplet was completely captured.
また、供給速度３０１ ／Ｈｒ及び４０ ｊ！ ／Ｈｒ
では一部内側液膜を通過する液滴が見られたが、それら
は外側の液膜によって完全に捕捉された。内側及び外側
の液膜によって捕捉され凝固した造粒体と落下した凝固
液とは底部傾斜板に沿って取出管部へ集められた。Also, the feed rate is 301/Hr and 40 j! /Hr
Although some droplets were seen passing through the inner liquid film, they were completely captured by the outer liquid film. The solidified granules captured and solidified by the inner and outer liquid films and the fallen solidified liquid were collected along the bottom inclined plate into the take-out pipe section.
捕捉された凝固造粒体の平均粒径は、原液供給速度が１
５１！、／Ｈｒのとき０．６２ｍｍφ、 ２０１２ ／
Ｈｒのとき０．６６ｍｍφ、３０１． ／Ｈｒのとき０
．７３ｍｍφ並びに４０１ ／Ｈｒのとき０．７７ｍｍ
φであった。The average particle size of the captured coagulated granules is
51! , /Hr when 0.62mmφ, 2012 /
When Hr, 0.66mmφ, 301. 0 when /Hr
．． 0.77mm when 73mmφ and 401/Hr
It was φ.
このときの造粒体の粒度構成は第４図記載のとおりであ
る。The particle size structure of the granules at this time is as shown in FIG.
なお、第３図及び第４図において、μは分布の代表値で
あり、σは分布の散布度を表すものである。Note that in FIGS. 3 and 4, μ is a representative value of the distribution, and σ represents the degree of dispersion of the distribution.
本発明に係る凝固造粒装置は、凝固液を装置の上部に配
設した液膜発生器内に供給し、該液膜発生器より前記凝
固液を装置内に流下せしめ、該凝固液と接触することに
より凝固する性質を有する液状物質を遠心力によって液
滴化し、該液滴と前記流下している凝固液とを接触せし
めて固体粒状物とするようにしたので、造粒原液の液滴
は流下する凝固液の内面に接触した際表面全体が凝固液
で瞬間的に包み込まれて凝固し落下する。したがって、
造粒体には重なり合った固着塊などの発生はなく、水平
凝固液槽に比較し造粒体の回収率が高い。The coagulation granulation device according to the present invention supplies a coagulation liquid into a liquid film generator disposed in the upper part of the device, causes the coagulation liquid to flow down into the device from the liquid film generator, and comes into contact with the coagulation liquid. By doing so, the liquid substance that has the property of solidifying is turned into droplets by centrifugal force, and the droplets are brought into contact with the flowing coagulating liquid to form solid granules. When it comes into contact with the inner surface of the flowing coagulating liquid, the entire surface is instantly wrapped in the coagulating liquid, solidifying, and falling. therefore,
There are no overlapping fixed lumps in the granules, and the recovery rate of the granules is higher than in a horizontal coagulation tank.
また、凝固液及び造粒体が連続的に取り出せるために凝
固液と造粒体との分離が容易に行うことができ、分離さ
れた凝固液を循環再使用に供するに際して、中間貯槽を
用いて混入蓄積されるポリマー溶剤の濃度を一定に調整
管理することができるので長時間の連続造粒が可能であ
る。In addition, since the coagulated liquid and granules can be taken out continuously, the coagulated liquid and granules can be easily separated, and when the separated coagulated liquid is recycled and reused, an intermediate storage tank can be used. Since the concentration of the polymer solvent mixed and accumulated can be adjusted and controlled to a constant level, continuous granulation for a long period of time is possible.
更に、造粒原液の液滴が流下する凝固液の内面に接触し
てポリマー溶剤を放出し凝固するために、ポリマー溶剤
の蒸気あるいは揮発物質の散逸が抑えられ作業環境が汚
染されることがない。Furthermore, since the droplets of the granulation stock solution come into contact with the inner surface of the flowing coagulation liquid and release the polymer solvent and solidify, the dissipation of vapor or volatile substances of the polymer solvent is suppressed and the working environment is not contaminated. .
図面は本発明の凝固造粒装置の実施例を示し、第１図は
液膜が単一である第一実施例の説明図、第２図は液膜が
複数層とされた第二実施例の説明図である。
第３図は、具体例−１で得られた造粒体の粒度構成を示
すグラフ、第４図は具体例−２で得られた造粒体の粒度
構成を示すグラフである。
４：液膜発生器
７．７’：；ｉ固液導入管
８．８’ ：頂 板 ９．９’ ：吐出口
１０、１０’ ：底板The drawings show embodiments of the coagulation and granulation apparatus of the present invention, and FIG. 1 is an explanatory diagram of the first embodiment with a single liquid film, and FIG. 2 is an explanatory diagram of the second embodiment with a plurality of liquid films. FIG. FIG. 3 is a graph showing the particle size structure of the granules obtained in Specific Example-1, and FIG. 4 is a graph showing the particle size structure of the granules obtained in Specific Example-2. 4: Liquid film generator 7.7': i Solid-liquid introduction pipe 8.8': Top plate 9.9': Discharge ports 10, 10': Bottom plate
Claims (4)
給し、該液膜発生器より前記凝固液を装置内に流下せし
め、該凝固液と接触することにより凝固する性質を有す
る液状物質を遠心力によって液滴化し、該液滴と前記の
凝固液とを接触せしめて固体粒状物とすることを特徴と
する凝固造粒装置。(1) A coagulating liquid is supplied into a liquid film generator disposed at the top of the device, and the coagulating liquid is caused to flow down into the device from the liquid film generator, and has the property of solidifying upon contact with the coagulating liquid. A coagulation and granulation device characterized by forming a liquid substance into droplets by centrifugal force, and bringing the droplets into contact with the coagulation liquid to form solid granules.
の液滴が前記液膜の内面に接触して凝固することを特徴
とする前記特許請求の範囲第１項記載の凝固造粒装置。(2) The coagulation according to claim 1, wherein the flowing coagulating liquid is a bell-shaped liquid film, and the droplets are solidified by contacting the inner surface of the liquid film. Granulation equipment.
徴とする前記特許請求の範囲第１項又は第２項記載の凝
固造粒装置。(3) The coagulation granulation apparatus according to claim 1 or 2, wherein the liquid film is composed of multiple layers.
を行った後、凝固液を再使用のために循環することを特
徴とする前記特許請求の範囲第１項、第２項又は第３項
記載の凝固造粒装置。(4) Claims 1 and 2 above, characterized in that the coagulation liquid and granules are continuously taken out, solid-liquid separation is performed, and then the coagulation liquid is circulated for reuse. Or the coagulation granulation device according to item 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7017587A JPS63236608A (en) | 1987-03-26 | 1987-03-26 | Apparatus for coagulation and granulation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7017587A JPS63236608A (en) | 1987-03-26 | 1987-03-26 | Apparatus for coagulation and granulation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63236608A true JPS63236608A (en) | 1988-10-03 |
Family
ID=13423930
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7017587A Pending JPS63236608A (en) | 1987-03-26 | 1987-03-26 | Apparatus for coagulation and granulation |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63236608A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5246636A (en) * | 1991-05-07 | 1993-09-21 | Southwest Research Institute | Process for making microcapsules and apparatus therefor |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5829825A (en) * | 1981-07-22 | 1983-02-22 | バスフ・アクチエンゲゼルシヤフト | Reproductive manufacture of various geometrical shape products from polymer dispersion, melt or solution |
| JPS61185416A (en) * | 1985-02-13 | 1986-08-19 | Japan Steel Works Ltd:The | Vertical type apparatus for producing particles in air |
-
1987
- 1987-03-26 JP JP7017587A patent/JPS63236608A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5829825A (en) * | 1981-07-22 | 1983-02-22 | バスフ・アクチエンゲゼルシヤフト | Reproductive manufacture of various geometrical shape products from polymer dispersion, melt or solution |
| JPS61185416A (en) * | 1985-02-13 | 1986-08-19 | Japan Steel Works Ltd:The | Vertical type apparatus for producing particles in air |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5246636A (en) * | 1991-05-07 | 1993-09-21 | Southwest Research Institute | Process for making microcapsules and apparatus therefor |
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