JP6255649B2 - Continuous reaction crystallization apparatus and inorganic particle continuous reaction crystallization method - Google Patents
Continuous reaction crystallization apparatus and inorganic particle continuous reaction crystallization method Download PDFInfo
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Description
本発明は、接触処理液を循環させ、反応を行う連続反応晶析装置及び無機粒子の連続反応晶析方法に関する。 The present invention relates to a continuous reaction crystallization apparatus for circulating a contact treatment solution and performing a reaction, and a continuous reaction crystallization method for inorganic particles.
液液反応、気液反応又は触媒反応などの反応によって、あるいは晶析処理により粒子を生成させるなど、工業的な処理を経て製品又は中間品を得る操作としては限りなく多くある。 There are an unlimited number of operations for obtaining a product or an intermediate product through industrial treatment such as liquid-liquid reaction, gas-liquid reaction, catalytic reaction, or the like, or generation of particles by crystallization treatment.
代表的な処理は、たとえば図１２に示すように、Ａ成分、Ｂ成分あるいはＣ成分を撹拌接触処理槽１内に投入し、攪拌モータ２付き攪拌羽根３により攪拌し、各成分の反応を促進させるのが一般的である。適宜の時点で、排出口５から成品液を抜き出し、その後、たとえば濾過、洗浄及び乾燥により目的の晶析粒子を得る。４はバッフルである。 For example, as shown in FIG. 12, for example, A component, B component or C component is put into stirring contact treatment tank 1 and stirred by stirring blade 3 with stirring motor 2 to promote the reaction of each component. It is common to make it. At an appropriate time, the product liquid is withdrawn from the discharge port 5, and then target crystallized particles are obtained by, for example, filtration, washing and drying. 4 is a baffle.
しかし、この処理形態では、接触処理槽１として大きなものを必要とし、均一な反応や処理のために攪拌羽根３により攪拌しているが、高い均一性を期待するのに限界がある。
他方、処理方法として、各成分の接触処理槽１内への投入及びその後の撹拌をバッチ式で処理する場合には、生産効率が悪い。したがって、撹拌中に連続的に各成分を投入する連続生産方式が高い効率が得られるが、接触処理の条件設定（対時間での投入量コントロールなど）が難しく、必ずしも均一な製品を効率良く得ることができるものでもない。
これらを改善する試みとして、流路を１ｍｍ以下にしたマイクロリアクターが提唱されているが、生産量が乏しく流路の閉塞による連続生産の不具合が指摘されており、工業規模での実用化事例は少ない。
However, in this processing mode, a large contact processing tank 1 is required and stirring is performed by the stirring blade 3 for uniform reaction and processing, but there is a limit to expecting high uniformity.
On the other hand, as a processing method, when each component is charged into the contact processing tank 1 and then stirred, the production efficiency is poor. Therefore, the continuous production method in which each component is continuously added during stirring can provide high efficiency, but it is difficult to set the conditions for contact treatment (such as controlling the amount of input over time), and a uniform product can always be obtained efficiently. It is not something that can be done.
As an attempt to improve these, a microreactor with a flow path of 1 mm or less has been proposed, but the production volume is low and problems with continuous production due to blockage of the flow path have been pointed out. Few.
成分をサイクロン方式で移動させる過程で他の成分と接触させる技術は、特許文献１に記載されている。 Patent Document 1 discloses a technique for bringing a component into contact with another component in the process of moving the component in a cyclone system.
しかし、先行技術は、成分の分離技術であって、反応や処理を目的にしたものではない。 However, the prior art is a component separation technique and is not intended for reaction or treatment.
化学工業界をはじめとする接触処理分野において、小型の処理装置でありながら、十分な処理量を発揮し、しかも均一な接触処理性を示す反応装置が求める要望は大きい。 In the contact processing field including the chemical industry, there is a great demand for a reaction apparatus that exhibits a sufficient throughput while exhibiting a uniform contact processability even though it is a small processing apparatus.
したがって、本発明の主たる課題は、小型の処理装置でありながら、十分な処理量を発揮し、しかも均一な接触処理性を示す反応晶析装置及び無機粒子の連続反応晶析方法を提供することにある。 Accordingly, the main object of the present invention is to provide a reaction crystallizer and a continuous reaction crystallization method of inorganic particles that exhibit a sufficient throughput while exhibiting a uniform contact processability even though they are small processing apparatuses. It is in.
この課題を解決した本発明は、次の通りである。
〔請求項１記載の発明〕
一方端部及び他方端部を有する反応器と、この反応器内に無機物質を含む反応液を注入する注入手段と、前記反応器の前記他方端部から接触処理液を抜き出して、抜き出した接触処理液の少なくとも一部を、液流れ変換器を介して、前記反応器の前記一方端部へ返送する循環手段とを有し、
前記液流れ変換器は、流れ中心線回りの旋回流を生成させる旋回流生成器であり、
前記反応器内の液流れを前記接触処理液の返送により前記他方端部に向かう旋回流とし、前記注入手段により反応液を、前記反応器の内表面より中心側位置に注入し、前記旋回流と接触させるよう構成されており、
前記液流れ変換器は、直線的液流れを半径方向の乱れを伴った液流れに変換するものであることを特徴とする無機粒子の連続反応晶析装置。
The present invention that has solved this problem is as follows.
[Invention of Claim 1]
A reactor having one end and the other end; an injection means for injecting a reaction liquid containing an inorganic substance into the reactor; and a contact treatment liquid extracted from the other end of the reactor. A circulation means for returning at least a part of the processing liquid to the one end of the reactor via a liquid flow converter;
The liquid flow converter is a swirl flow generator that generates a swirl flow around a flow center line,
The liquid flow in the reactor is turned into a swirl flow toward the other end by returning the contact treatment liquid, the reaction liquid is injected into the central position from the inner surface of the reactor by the injection means, and the swirl flow Configured to come into contact with
The said liquid flow converter converts a linear liquid flow into the liquid flow accompanied by the disturbance of a radial direction, The continuous reaction crystallization apparatus of the inorganic particle characterized by the above-mentioned.
（作用効果）
液流れとして旋回流を示す場においては、竜巻のように中心の渦部分あるいは中心の空洞部分近傍の内周部分の流れは、反応を左右する物質移動・攪拌混合効果が高いなど流れの乱れが大きい。この部分は、注入する反応物質もしくはガスを含む注入液の急激な拡散場となり、均質な反応が可能となる。
さらに、流路の壁面には旋回流の外周部分が接しているので、外周の旋回流が反応物質の供給体となり、物質・熱の急激な変化を和らげている。注入した注入物質（液・ガス・固形物）の反応物質に対してバリヤー（障壁）として機能するために、反応物質の反応器内面及び流路内面への付着が防止され、長時間にわたり安定した運転が可能となるものと考えられる
当初、本発明者は、小型の処理装置でありながら、十分な処理量を発揮する装置として、チューブリアクターを使用する反応処理装置の開発を試みた。しかし、ある種の反応処理材料系では、流路の壁面に微細なシャワー（一次核）が付着し、その後にこれを核として結晶が成長し、流れを阻害し、長時間の安定した運転ができ難いケースが散見された。
(Function and effect)
In a field that shows a swirling flow as a liquid flow, the flow in the central vortex part or the inner peripheral part in the vicinity of the central cavity part like a tornado has a disturbed flow such as high mass transfer / stirring mixing effect that affects the reaction. large. This portion becomes an abrupt diffusion field of the injection solution containing the reactant or gas to be injected, and a homogeneous reaction is possible.
Furthermore, since the outer peripheral portion of the swirl flow is in contact with the wall surface of the flow path, the swirl flow on the outer periphery serves as a reactant supply body, and abrupt changes in material and heat are mitigated. Since it functions as a barrier against the reactants of the injected injection material (liquid, gas, solid), it prevents the reactant from adhering to the inner surface of the reactor and the inner surface of the flow path and is stable for a long time The present inventor tried to develop a reaction processing apparatus that uses a tube reactor as an apparatus that exhibits a sufficient throughput even though it is a small processing apparatus. However, in certain types of reaction processing material systems, fine showers (primary nuclei) adhere to the walls of the flow channel, and then crystals grow from this as the nuclei, blocking the flow and long-term stable operation. Some cases were difficult to do.
その対策として、反応径路を並設し、詰まりが発生したならば、他方の反応経路に切換えて流通させ、その間に詰まりが生じた反応経路は清浄する方策が考えられる。しかし、切換えの僅かな時間においても、接触の場における、不連続運転に起因した粒径の変動を避けるべきであり、長時間にわたり安定した運転に耐えるべく新たな機構が必要と判断した。 As a countermeasure, it is conceivable to arrange reaction paths in parallel and, if clogging occurs, switch to the other reaction path for circulation, and clean the reaction path in which clogging occurred. However, it was judged that a change in particle size due to discontinuous operation should be avoided even in a short time of switching, and that a new mechanism was necessary to withstand stable operation over a long period of time.
これに対し、本発明に従って、反応器内の液流れを、接触処理液の返送による旋回流とし、この旋回流に対して注入手段により注入した反応液と接触させるよう構成したことにより前記課題を解決できることが知見された。 On the other hand, according to the present invention, the liquid flow in the reactor is a swirl flow by returning the contact treatment liquid, and the swirl flow is brought into contact with the reaction liquid injected by the injection means. It was found that this could be solved.
他方、反応器へ返送する接触処理液の入口部分に液流れ変換器を設け、この液流れ変換器により、直線的液流れを半径方向の乱れを伴った液流れに変換したうえで、反応器に返送すると、液流れ変換器を設けない場合に比較して、反応器内の旋回流がより複雑な流れとなり、外部から注入する粒子の拡散効果が大きくなり、反応性が高まり、しかも、粒子及び粒子の凝集体の回転が大きくなることにより、球形の粒子の生成率が高まり、高い充填密度の粒子を得ることができる。
液流れ変換器は、具体的には、たとえば管内を流れ、変換器内に流入する乱流を、たとえば先窄まりの内面あるいは円筒状内面をもった変換器の接線方向から導き、変換器内で渦を伴った旋回流に変換する、あるいはスタティックミキサーからなる変換器により、その変換器内で渦を伴った捻れ流れに変換するものである。
On the other hand, a liquid flow converter is provided at the inlet portion of the contact treatment liquid to be returned to the reactor, and the liquid flow converter converts the linear liquid flow into a liquid flow with radial disturbance, and then the reactor. In comparison with the case where the liquid flow converter is not provided, the swirl flow in the reactor becomes a more complicated flow, the diffusion effect of particles injected from the outside increases, the reactivity increases, and the particles Further, since the rotation of the particle aggregate increases, the generation rate of spherical particles increases, and particles with a high packing density can be obtained.
More specifically, the liquid flow converter, for example, guides the turbulent flow that flows in the tube and flows into the converter from the tangential direction of the converter having a tapered inner surface or a cylindrical inner surface, for example. It is converted into a swirl flow with a vortex, or is converted into a twisted flow with a vortex in the converter by a converter composed of a static mixer.
〔請求項２記載の発明〕
返送された接触処理液と注入した前記反応液との前記反応器内の接触の場を、前記反応器内に生成された旋回流の反応器の内表面より中心側領域とし、この接触の場において前記反応液の接触を行なわせるようにした請求項１記載の連続反応晶析装置。
[Invention of Claim 2]
The contact field in the reactor between the returned contact treatment liquid and the injected reaction liquid is defined as a region on the center side from the inner surface of the swirling flow reactor generated in the reactor. 2. The continuous reaction crystallization apparatus according to claim 1, wherein the reaction solution is brought into contact with each other.
（作用効果）
反応器に対し液を循環させるとともに、その反応器内に、循環液の返送液を流入させることにより旋回流を生成させると、旋回流の外周部分が反応器内面においてある厚さの筒状体部分を形成する。その結果、筒状体部分が、新たに注入した注入液との反応に対してバリヤー（障壁）として機能する現象が生じ、接触の場を旋回流の反応器の内表面より中心側領域とし、この接触の場において前記反応液の接触を行なわせるようにした。その結果、反応による吸熱・発熱に伴う温度変化の緩和、反応物質の流路内面への付着を防止することができる。
(Function and effect)
When a liquid is circulated through the reactor and a return flow of the circulating liquid is caused to flow into the reactor to generate a swirling flow, a cylindrical body having a thickness where the outer peripheral portion of the swirling flow is on the inner surface of the reactor Forming part. As a result, a phenomenon occurs in which the cylindrical body part functions as a barrier (barrier) against the reaction with the newly injected liquid, and the contact field is set to the central region from the inner surface of the swirling flow reactor. The reaction solution was brought into contact in this contact field. As a result, it is possible to alleviate temperature changes accompanying heat absorption and heat generation due to the reaction and to prevent the reactants from adhering to the inner surface of the flow path.
〔請求項３記載の発明〕
反応器は、その内面が一方端部側から他方端部に向かって先窄まりとなり、接触処理液流入位置が前記反応器の長手方向一方端部である請求項１記載の連続反応晶析装置。
[Invention of Claim 3]
The continuous reaction crystallization apparatus according to claim 1, wherein an inner surface of the reactor is tapered from one end portion toward the other end portion, and a contact treatment liquid inflow position is one end portion in the longitudinal direction of the reactor. .
（作用効果）
反応器は内空間が均一な半径をもつ筒状のものでもよいが、長手方向一方端部側から他方端部に向かって内面が先窄まりとなるものが、旋回流の生成に好適である。
また、反応器としては、旋回流の接触の場を長くするために長手方向に沿ったある程度長い空間を確保することが望ましい。そこで、反応器の長手方向一方端部から液を流入させ、長手方向の他方端部から流出させるのが好適な態様である。
(Function and effect)
The reactor may have a cylindrical shape with a uniform inner radius, but a reactor whose inner surface is tapered from one end to the other end in the longitudinal direction is suitable for generating a swirling flow. .
In addition, it is desirable for the reactor to ensure a certain long space along the longitudinal direction in order to lengthen the contact field of the swirl flow. In view of this, it is a preferred embodiment that the liquid is allowed to flow from one end portion in the longitudinal direction of the reactor and to flow out from the other end portion in the longitudinal direction.
〔請求項４記載の発明〕
前記液流れ変換器は、スタティックミキサーである請求項１記載の連続反応晶析装置。
[Invention of Claim 4 ]
The continuous reaction crystallization apparatus according to claim 1, wherein the liquid flow converter is a static mixer.
（作用効果）
液流れ変換器は、スタティックミキサーであってもよい。
(Function and effect)
The liquid flow transducer may be a static mixer.
〔請求項５記載の発明〕
一方端部及び他方端部を有する反応器と、この反応器内に無機物質を含む反応液を注入する注入手段と、前記反応器の前記他方端部から接触処理液を抜き出して、抜き出した接触処理液の少なくとも一部を、直線的液流れを半径方向の乱れを伴った液流れに変換する液流れ変換器を介して、前記反応器の前記一方端部へ返送する循環手段とを有し、
前記液流れ変換器は、流れ中心線回りの旋回流を生成させる旋回流生成器であり、
前記反応器内の液流れを前記接触処理液の返送により前記他方端部に向かう旋回流とし、前記注入手段により反応液を、前記反応器の内表面より中心側位置に注入し、前記旋回流と接触させて反応を行わせ、
無機粒子の反応晶析を行うことを特徴とする無機粒子の連続反応晶析方法。
[Invention of Claim 5 ]
A reactor having one end and the other end; an injection means for injecting a reaction liquid containing an inorganic substance into the reactor; and a contact treatment liquid extracted from the other end of the reactor. A circulation means for returning at least a part of the processing liquid to the one end of the reactor via a liquid flow converter for converting a linear liquid flow into a liquid flow with a radial disturbance. ,
The liquid flow converter is a swirl flow generator that generates a swirl flow around a flow center line,
The liquid flow in the reactor is turned into a swirl flow toward the other end by returning the contact treatment liquid, the reaction liquid is injected into the central position from the inner surface of the reactor by the injection means, and the swirl flow To react with it,
A method for continuous reaction crystallization of inorganic particles, characterized by performing reaction crystallization of inorganic particles.
（作用効果）
請求項１と同様の作用効果を奏する。
(Function and effect)
There exists an effect similar to Claim 1.
以上のとおり、本発明によれば、小型の処理装置でありながら、十分な処理量を発揮し、しかも均一な接触処理性を示すものとなる等の利点がある。 As described above, according to the present invention, there is an advantage that a sufficient amount of processing can be achieved and a uniform contact processing property can be exhibited while being a small processing apparatus.
次に、本発明を実施するための形態を説明する。
後に説明するように、本発明の適用範囲は広範である。しかし、種々の例を総合的に説明すると、混乱の原因になりかねないので、一例を挙げながら装置例を説明し、後に他の適用範囲について説明することとする。
Next, the form for implementing this invention is demonstrated.
As will be described later, the scope of application of the present invention is wide. However, a comprehensive description of various examples may cause confusion, so an example of the apparatus will be described with an example, and another application range will be described later.
本発明の典型例は、たとえば金属粒子を得るための連続反応晶析装置である。その具体例の一つはＮｉ，Ｃｏの遷移金属を用いた凝集粒子を製造することを対象とするものである。
本発明に従って、注入すべき無機物質を含む注入液を、反応器内の旋回流の接触の場において、反応器の内表面より中心側位置において注入し、接触処理を行なわせる方法は、広く一般に無機物質により凝集粒子を得る場合に適用できるものであるから、前記遷移金属以外の金属や他の無機物質を対象にしてもよい。
A typical example of the present invention is a continuous reaction crystallizer for obtaining metal particles, for example. One specific example is intended to produce aggregated particles using Ni and Co transition metals.
According to the present invention, a method for injecting an injection solution containing an inorganic substance to be injected at a position closer to the center than the inner surface of the reactor in the contact field of the swirling flow in the reactor and performing the contact treatment is generally widely used. Since it can be applied to the case where aggregated particles are obtained from an inorganic substance, metals other than the transition metal and other inorganic substances may be targeted.
図１〜図４は、本発明の第１例を示したもので、反応器１０内の液流れを旋回流とし、注入すべき無機物質を含む注入液を、反応器内１０の接触の場（図２及び図４に概念的に符号Ｑとして示した）において、反応器１０の内表面より中心側位置において注入し、接触処理を行なわせるものである。
図示例では、注入すべき無機物質を含む注入液として、Ａ液、Ｂ液及びＣ液を注入している。図示しないが、併せて並行的にガス（窒素ガスや二酸化炭素ガスなどの不活性ガス）を注入することもできる。
また、本発明の第１例は、注入すべき無機物質を含む注入液の接触の場に対する注入方向が、液の旋回流の下流方向に向いている例である。
図示の反応器１０は横向きであるが、原理的に流れに影響はないため竪向きでもよい。
1 to 4 show a first example of the present invention, in which a liquid flow in the reactor 10 is a swirl flow, and an injection liquid containing an inorganic substance to be injected is contacted in the reactor 10. In FIG. 2 and FIG. 4 conceptually indicated by the symbol Q, the injection is performed at the center side position from the inner surface of the reactor 10 to perform the contact treatment.
In the illustrated example, A liquid, B liquid, and C liquid are injected as an injection liquid containing an inorganic substance to be injected. Although not shown, a gas (inert gas such as nitrogen gas or carbon dioxide gas) can be injected in parallel.
Further, the first example of the present invention is an example in which the injection direction with respect to the contact field of the injection liquid containing the inorganic substance to be injected is directed to the downstream direction of the swirling flow of the liquid.
Although the illustrated reactor 10 is in the horizontal direction, it may be in the vertical direction because it does not affect the flow in principle.
図示の反応器１０は、循環ポンプ１３により液を循環路１１、１４（抜き出し路１１、返送路１４）を介して循環させるとともに、反応器１０内に、循環液の返送液を流入させることにより旋回流を生成させるものである。１５は、必要により設けられる、液の加温又は冷却の温度調節器である。
図面に示されているように、反応器１０はその長手方向一方端部側から他方端部に向かって内面が先窄まりとなり、循環液の返送液の流入口１０Ｘを含む流入位置が反応器１０の長手方向一方端部にあり、図３に示されているように、その内周面に沿う形態で、ほぼ接線方向に沿って、返送液を流入させるようにしてある。これによって、旋回流Ｒが形成されている。
接触処理がなされた後の接触処理液の流出口１０Ｙを含む流出位置は、長手方向他方端部となっている。
The illustrated reactor 10 circulates the liquid through the circulation paths 11 and 14 (the extraction path 11 and the return path 14) by the circulation pump 13, and allows the return liquid of the circulating liquid to flow into the reactor 10. A swirl flow is generated. Reference numeral 15 denotes a temperature controller for heating or cooling the liquid provided as necessary.
As shown in the drawing, the reactor 10 has a tapered inner surface from one end side in the longitudinal direction to the other end, and the inflow position including the inlet 10X for returning the circulating fluid is the reactor. 10 at one end in the longitudinal direction, and as shown in FIG. 3, the return liquid is allowed to flow in substantially the tangential direction in a form along the inner peripheral surface thereof. Thereby, a swirl flow R is formed.
The outflow position including the outflow port 10Y of the contact processing liquid after the contact processing is performed is the other end portion in the longitudinal direction.
接触処理液は、一時貯留器２０に導かれ、この一時貯留器２０内において接触処理液の安定化や粒子の沈降が図られ、最終接触処理液１０Ｚは、一時貯留器２０からオーバーフロー液として、または抜き出しポンプ２２により、後続の製品化手段（図示せず）に移送される。２１は取出し弁である。２３は調整用撹拌機である。
残部の液は、循環ポンプ１３により、返送路１４を介して反応器１０へ返送される。
The contact treatment liquid is guided to the temporary storage device 20, and the contact treatment liquid is stabilized and particles are settled in the temporary storage device 20. The final contact treatment liquid 10 </ b> Z is used as an overflow liquid from the temporary storage device 20. Or it is transferred to the subsequent productization means (not shown) by the extraction pump 22. 21 is a take-off valve. 23 is an adjustment stirrer.
The remaining liquid is returned to the reactor 10 by the circulation pump 13 via the return path 14.
しかるに、本発明においては、反応器１０の入口部分に、図１に示す液流れ変換器５０、図６に示す液流れ変換器５１などの液流れ変換器が設けられる。
図１に示す液流れ変換器５０は、基本的に反応器１０と同様なもので、この液流れ変換器５０により、直線液流れを半径方向の液流れを伴った液流れに変換した、図１の例では直線液流れを半径方向の液流れを伴った旋回流れに変換したうえで、反応器１０に返送するものである。
かかる液流れ変換器を設けない場合に比較して、反応器１０内の旋回流がより複雑な流れとなり、外部から注入する粒子の拡散効果が大きくなり、反応性が高まり、しかも、粒子及び粒子の凝集体の回転が大きくなることにより、球形の粒子の生成率が高まり、高い充填密度の粒子を得ることができる。
However, in the present invention, a liquid flow converter such as the liquid flow converter 50 shown in FIG. 1 or the liquid flow converter 51 shown in FIG. 6 is provided at the inlet of the reactor 10.
The liquid flow converter 50 shown in FIG. 1 is basically the same as the reactor 10, and the liquid flow converter 50 converts a linear liquid flow into a liquid flow with a radial liquid flow. In the first example, the linear liquid flow is converted into a swirl flow accompanied by a liquid flow in the radial direction and then returned to the reactor 10.
Compared with the case where such a liquid flow converter is not provided, the swirl flow in the reactor 10 becomes a more complicated flow, the diffusion effect of particles injected from the outside increases, the reactivity increases, and the particles and particles By increasing the rotation of the agglomerates, the generation rate of spherical particles increases, and particles with a high packing density can be obtained.
反応器１０内の液流れは旋回流Ｒとなるが、その渦中心部には空洞部分Ｖ（図４参照）ができる傾向にある。そして、特に、旋回流Ｒの渦中心近傍の内周部分の流れは、平均流速に比較して著しく高速であり、かつ、流れの乱れも大きい。
かかる位置において、注入すべき金属を含む注入液Ａ液〜Ｃ液を注入すると、注入液が急激に拡散し、均質な反応が可能となる。
そこで、図２に示すように、各注入液Ａ液〜Ｃ液は注入管１６Ａ、１６Ｂ…を使用してその先端から吐出されるまで、相互の接触を防止することが望ましい。
さらに、旋回流Ｒの影響が及ばないように、ガイド管１７を挿入するのが望ましい。
The liquid flow in the reactor 10 becomes a swirl flow R, but there is a tendency that a hollow portion V (see FIG. 4) is formed at the center of the vortex. In particular, the flow in the inner peripheral portion in the vicinity of the vortex center of the swirling flow R is remarkably faster than the average flow velocity, and the flow disturbance is large.
When the injection liquids A to C containing the metal to be injected are injected at such positions, the injection liquid diffuses rapidly and a homogeneous reaction is possible.
Therefore, as shown in FIG. 2, it is desirable to prevent each of the infusion solutions A to C until they are discharged from their tips using the infusion tubes 16A, 16B.
Furthermore, it is desirable to insert the guide tube 17 so as not to be affected by the swirling flow R.
ここで、注入すべき無機物質を含む注入液Ａ液〜Ｃ液の注入位置は、反応器１０内の接触の場において、反応器１０の内壁表面より中心側位置において注入すれば足りるが、図４に位置を示すように、中心から半径ｒの２／３以内、好ましくは１／２以内が好適である。 Here, the injection positions of the injection liquids A to C containing the inorganic substance to be injected may be injected at a position closer to the center than the inner wall surface of the reactor 10 in the contact area in the reactor 10. As indicated by position 4, the radius is preferably within 2/3 of the radius r, preferably within 1/2.
必要ならば、図示はしていないが、接触の場を与える反応器１０、１０…を、直列的に配置することができる。 If necessary, although not shown, the reactors 10, 10... For providing a contact field can be arranged in series.
他方、図６に示すスタティックミキサーと呼ばれる液流れ変換器５１を用いてもよい。スタティックミキサーは、捻れたエレメント５１ａとエレメント５１ｂとを配置方向を９０度異ならせながら交互に管路５１ｃ内に固定配置してもので、汎用のラインミキサーである。
このスタティックミキサー型液流れ変換器５１においては、出口部分で旋回流ではなく乱流の流れを得ることができ、漏斗型液流れ変換器５０の作用効果と実質的に同じ作用効果を得ることができる。
On the other hand, a liquid flow converter 51 called a static mixer shown in FIG. 6 may be used. The static mixer is a general-purpose line mixer because the twisted element 51a and the element 51b are alternately fixed and arranged in the pipe line 51c while being different in arrangement direction by 90 degrees.
In this static mixer type liquid flow converter 51, it is possible to obtain a turbulent flow instead of a swirling flow at the outlet portion, and to obtain substantially the same operational effects as the operational effects of the funnel type liquid flow converter 50. it can.
上記例の反応器１０は、長手方向一方端部側から他方端部に向かって内面が先窄まりとなるものが、旋回流の生成に好適であるが、内空間が均一な半径をもつ筒状のものでもよい。
さらに、図７のように、反応器１０内に回転筒または固定筒４０を設け、注入すべき金属を含む注入液Ａ液、Ｂ液を、注入管４２、４３を介して内壁面の接線方向に注入し、他方の端部の流出管４４から、接触処理がなされた後の流出液を流出するようにすることもができる。図７の形態では、スタティックミキサー型液流れ変換器５１を設けてある。
In the reactor 10 of the above example, the one whose inner surface is tapered from the one end side in the longitudinal direction toward the other end is suitable for generating a swirl flow, but the inner space has a uniform radius. It may be in a shape.
Further, as shown in FIG. 7, a rotating cylinder or a fixed cylinder 40 is provided in the reactor 10, and the injection liquids A and B containing the metal to be injected are tangential to the inner wall surface through the injection pipes 42 and 43. The effluent after the contact treatment is made to flow out from the outflow pipe 44 at the other end. In the form of FIG. 7, a static mixer type liquid flow converter 51 is provided.
図１〜図４に示す、内空間が均一な半径をもつ筒状部分及び先窄まり部分を有する例において、筒状部分から先窄まり部分への変化位置は、適宜選択できる。しかるに、接触処理液の流入口１０Ｘは、筒状部分に位置するのが、螺旋流れ生成に好適である。 In the example shown in FIGS. 1 to 4 in which the inner space includes a cylindrical portion having a uniform radius and a tapered portion, the change position from the cylindrical portion to the tapered portion can be selected as appropriate. However, the inflow port 10X for the contact treatment liquid is preferably located in the cylindrical portion for generating a spiral flow.
先に示した図２の形態では、反応器１０の比較的下流側において注入液を注入したが、図８のように、ガイド管１７を短くし、注入液Ａ液〜Ｃ液の注入管１６Ａ、１６Ｂ…を上流側に設けてもよい。もしくはガイド管を無くして端に注入管を設けても良い。また、図２に示すように注入管１６Ａ、１６Ｂ…先端位置を異ならせるほか、注入管１６Ａ、１６Ｂ…先端位置を一致させるようにしてもよい。
図８に示す形態によれば、旋回流場での反応長が稼げるため、下流側での流路内の材料の付着が激減する。
In the embodiment shown in FIG. 2, the injection solution is injected on the relatively downstream side of the reactor 10. However, as shown in FIG. 8, the guide tube 17 is shortened and the injection tubes A to C are injected. 16B... May be provided on the upstream side. Alternatively, the guide tube may be eliminated and an injection tube may be provided at the end. Further, as shown in FIG. 2, the injection tubes 16 </ b> A, 16 </ b> B—the tip positions may be made different, and the injection tubes 16 </ b> A, 16 </ b> B—the tip positions may be matched.
According to the form shown in FIG. 8, since the reaction length in the swirl flow field can be gained, the adhesion of the material in the flow path on the downstream side is drastically reduced.
本発明に係る装置は、適宜の材料で形成できるが、特に反応器１０をプラスチック成形品に流路を加工したものなども使用できる。そのブロックユニット反応器例を図９に示す。また、反応器は処理材料や液によって適宜の寸法関係とすることができる。
しかるに、小型の処理装置でありながら、十分な処理量を発揮し、しかも均一な接触処理性を示すものを得る観点から、図９に示す寸法基準で、旋回流を形成する接触の場の直径Ｄ２に対する旋回流を形成する主流の注入口径Ｄ１の比が、Ｄ２／Ｄ１＝２．５〜１０であることが望ましい。この比が小さいと旋回流の生成が十分でなく、過度に大きい場合には、速度が遅くなり、旋回流が不安定となる。
また、旋回流が安定して生成されるためには、旋回流を形成する接触の場の直径Ｄ２に対する抜き出し部の口径Ｄ３の比が、Ｄ２／Ｄ３＝０．５〜１０であるのが望ましい。
さらに、接触反応時間を確保するために、旋回流を形成する接触の場の直径Ｄ２に対する流路方向長さＨの比が、Ｈ／Ｄ２＝１〜１０であるのが望ましい。
The apparatus according to the present invention can be formed of an appropriate material. In particular, the reactor 10 in which a flow path is processed into a plastic molded article can be used. An example of the block unit reactor is shown in FIG. The reactor can have an appropriate dimensional relationship depending on the processing material and liquid.
However, the diameter of the contact field that forms the swirl flow on the basis of the dimensions shown in FIG. 9 from the viewpoint of obtaining a device that exhibits a sufficient throughput and exhibits uniform contact processability even though it is a small processing apparatus. The ratio of the main-flow inlet diameter D1 that forms the swirling flow with respect to D2 is preferably D2 / D1 = 2.5-10. When this ratio is small, the generation of the swirling flow is not sufficient, and when it is excessively large, the speed becomes slow and the swirling flow becomes unstable.
In order to generate a swirl flow stably, it is desirable that the ratio of the diameter D3 of the extraction portion to the diameter D2 of the contact field forming the swirl flow is D2 / D3 = 0.5-10. .
Further, in order to ensure the contact reaction time, it is desirable that the ratio of the length H in the flow path direction to the diameter D2 of the contact field forming the swirling flow is H / D2 = 1 to 10.
本発明の製造方法によって得られた金属の凝集粒子を、リチウムイオン電池用正極活物質に利用してリチウムイオン電池用正極活物質を製造できるほか、しいてはリチウムイオン電池を得ることができる。
本発明の製造方法によって得られた金属の凝集粒子は、粒子径が小さく粒子径が揃い、かつ優れた球形状である。
The metal agglomerated particles obtained by the production method of the present invention can be used as a positive electrode active material for a lithium ion battery to produce a positive electrode active material for a lithium ion battery, and thus a lithium ion battery can be obtained.
The metal agglomerated particles obtained by the production method of the present invention have a small particle size, a uniform particle size, and an excellent spherical shape.
ところで本発明は、 反応より物質移動律速となっている反応場において、物質移動と化学反応を効率よく行うものであり、無機反応、有機反応に関わらず利用可能なものである。
また、液液抽出における本装置の適用、水と油のエマルション等、液液の混合装置としても利用可能である。
他にも気液反応、固体粒子表面への反応（コーティング）等、液液反応以外のプロセスにも用途展開可能な装置である。
By the way, the present invention efficiently performs mass transfer and chemical reaction in a reaction field that is controlled by mass transfer rather than reaction, and can be used regardless of inorganic reaction or organic reaction.
It can also be used as a liquid-liquid mixing device such as application of this device in liquid-liquid extraction, water-oil emulsion, and the like.
In addition, it is an apparatus that can be used for processes other than liquid-liquid reactions such as gas-liquid reactions and reactions (coating) on the surface of solid particles.
なお、旋回流を少ない動力にて得るためには液粘性として１０００ｃＰ以下、特に１００ｃＰ以下のものが望ましい。 In order to obtain a swirl flow with less power, a liquid viscosity of 1000 cP or less, particularly 100 cP or less is desirable.
次に実施例及び比較例を示し、本発明の効果を明らかにする。
（参考例）ニッケルコバルト水酸化物の例
反応物質Ａとして硫酸ニッケル、硫酸コバルトを８５：１５の割合にて１．４Ｍとした液。反応物質Ｂとして２５％濃度の水酸化ナトリウム、反応物質Ｃとして２５％濃度のアンモニア水を使用した。反応物質Ａには所定の反応を進めるために硫酸アンモニウム、過酸化水素水、エタノール、グリセリン等の添加による溶媒調整を行うが、ここではこれらを無添加とした。
図１〜図４に示す形態であるが、漏斗型液流れ変換器５０を設けない態様で、反応物質Ａ、反応物質Ｂ及び反応物質Ｃを反応器１０内に注入した。運転条件として、装置容量は２Ｌ、操作ｐＨは１１．２(温度４５℃)、滞留時間は６０ｍｉｎとした。
スタート母液としてはイオン交換水２ｋｇにアンモニア水４０ｇ加えたものを使用した。
循環ポンプは７Ｌ／ｍｉｎにて運転し、Ａは約２８ｇ／ｍｉｎ、Ｂは約１１ｇ／ｍｉｎ，Ｃは約１ｇ／ｍｉｎにて注入した。さらに、Ｎ2ガスを５０ｍｌ／ｍｉｎ注入した。６時間実施した時点での粒子のＳＥＭ写真を取得し、観察に供した。ＳＥＭ写真は図１１に示した。
＜考察＞
その結果、粒子径が小さく、好適な凝集粒子を得ることができた。
このときの平均粒子径は約４．０μｍであり、充填密度は１．２７ｇ／ｍｌとなった。
充填密度の評価は、２５ｍｌメスシリンダーに２４ｈｒ，１０５℃にて乾燥した試料１０ｇを投入し、これを振動板の上に１分間のせ十分に均一になったときの嵩を測定したものである。このとき振動モータの回転数は２５００ｒｐｍとした。
（実施例）
漏斗型液流れ変換器５０を設けた図１〜図４に示す形態で、参考例と同様の方法で凝集粒子を得た。その結果、平均粒子径４．５μｍ，充填密度は１．４５ｇ／ｍｌとなり、液流れ変換器５０を用いない場合と比較して、球形の粒子の生成率が高まるとともに、より高い充填密度の粒子を得ることができた。ＳＥＭ写真は図１２に示した。
Next, examples and comparative examples will be shown to clarify the effects of the present invention.
(Reference example) Example of nickel cobalt hydroxide
A solution in which nickel sulfate and cobalt sulfate were made 1.4M in a ratio of 85:15 as the reactant A. 25% strength sodium hydroxide was used as the reactant B, and 25% ammonia water was used as the reactant C. In order to proceed a predetermined reaction to the reactant A, the solvent is adjusted by adding ammonium sulfate, hydrogen peroxide solution, ethanol, glycerin, etc., but these are not added here.
Although it is a form shown in FIGS. 1-4, the reaction material A, the reaction material B, and the reaction material C were inject | poured in the reactor 10 in the aspect which does not provide the funnel type liquid flow converter 50. FIG. As operating conditions, the apparatus capacity was 2 L, the operating pH was 11.2 (temperature 45 ° C.), and the residence time was 60 min.
As the starting mother liquor, a solution obtained by adding 40 g of ammonia water to 2 kg of ion-exchanged water was used.
The circulation pump was operated at 7 L / min, A was injected at about 28 g / min, B was about 11 g / min, and C was injected at about 1 g / min. Further, N 2 gas was injected at 50 ml / min. The SEM photograph of the particle | grains at the time of implementing for 6 hours was acquired, and it used for observation. The SEM photograph is shown in FIG.
<Discussion>
As a result, it was possible to obtain suitable aggregated particles having a small particle size.
The average particle size at this time was about 4.0 μm, and the packing density was 1.27 g / ml.
The evaluation of the packing density was performed by putting 10 g of a sample dried at 24 hours and 105 ° C. into a 25 ml graduated cylinder and measuring the bulk when the sample was sufficiently uniform on the diaphragm for 1 minute. At this time, the rotation speed of the vibration motor was 2500 rpm.
(Example)
Agglomerated particles were obtained in the same manner as in the reference example in the form shown in FIGS. As a result, the average particle diameter is 4.5 μm, and the packing density is 1.45 g / ml. Compared with the case where the liquid flow converter 50 is not used, the generation rate of spherical particles is increased, and the particles having a higher packing density. Could get. The SEM photograph is shown in FIG.
リチウムイオン電池用正極活物質用のほか各種の用途のものに適用できる。その例を列挙すると次のとおりである。
１）エマルション燃料製造
２）小径粒子製造 ナノ粒子を結晶成長させる等
３）ジアゾ化合物製造
４）触媒反応
５）その他マイクロリアクターでの反応処理例
ア 気液界面反応
フッ素ガスによるフッ素化反応
一酸化炭素ガスによるカルボニル化反応
イ 液液界面反応
ニトロ化反応（有機相/水相）
エステル還元
ジアゾカップリング
ウ 固液界面反応
固体担持触媒利用反応
エ 気・液・固界面反応
水素化反応
It can be applied to various uses in addition to the positive electrode active material for lithium ion batteries. Examples are listed as follows.
1) Emulsion fuel production 2) Small-diameter particle production Nanoparticle crystal growth, etc. 3) Diazo compound production 4) Catalytic reaction 5) Other reaction processes in microreactors a Gas-liquid interface reaction Fluorination reaction with fluorine gas Carbon monoxide Carbonylation reaction by gas b Liquid-liquid interface reaction Nitration reaction (organic phase / water phase)
Ester reduction Diazo coupling c Solid-liquid interface reaction Solid-supported catalyst reaction Air-liquid-solid interface reaction Hydrogenation reaction
１０…反応器、１０Ｘ…流入口、１０Ｙ…流出口、１１、１４…循環路、１６Ａ、１６Ｂ…注入管、１７…ガイド管、２０…貯留器、４０…回転筒、Ａ，Ｂ，Ｃ…注入液。 DESCRIPTION OF SYMBOLS 10 ... Reactor, 10X ... Inlet, 10Y ... Outlet, 11, 14 ... Circulation path, 16A, 16B ... Injection pipe, 17 ... Guide pipe, 20 ... Reservoir, 40 ... Rotating cylinder, A, B, C ... Infusion solution.
Claims (6)
前記液流れ変換器は、流れ中心線回りの旋回流を生成させる旋回流生成器であり、
前記反応器内の液流れを前記接触処理液の返送により前記他方端部に向かう旋回流とし、前記注入手段により反応液を、前記反応器の内表面より中心側位置に注入し、前記旋回流と接触させるよう構成されており、
前記液流れ変換器は、直線的液流れを半径方向の乱れを伴った液流れに変換するものであることを特徴とする無機粒子の連続反応晶析装置。 A reactor having one end and the other end; an injection means for injecting a reaction liquid containing an inorganic substance into the reactor; and a contact treatment liquid extracted from the other end of the reactor. A circulation means for returning at least a part of the processing liquid to the one end of the reactor via a liquid flow converter;
The liquid flow converter is a swirl flow generator that generates a swirl flow around a flow center line,
The liquid flow in the reactor is turned into a swirl flow toward the other end by returning the contact treatment liquid, the reaction liquid is injected into the central position from the inner surface of the reactor by the injection means, and the swirl flow Configured to come into contact with
The said liquid flow converter converts a linear liquid flow into the liquid flow accompanied by the disturbance of a radial direction, The continuous reaction crystallization apparatus of the inorganic particle characterized by the above-mentioned.
前記液流れ変換器は、流れ中心線回りの旋回流を生成させる旋回流生成器であり、
前記反応器内の液流れを前記接触処理液の返送により前記他方端部に向かう旋回流とし、前記注入手段により反応液を、前記反応器の内表面より中心側位置に注入し、前記旋回流と接触させて反応を行わせ、
無機粒子の反応晶析を行うことを特徴とする無機粒子の連続反応晶析方法。 A reactor having one end and the other end; an injection means for injecting a reaction liquid containing an inorganic substance into the reactor; and a contact treatment liquid extracted from the other end of the reactor. A circulation means for returning at least a part of the processing liquid to the one end of the reactor via a liquid flow converter for converting a linear liquid flow into a liquid flow with a radial disturbance. ,
The liquid flow converter is a swirl flow generator that generates a swirl flow around a flow center line,
The liquid flow in the reactor is turned into a swirl flow toward the other end by returning the contact treatment liquid, the reaction liquid is injected into the central position from the inner surface of the reactor by the injection means, and the swirl flow To react with it,
A method for continuous reaction crystallization of inorganic particles, characterized by performing reaction crystallization of inorganic particles.
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