JPH04257527A - Solidification of organic compound and equipment therefor - Google Patents
Solidification of organic compound and equipment thereforInfo
- Publication number
- JPH04257527A JPH04257527A JP1893491A JP1893491A JPH04257527A JP H04257527 A JPH04257527 A JP H04257527A JP 1893491 A JP1893491 A JP 1893491A JP 1893491 A JP1893491 A JP 1893491A JP H04257527 A JPH04257527 A JP H04257527A
- Authority
- JP
- Japan
- Prior art keywords
- organic compound
- concentrated solution
- solution
- reduced pressure
- heating 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.)
- Pending
Links
- 150000002894 organic compounds Chemical class 0.000 title claims abstract description 70
- 238000007711 solidification Methods 0.000 title abstract description 6
- 230000008023 solidification Effects 0.000 title abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 40
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 239000013078 crystal Substances 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000000243 solution Substances 0.000 description 64
- 238000006243 chemical reaction Methods 0.000 description 11
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 3
- 239000011550 stock solution Substances 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000009477 glass transition Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000007664 blowing Methods 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001226 reprecipitation Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Silver Salt Photography Or Processing Solution Therefor (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
【0001】0001
【産業上の利用分野】本発明は、写真用カプラー、色像
形成材料(色材)等写真用素材を含む有機化合物の固化
方法および装置に係わり、特に、有機化合物をその溶液
から固化させる方法および装置に関する。[Field of Industrial Application] The present invention relates to a method and apparatus for solidifying organic compounds including photographic materials such as photographic couplers and color image forming materials (coloring materials), and particularly to a method for solidifying organic compounds from their solutions. and regarding equipment.
【0002】0002
【従来の技術】化学反応によって生成した写真用素材等
の有機化合物を、反応溶液から固体状態で取り出すこと
は、その搬送、計量等の取り扱い性を向上させる上で好
都合である。その最も一般的な方法は、いわゆる再沈殿
を利用する方法である。この方法は、反応溶液に溶解し
ている有機化合物に対し貧溶媒であり、かつ反応溶媒に
対して良溶媒であるところの晶析溶媒中に反応溶液を加
えて有機化合物を晶析させ、これをろ過した後、乾燥す
るものである。BACKGROUND OF THE INVENTION It is advantageous to take out organic compounds such as photographic materials produced by chemical reactions in a solid state from a reaction solution in order to improve their ease of handling such as transportation and weighing. The most common method is a method using so-called reprecipitation. In this method, the reaction solution is added to a crystallization solvent that is a poor solvent for the organic compound dissolved in the reaction solution and a good solvent for the reaction solvent, and the organic compound is crystallized. After filtering, it is dried.
【0003】しかしながら、この方法を工業的規模で実
施するためには、大量の晶析溶媒を使用しなければなら
ず、設備も大型化し、経済的でない。また、晶析から乾
燥までに長時間を要する。However, in order to carry out this method on an industrial scale, it is necessary to use a large amount of crystallization solvent, and the equipment is also large-sized, making it uneconomical. Moreover, it takes a long time from crystallization to drying.
【0004】乾燥までの時間を短縮するために、特開昭
58−79501号公報および同60−90001号公
報に、長管型蒸気加熱管を用いた方法が開示されてる。
この方法は、揮発成分と難揮発成分とを含む原液を長管
型蒸気加熱管内に供給して揮発成分を蒸発させ、得られ
た難揮発成分を冷却粉砕機に連続的に供給して難揮発成
分を冷却・固化および粉砕しつつ、さらに難揮発成分中
の揮発成分を蒸発させものである。[0004] In order to shorten the time required for drying, Japanese Unexamined Patent Publications Nos. 58-79501 and 60-90001 disclose a method using a long steam heating tube. In this method, a stock solution containing volatile components and non-volatile components is supplied into a long steam heating tube to evaporate the volatile components, and the obtained non-volatile components are continuously supplied to a cooling grinder to evaporate the non-volatile components. While cooling, solidifying, and pulverizing the components, volatile components in the non-volatile components are further evaporated.
【0005】また、特開平2−191501号公報には
、長管型蒸気加熱管を用いた乾燥により、重合体溶液か
ら粉末状の重合体を得る方法が開示されている。この方
法は、該加熱管に供給する重合体溶液の粘性を予め特定
の粘度に調整している。Furthermore, JP-A-2-191501 discloses a method for obtaining a powdery polymer from a polymer solution by drying using a long steam heating tube. In this method, the viscosity of the polymer solution supplied to the heating tube is adjusted in advance to a specific viscosity.
【0006】しかしながら、上気長管型蒸気加熱管を用
いた方法は、乾燥しようとする溶液が25℃以下でガラ
ス状態にある場合、その溶液から所定物質を固化状態で
得ることができないか、非常に困難であることがわかっ
た。However, when the solution to be dried is in a glass state at 25° C. or lower, the method using an upper long tube type steam heating tube may not be able to obtain the desired substance in a solidified state from the solution, or may be extremely difficult to obtain. proved to be difficult.
【0007】なお、特公昭61−14777号公報は、
キャンデーを作る方法であるが、減圧下、130℃程度
の温度で原料を濃縮した後、80〜85℃に冷却して固
化させる方法を開示している。しかしながら、この方法
も、上記のようなガラス状態にある溶液から所定の物質
を固化状態で得ることができない。[0007] In addition, Japanese Patent Publication No. 14777/1983 states that
As a method for making candy, the patent discloses a method in which raw materials are concentrated at a temperature of about 130°C under reduced pressure, and then cooled to 80 to 85°C to solidify. However, even with this method, it is not possible to obtain a predetermined substance in a solidified state from a solution in a glassy state as described above.
【0008】[0008]
【発明が解決しようとする課題】従って、本発明の課題
は、常温で固体の物質をそのガラス状態にある溶液から
比較的容易かつ短時間に固化させることができる固化方
法および装置を提供することである。SUMMARY OF THE INVENTION Therefore, it is an object of the present invention to provide a solidification method and apparatus that can relatively easily and quickly solidify a substance that is solid at room temperature from its glassy solution. It is.
【0009】[0009]
【課題を解決するための手段および作用】上記課題を解
決するために、本発明は、常温で固体の有機化合物、お
よびこれに対して1〜50重量%の該有機化合物に対す
る溶剤を含有する混合物を−10℃〜50℃に保ち、こ
れに該有機化合物の種晶を1〜20重量%の割合で加え
て混合し、該有機化合物を固化させることを特徴とする
有機化合物の固化方法を提供する。[Means and effects for solving the problems] In order to solve the above problems, the present invention provides a mixture containing an organic compound that is solid at room temperature and a solvent for the organic compound in an amount of 1 to 50% by weight. Provided is a method for solidifying an organic compound, which comprises maintaining the organic compound at -10°C to 50°C, adding and mixing seed crystals of the organic compound at a ratio of 1 to 20% by weight, and solidifying the organic compound. do.
【0010】上記方法において、有機化合物の溶液を長
管型蒸気加熱管に供給し、該加熱管内で生じた該有機化
合物の濃厚溶液と気体との混合物を減圧雰囲気内に噴出
させ、得られた該濃厚溶液に該有機化合物の種晶を加え
る。In the above method, a solution of an organic compound is supplied to a long steam heating tube, and a mixture of a concentrated solution of the organic compound and a gas generated in the heating tube is ejected into a reduced pressure atmosphere. Seed crystals of the organic compound are added to the concentrated solution.
【0011】また、本発明によれば、常温で固体の有機
化合物の溶液を供給するための手段、該供給手段に接続
され、該有機化合物の濃厚溶液を生成させるための長管
型蒸気加熱管、該加熱管の該供給手段の接続端とは異な
る端部に接続され、該濃厚溶液を減圧下に受容するため
の減圧状態にし得る容器、該容器の底部に接続され、該
減圧状態を維持しつつ該濃厚溶液を取り出すための手段
、および取り出された濃厚溶液に該有機化合物の種晶を
供給した後、常圧下で混合するための手段を備えた有機
化合物の固化装置が提供される。以下、本発明をさらに
詳しく説明する。Further, according to the present invention, there is provided a means for supplying a solution of an organic compound that is solid at room temperature, and a long steam heating tube connected to the supply means for producing a concentrated solution of the organic compound. , a container connected to an end of the heating tube different from the connecting end of the supply means and capable of being brought into a reduced pressure state for receiving the concentrated solution under reduced pressure; connected to the bottom of the container and maintaining the reduced pressure state; An apparatus for solidifying an organic compound is provided, which includes means for taking out the concentrated solution, and means for supplying seed crystals of the organic compound to the taken out concentrated solution and then mixing under normal pressure. The present invention will be explained in more detail below.
【0012】本発明者らは、写真用素材である下記化1
に示す式(1)で表わされるイエローカプラーA(以下
、YCp−A)や下記化2に示す式(2)で表わされる
イエローカプラーB(以下、YCp−B)等常温(25
℃)で固体の有機化合物の溶液を長管型蒸気加熱管を用
いて乾燥固化させようと試みたところ、有機化合物は、
濃縮された状態ではあるが、なお高粘性の濃厚溶液の形
態にあり(これらの溶液は、常温で1万ないし10万セ
ンチポイズ(cp)の粘度を示し、蜂蜜状でありほとん
ど流動しない)、固体状態では得られなかった。[0012] The present inventors have discovered the following chemical formula 1, which is a photographic material.
At room temperature (25
When an attempt was made to dry and solidify a solution of a solid organic compound using a long steam heating tube, the organic compound was
Although concentrated, they are still in the form of highly viscous concentrated solutions (these solutions have a viscosity of 10,000 to 100,000 centipoise (cp) at room temperature, are honey-like and hardly flowable), and are solids. could not be obtained in this condition.
【0013】[0013]
【化1】[Chemical formula 1]
【0014】[0014]
【化2】[Case 2]
【0015】そこで、このような濃縮された濃厚溶液の
形態にある有機化合物を固化させる方法について鋭意研
究した結果、該濃縮溶液を−10℃ないし50℃の温度
に保ち、これに当該有機化合物の種晶を1ないし20重
量%の割合で加えた後、混合することにより、該有機化
合物を比較的短時間で固化(例えば、結晶として析出)
させることができることを見い出し、本発明を完成する
に至った。[0015] Therefore, as a result of intensive research on a method for solidifying such a concentrated organic compound in the form of a concentrated solution, the concentrated solution was kept at a temperature of -10°C to 50°C, and the organic compound was added to the concentrated solution. By adding seed crystals at a ratio of 1 to 20% by weight and mixing, the organic compound can be solidified (for example, precipitated as crystals) in a relatively short time.
The present inventors have discovered that it is possible to do this, and have completed the present invention.
【0016】本発明は、ガラス転移点が常温(25℃)
以下の、有機化合物の濃厚溶液から比較的短時間(例え
ば、種晶を添加後1時間以内)で有機化合物を結晶化さ
せることができる。有機化合物としては、上記YCp−
A、YCp−B等の写真用カプラーや、色材等の写真用
素材の他、有機化合物一般を使用できる。[0016] The present invention has a glass transition point of room temperature (25°C).
An organic compound can be crystallized from a concentrated solution of the organic compound in a relatively short period of time (for example, within 1 hour after adding seed crystals). As the organic compound, the above YCp-
In addition to photographic couplers such as A and YCp-B and photographic materials such as colorants, organic compounds in general can be used.
【0017】本発明において、有機化合物の濃厚溶液中
の溶媒濃度は、有機化合物に対し1ないし50重量%で
あり、この範囲を逸脱すると、本発明の効果が得られな
い。好ましい溶媒濃度は、1.5ないし15重量%であ
り、さらに好ましくは2ないし10重量%である。In the present invention, the concentration of the solvent in the concentrated solution of the organic compound is 1 to 50% by weight based on the organic compound, and if it deviates from this range, the effects of the present invention cannot be obtained. A preferred solvent concentration is 1.5 to 15% by weight, more preferably 2 to 10% by weight.
【0018】このような濃縮形態にある粘稠な有機化合
物溶液(例えば、粘度10〜1000cp)は、反応溶
液等の有機化合物溶液中の溶媒濃度が上記範囲内にあれ
ばこれをそのまま使用することができる。しかしながら
、通常、反応溶液中の溶媒濃度は、上記範囲よりも高い
濃度にあり、これを濃縮することが望ましい。この濃縮
には、長管型蒸気加熱管を用いることが好ましい。すな
わち、水蒸気で加熱された長管型加熱管に一端から反応
溶液を供給する。加熱管内では、溶媒が気化し、残存す
る有機化合物の濃縮溶液と溶媒蒸気との混合物が生じ、
これを加熱管の他端から減圧雰囲気内に噴出させると、
有機化合物の濃縮溶液が得られる。[0018] Such a viscous organic compound solution in a concentrated form (for example, viscosity 10 to 1000 cp) can be used as is if the solvent concentration in the organic compound solution such as the reaction solution is within the above range. Can be done. However, the solvent concentration in the reaction solution is usually higher than the above range, and it is desirable to concentrate this. It is preferable to use a long steam heating tube for this concentration. That is, the reaction solution is supplied from one end to a long heating tube heated with steam. In the heating tube, the solvent evaporates, forming a mixture of concentrated solution of the remaining organic compound and solvent vapor,
When this is injected into the reduced pressure atmosphere from the other end of the heating tube,
A concentrated solution of organic compounds is obtained.
【0019】上記長管型蒸気加熱管としては、例えば、
実公昭52−28862号に記載されているような、公
知の二重加熱管を使用することができる。この二重加熱
管の有機化合物溶液が通過する内管は、内径に対する長
さの比が、好ましくは100ないし10,000、特に
好ましくは500ないし2,000のものである。内管
の内径は、通常、3ないし50mm、好ましくは、10
ないし25mmである。この内管を覆う外管は、これを
加熱するための蒸気を通じることができる形状であれば
、任意のものが使用できる。典型的には、外管は、内管
と同心配置された円筒である。加熱に使用する水蒸気と
しては、固化すべき有機化合物が常温以下でガラス状態
にあるので、50ないし100℃の低圧スチームを使用
することが好ましい。このような低圧スチームの発生方
法に特に制限はない。例えば、特開昭60−64108
号公報に記載された方法によって低圧スチームを発生さ
せることができる。[0019] Examples of the long steam heating tube include:
A known double heating tube, such as that described in Utility Model Publication No. 52-28862, can be used. The inner tube of the double heating tube through which the organic compound solution passes preferably has a length to inner diameter ratio of 100 to 10,000, particularly preferably 500 to 2,000. The inner diameter of the inner tube is usually 3 to 50 mm, preferably 10 mm.
The length is between 25mm and 25mm. Any shape can be used for the outer tube that covers the inner tube as long as it can pass the steam for heating the outer tube. Typically, the outer tube is a cylinder arranged concentrically with the inner tube. As the steam used for heating, it is preferable to use low pressure steam of 50 to 100° C., since the organic compound to be solidified is in a glass state at room temperature or lower. There are no particular restrictions on the method of generating such low pressure steam. For example, JP-A-60-64108
Low pressure steam can be generated by the method described in the publication.
【0020】長管型蒸気加熱管の他端は、減圧雰囲気に
、具体的には、減圧を達成・維持できる容器(減圧容器
)に接続されている。長管型蒸気加熱管中で生成した溶
媒蒸気を含む気体と有機化合物濃縮溶液とは、この減圧
容器内に噴出され、減圧容器内に有機化合物の濃縮溶液
が得られる。この濃縮溶液中の溶媒濃度を上記範囲内に
調整するには、有機化合物溶液の加熱管への供給速度、
蒸気による加熱温度、および/または加熱管中での滞留
時間等の条件を適宜調節することができる。これらの条
件は、予備実験により容易に決定できる。The other end of the long steam heating tube is connected to a reduced pressure atmosphere, specifically to a container capable of achieving and maintaining reduced pressure (reduced pressure container). The gas containing the solvent vapor and the concentrated organic compound solution generated in the long steam heating tube are ejected into the vacuum container, and a concentrated solution of the organic compound is obtained in the vacuum container. In order to adjust the solvent concentration in this concentrated solution within the above range, the feeding rate of the organic compound solution to the heating tube,
Conditions such as the heating temperature by steam and/or the residence time in the heating tube can be adjusted as appropriate. These conditions can be easily determined through preliminary experiments.
【0021】こうして準備された1ないし50重量%の
溶媒を含有する有機化合物の濃縮溶液は、別の第2の容
器(これも減圧容器であることが取り出しに都合がよい
)に取り出すことができる。取り出し後、第2の容器内
を大気圧に戻し、濃縮溶液を混合容器へ移し、この混合
容器内で−10℃ないし50℃、好ましくは0℃ないし
30℃、さらに好ましくは10ないし25℃の温度に保
ちながら、当該有機化合物の種晶を該有機化合物に対し
て1ないし20重量%の割合で加え、混合する。種晶の
添加量は、好ましくは1.5〜15重量%であり、さら
に好ましくは、2〜10重量%である。この濃縮溶液の
所定温度での保持と、種晶の所定量の添加によって、濃
厚溶液中の有機化合物は、比較的短時間に固化する。
なお、種晶を濃縮溶液に添加し、混合した後、この混合
物を常温に維持された例えばベルト上に放置し、有機化
合物の固化を待つことができる。こうして固化した有機
化合物塊を粉砕機で粉砕し、これを乾燥機でさらに乾燥
し、有機化合物の乾燥粉末を得ることができる。図1に
、本発明を実施するために使用される有機化合物の(濃
縮)固化装置の一例を示す。[0021] The concentrated solution of the organic compound containing 1 to 50% by weight of solvent thus prepared can be taken out into a separate second container (also a vacuum container for convenient removal). . After taking out, the inside of the second container is returned to atmospheric pressure, and the concentrated solution is transferred to a mixing container, where it is heated at -10°C to 50°C, preferably 0°C to 30°C, more preferably 10 to 25°C. While maintaining the temperature, seed crystals of the organic compound are added in a proportion of 1 to 20% by weight based on the organic compound and mixed. The amount of seed crystals added is preferably 1.5 to 15% by weight, more preferably 2 to 10% by weight. By maintaining this concentrated solution at a predetermined temperature and adding a predetermined amount of seed crystals, the organic compound in the concentrated solution is solidified in a relatively short time. Incidentally, after the seed crystals are added to the concentrated solution and mixed, the mixture can be left on, for example, a belt maintained at room temperature to wait for solidification of the organic compound. The thus solidified organic compound mass is pulverized using a pulverizer and further dried using a drier to obtain a dry powder of the organic compound. FIG. 1 shows an example of an organic compound (concentration) solidification apparatus used to carry out the present invention.
【0022】この装置は、長管型蒸気加熱二重管4を水
平に配置して備えている。加熱管4近傍には、これを熱
するための低圧スチームを発生する発生装置5が設けら
れており、ここで発生したスチームは、加熱管4の外管
内に循環して通じられる。[0022] This device is equipped with a long steam heating double pipe 4 arranged horizontally. A generator 5 that generates low-pressure steam for heating the heating tube 4 is provided near the heating tube 4, and the steam generated here is circulated into the outer tube of the heating tube 4.
【0023】加熱管4の一端は、ラインL1により、定
量供給ポンプ3を介して反応溶液等の原液を収容するた
めの溶液収容タンク1の底部に接続している。タンク1
は、有機化合物を製造した反応タンクであり得る。原液
は、タンク1に付設され、モーターMにより駆動される
撹拌装置2により撹拌され、定量供給ポンプ3により所
定の割合で加熱管4に供給される。One end of the heating tube 4 is connected via a metering pump 3 to the bottom of a solution storage tank 1 for storing a stock solution such as a reaction solution through a line L1. tank 1
can be the reaction tank in which the organic compound was produced. The stock solution is stirred by a stirring device 2 attached to the tank 1 and driven by a motor M, and is supplied to the heating tube 4 at a predetermined rate by a quantitative supply pump 3.
【0024】加熱管4の他端は、加熱管4中で発生した
気体と濃縮濃厚溶液との混合物を噴出させるための減圧
雰囲気を達成する減圧容器6の上部に、ラインL2によ
り、接続している。減圧容器6は、モーターMにより駆
動される撹拌装置7を備え、またその周囲には、容器全
体を外温から保温するためのジャケット8を設けること
ができる。The other end of the heating tube 4 is connected by a line L2 to the upper part of a vacuum container 6 which achieves a reduced pressure atmosphere for blowing out the mixture of gas and concentrated concentrated solution generated in the heating tube 4. There is. The reduced pressure container 6 is equipped with a stirring device 7 driven by a motor M, and a jacket 8 can be provided around the stirring device 7 to keep the entire container warm from the outside temperature.
【0025】減圧容器6の頂部には、ラインをL3介し
て、減圧発生装置12が接続しており、これにより、減
圧容器6内は、減圧状態に保たれる。ラインL3には、
装置上流側から順に、溶媒蒸気凝縮器9、およびこの凝
縮器9により凝縮された溶媒を収容するための溶媒受け
タンク10が設けられている。溶媒受けタンク10の周
囲にも保温ジャケット11を設けることができる。また
、溶媒受けタンク10の底部には、溶媒抜き出しポンプ
13が接続している。A reduced pressure generating device 12 is connected to the top of the reduced pressure container 6 via a line L3, thereby maintaining the inside of the reduced pressure container 6 in a reduced pressure state. On line L3,
A solvent vapor condenser 9 and a solvent receiving tank 10 for accommodating the solvent condensed by the condenser 9 are provided in order from the upstream side of the apparatus. A heat insulation jacket 11 can also be provided around the solvent receiving tank 10. Further, a solvent extraction pump 13 is connected to the bottom of the solvent receiving tank 10.
【0026】減圧容器6の底部は、弁14を介して、第
2の減圧容器15と接続している。この減圧容器15は
、減圧容器6内の濃縮溶液を受けるものであり、その周
囲に、冷却または保温ジャケット16を設けることがで
きる。減圧容器15の頂部には、ラインL4を介して、
第2の減圧発生装置17が接続しており、これにより減
圧容器15内は、減圧状態に保たれる。減圧容器15で
所定量の濃縮溶液を受けた後、減圧容器15を大気圧に
戻し、容器15の底部に設けられた弁17を開き、ライ
ンL5を介して、濃縮溶液を、混合容器18に移す。The bottom of the reduced pressure container 6 is connected to a second reduced pressure container 15 via a valve 14. This reduced pressure container 15 receives the concentrated solution in the reduced pressure container 6, and a cooling or heat insulation jacket 16 can be provided around it. At the top of the reduced pressure container 15, via a line L4,
A second reduced pressure generator 17 is connected, thereby maintaining the inside of the reduced pressure container 15 in a reduced pressure state. After receiving a predetermined amount of the concentrated solution in the reduced pressure container 15, the reduced pressure container 15 is returned to atmospheric pressure, the valve 17 provided at the bottom of the container 15 is opened, and the concentrated solution is transferred to the mixing container 18 via the line L5. Move.
【0027】混合容器18は、モーターMで駆動される
撹拌機19を有し、頂部には、種晶を導入添加するため
の導入口20が設けられている。混合容器18の周囲に
は、その内容物(濃縮有機化合物溶液)を所定の温度に
維持するための保温ジャケット21を付設することがで
きる。この混合容器18内の濃縮溶液に導入口20から
所定量の種晶を添加し、この混合物を撹拌機19で撹拌
する。The mixing vessel 18 has a stirrer 19 driven by a motor M, and has an inlet 20 at the top for introducing and adding seed crystals. A heat insulating jacket 21 can be attached around the mixing container 18 to maintain its contents (concentrated organic compound solution) at a predetermined temperature. A predetermined amount of seed crystals is added to the concentrated solution in the mixing container 18 from the inlet 20, and the mixture is stirred by the stirrer 19.
【0028】混合容器18の下方には、一対のドラム2
3,23により適宜駆動される水平無端ベルト22が設
置されている。このベルト22は、冷却水が循環する冷
却ジャケット24により例えば常温に保たれる。混合容
器18内で撹拌された濃縮溶液と種晶との混合物は、混
合容器18からドラム23,23により回転されるベル
ト22上に例えば2〜4cmの厚さに広げられ、ベルト
移動方向先端の混合物が上部ベルトの水平先端に位置し
た時点でドラム23,23の回転と混合物の供給を停止
し、混合物をベルト22上に放置し、有機化合物の固化
を待つ。A pair of drums 2 are provided below the mixing container 18.
A horizontal endless belt 22 is installed which is appropriately driven by belts 3 and 23. This belt 22 is kept at room temperature, for example, by a cooling jacket 24 through which cooling water circulates. The mixture of the concentrated solution and the seed crystals stirred in the mixing container 18 is spread from the mixing container 18 onto the belt 22 rotated by the drums 23, 23 to a thickness of, for example, 2 to 4 cm. When the mixture reaches the horizontal tip of the upper belt, the rotation of the drums 23 and the supply of the mixture are stopped, and the mixture is left on the belt 22 to wait for the organic compound to solidify.
【0029】固化した有機化合物は、ドラム23,23
の回転駆動により、ベルト22から粉砕機25(例えば
、一対の歯車)に導入され、ここで粉砕される。得られ
た有機化合物粉末は、加熱ジャケット27を有する乾燥
機26に移され、ここで、有機化合物粉末は、さらに乾
燥され、生じた溶媒蒸気は、排出口27から排出される
。The solidified organic compound is transferred to drums 23, 23.
is introduced from the belt 22 into a crusher 25 (for example, a pair of gears), where it is crushed. The obtained organic compound powder is transferred to a dryer 26 having a heating jacket 27, where the organic compound powder is further dried and the resulting solvent vapor is discharged through an outlet 27.
【0030】[0030]
【実施例】実施例 1
この実施例では、図1に示した装置を用い、YCp−A
の溶液から、固化したYCp−Aを得た。[Example] Example 1 In this example, YCp-A
Solidified YCp-A was obtained from the solution.
【0031】すなわち、タンク1内で製造され、精製さ
れたYCp−A100kgとメチレンクロリド500リ
ットルの溶液を、定量ポンプ3により加熱管4に供給し
、その中でメチレンクロリドを蒸発させ、減圧容器6内
に噴出させ、YCp−Aに対するメチレンクロリドの割
合が10重量%まで濃縮された濃縮溶液を約90℃で得
た。この濃縮溶液は、粘度500〜1,000cpの高
粘液であった。That is, a solution of 100 kg of YCp-A produced and purified in the tank 1 and 500 liters of methylene chloride is supplied to the heating tube 4 by the metering pump 3, and the methylene chloride is evaporated therein. A concentrated solution in which the ratio of methylene chloride to YCp-A was concentrated to 10% by weight was obtained at about 90°C. This concentrated solution was a highly viscous liquid with a viscosity of 500 to 1,000 cp.
【0032】上記濃縮溶液を減圧容器6から第2の減圧
容器15に移した後、容器15内を大気圧に戻し、弁1
7を開いて、内容物を混合容器18に移した。この混合
容器18内で、濃縮溶液の温度は、40〜60℃であっ
た。ついで、濃縮溶液中のYCp−Aに対して7重量%
相当のYCp−A種晶を添加し、撹拌機19で約5分間
混合した後、ベルト22上に約2〜4cmの厚さに広げ
た。ベルトは、冷却ジャケット24により25℃に維持
した。ベルト22上に1時間放置したところ、YCp−
Aは固化した。固化したYCp−Aを粉砕機25で粉砕
し、乾燥装置26中でさらに乾燥して粉末製品とした。
実施例 2
YCp−Aの代りに、YCp−Bを用いた以外は、実施
例1と全く同様の操作をおこない、同様にYCp−Bの
粉末を得た。After transferring the concentrated solution from the vacuum container 6 to the second vacuum container 15, the inside of the container 15 is returned to atmospheric pressure, and the valve 1 is closed.
7 was opened and the contents were transferred to mixing vessel 18. In this mixing vessel 18, the temperature of the concentrated solution was 40-60°C. Then, 7% by weight based on YCp-A in the concentrated solution
A corresponding amount of YCp-A seeds were added and mixed for about 5 minutes with a stirrer 19 before being spread on belt 22 to a thickness of about 2-4 cm. The belt was maintained at 25°C by a cooling jacket 24. When left on the belt 22 for 1 hour, YCp-
A was solidified. The solidified YCp-A was pulverized by a pulverizer 25 and further dried in a drying device 26 to obtain a powder product. Example 2 A powder of YCp-B was obtained in the same manner as in Example 1 except that YCp-B was used instead of YCp-A.
【0033】[0033]
【発明の効果】以上述べたように、本発明によれば、そ
の濃厚溶液のガラス転移点が25℃以下と低く、常温で
高粘度をとりやすい物質であっても、この濃厚溶液から
これを比較的容易かつ短時間に固化させることができる
。ちなみに、反応液から晶析、乾燥により粉末を得る従
来方法に比べて、本発明の方法は、その時間が1/2〜
1/10に短縮される。また、従来の晶析法では、反応
生成物が、5%以上、通常は10%以上も損失するのに
対し、本発明では、反応液から反応生成物を損失無く回
収できる。As described above, according to the present invention, even if the concentrated solution has a low glass transition point of 25°C or lower and tends to have a high viscosity at room temperature, it can be removed from the concentrated solution. It can be solidified relatively easily and in a short time. Incidentally, compared to the conventional method of obtaining powder from a reaction solution by crystallization and drying, the method of the present invention takes 1/2 to 1/2 the time.
It will be shortened to 1/10. Furthermore, in the conventional crystallization method, the reaction product is lost by 5% or more, usually by 10% or more, whereas in the present invention, the reaction product can be recovered from the reaction solution without loss.
【図1】本発明の一実施例による有機化合物の固化装置
の概略図。FIG. 1 is a schematic diagram of an organic compound solidification apparatus according to an embodiment of the present invention.
1…溶液タンク、2,7,19…撹拌装置、4…長管型
蒸気加熱管、5…減圧スチーム発生装置、6,15…減
圧容器、12,17…減圧発生装置、18…混合容器、
22…ベルト、25…粉砕機。DESCRIPTION OF SYMBOLS 1... Solution tank, 2, 7, 19... Stirring device, 4... Long steam heating tube, 5... Reduced pressure steam generator, 6, 15... Reduced pressure container, 12, 17... Reduced pressure generator, 18... Mixing container,
22...Belt, 25...Crusher.
Claims (3)
に対して1〜50重量%の該有機化合物に対する溶剤を
含有する混合物を−10℃〜50℃に保ち、これに該有
機化合物の種晶を1〜20重量%の割合で加えて混合し
、該有機化合物を固化させることを特徴とする有機化合
物の固化方法。Claim 1: A mixture containing an organic compound that is solid at room temperature and a solvent for the organic compound in an amount of 1 to 50% by weight is kept at -10°C to 50°C, and seed crystals of the organic compound are added to the mixture. A method for solidifying an organic compound, which comprises adding and mixing 1 to 20% by weight of the organic compound to solidify the organic compound.
型蒸気加熱管に供給し、該加熱管内で生じた該有機化合
物の濃厚溶液と気体との混合物を減圧雰囲気内に噴出さ
せ、得られた該濃厚溶液に該有機化合物の種晶を加える
ことを特徴とする請求項1記載の有機化合物の固化方法
。2. A solution of an organic compound that is solid at room temperature is supplied to a long steam heating tube, and a mixture of a concentrated solution of the organic compound and a gas generated in the heating tube is spouted into a reduced pressure atmosphere. 2. The method for solidifying an organic compound according to claim 1, further comprising adding seed crystals of the organic compound to the concentrated solution.
するための手段、該供給手段に接続され、該有機化合物
の濃厚溶液を生成させるための長管型蒸気加熱管、該加
熱管の該供給手段の接続端とは異なる端部に接続され、
該濃厚溶液を減圧下に受容するための減圧状態にし得る
容器、該容器の底部に接続され、該減圧状態を維持しつ
つ該濃厚溶液を取り出すための手段、および取り出され
た濃厚溶液に該有機化合物の種晶を供給した後、常圧下
で混合するための手段を備えた有機化合物の固化装置。3. A means for supplying a solution of an organic compound that is solid at room temperature; a long steam heating tube connected to the supply means for producing a concentrated solution of the organic compound; connected to an end different from the connecting end of the supply means,
a container capable of being placed under reduced pressure for receiving the concentrated solution under reduced pressure; means connected to the bottom of the container for removing the concentrated solution while maintaining the reduced pressure; and means for removing the concentrated solution while maintaining the reduced pressure; An apparatus for solidifying organic compounds, comprising means for feeding seed crystals of the compound and then mixing under normal pressure.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP1893491A JPH04257527A (en) | 1991-02-12 | 1991-02-12 | Solidification of organic compound and equipment therefor |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP1893491A JPH04257527A (en) | 1991-02-12 | 1991-02-12 | Solidification of organic compound and equipment therefor |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH04257527A true JPH04257527A (en) | 1992-09-11 |
Family
ID=11985475
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP1893491A Pending JPH04257527A (en) | 1991-02-12 | 1991-02-12 | Solidification of organic compound and equipment therefor |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH04257527A (en) |
-
1991
- 1991-02-12 JP JP1893491A patent/JPH04257527A/en active Pending
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