JPS6116736B2 - - Google Patents
Info
- Publication number
- JPS6116736B2 JPS6116736B2 JP11850178A JP11850178A JPS6116736B2 JP S6116736 B2 JPS6116736 B2 JP S6116736B2 JP 11850178 A JP11850178 A JP 11850178A JP 11850178 A JP11850178 A JP 11850178A JP S6116736 B2 JPS6116736 B2 JP S6116736B2
- Authority
- JP
- Japan
- Prior art keywords
- stirring
- alkali hydroxide
- ultrafine
- hydroxide
- present
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
【発明の詳細な説明】
本発明は、粒径がｍμ〜μといつた超微粒の水
酸化アルカリ微粒化物の製造方法に関するもので
ある。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing ultrafine atomized alkali hydroxide particles having a particle size of mμ to μ.
従来、水酸化アルカリは、強い吸湿性のために
超微粒化することはきわめて困難であつた。 Conventionally, it has been extremely difficult to make alkali hydroxide into ultra-fine particles due to its strong hygroscopicity.
本発明者らは、ｍμ〜μといつたきわめて微細
な粒子状の水酸化ナトリウム、水酸化カリウムそ
の他の水酸化アルカリを得べく種々研究を行なつ
た結果、不活性有機溶媒および分散性の存在下に
水酸化アルカリを加熱、融解状とし強撹拌した後
撹拌しながら降塩することによつて微粒化し得る
ことを認めて本発明をなしたものである。 The present inventors conducted various studies in order to obtain extremely fine particulate sodium hydroxide, potassium hydroxide, and other alkali hydroxides in the form of mμ to μ, and found that the presence of an inert organic solvent and dispersibility. The present invention was made based on the recognition that atomization can be achieved by heating and melting alkali hydroxide, stirring vigorously, and then salting out while stirring.
すなわち、本発明は、固形水酸化アルカリを不
活性有機溶媒および分散性の存在下に加熱融解状
とし強撹拌した後、撹拌しながら降温することに
よつて水酸化アルカリの超微粒化物を製造する方
法である。 That is, the present invention produces ultrafine particles of alkali hydroxide by heating and melting solid alkali hydroxide in the presence of an inert organic solvent and a dispersant, stirring vigorously, and then lowering the temperature while stirring. It's a method.
本発明において使用する不活性有機溶媒として
は、たとえば、ベンゼン、トルエン、キシレンそ
の他のような芳香族炭化水素類、クロロベンゼ
ン、クロロトルエンその他のようなハロゲン化芳
香族炭化水素類などのような不活性有機溶媒を使
用することが好ましく、融解状水酸化アルカリの
撹拌を容易にし、吸湿を防止し、さらに、水酸化
アルカリの融解状化を助長するものと推定され
る。しかして、溶媒の使用量は撹拌が十分に行な
い得るような量を用いればよく限定されない。 Inert organic solvents used in the present invention include, for example, aromatic hydrocarbons such as benzene, toluene, xylene, etc., halogenated aromatic hydrocarbons such as chlorobenzene, chlorotoluene, etc. It is preferable to use an organic solvent, which is presumed to facilitate stirring of the molten alkali hydroxide, prevent moisture absorption, and further promote the molten state of the alkali hydroxide. Therefore, the amount of solvent to be used is not limited as long as the amount allows sufficient stirring.
また、本発明における分散剤とは、一たん微粒
化した粒が再凝結し大粒化することを防止し得る
ものであればよく、これらが粒の相互間に界在し
再凝結を防止しているものと思われる。使用する
分散剤としては、例えば、Tween−20（商品
名、ポリオキシエチレンソルビタンモノラウレー
ト）、Tween−80（商品名、ポリオキシエチレン
ソルビタンモノオレエート）、ソルポール800A
（商品名、ポリオキシエチレンアルキルアリール
エーテル、ポリオキシエチレンソルビタンアルキ
レート及びポリオキシエチレン脂肪酸誘導体が45
％、アルキルアリールスルホネートが55％からな
る組成物）、ソルポ−ル800B（商品名、ポリオオ
キシエチレンソルビタンアルキレート）、アノン
BF（商品名、ジメチルアルキル（ヤシ）ベタイ
ン）、ノニポール200（商品名、ポリオキシエチレ
ンノニルフエニルエーテル）、KF−96（シリコー
ン消泡剤）等の界面活性剤が挙げられるが、これ
らに限定されるものではない。しかして、分散剤
は、水酸化アルカリに対して0.0001重量％以上用
いればよく、数種を混合して使用してもよい。 In addition, the dispersant used in the present invention may be any agent that can prevent the once atomized grains from re-agglomerating and becoming larger, and the dispersing agent may intersect between the grains to prevent re-agglomeration. It seems that there are. Examples of dispersants used include Tween-20 (trade name, polyoxyethylene sorbitan monolaurate), Tween-80 (trade name, polyoxyethylene sorbitan monooleate), Solpol 800A
(Product name: polyoxyethylene alkylaryl ether, polyoxyethylene sorbitan alkylate and polyoxyethylene fatty acid derivative)
%, composition consisting of 55% alkylaryl sulfonate), Sorpol 800B (trade name, polyoxyethylene sorbitan alkylate), Anon
Surfactants include, but are limited to, BF (trade name, dimethylalkyl (coconut) betaine), Nonipol 200 (trade name, polyoxyethylene nonyl phenyl ether), KF-96 (silicone antifoaming agent), etc. It is not something that will be done. Therefore, the dispersant may be used in an amount of 0.0001% by weight or more based on the alkali hydroxide, and several types may be used in combination.
本発明の方法は、このような不活性有機溶媒お
よび分散剤の存在下に固形水酸化アルカリを加熱
融解状とするか、加熱温度は、使用する溶媒の種
類によつて異なり、溶媒の沸点前後に加熱するこ
とが好ましく、低沸点の溶媒を使用する場合に
は、加圧缶を用い水酸化アルカリを融解状とす
る。 In the method of the present invention, solid alkali hydroxide is heated to melt in the presence of such an inert organic solvent and a dispersant, or the heating temperature varies depending on the type of solvent used, and the heating temperature is around the boiling point of the solvent. When using a low boiling point solvent, the alkali hydroxide is molten using a pressurized can.
ついで、融解状の水酸化アルカリを強撹拌した
後、撹拌しながら降温するのであるが、撹拌は、
たとえば、ホモミキサー、超音波粉砕、あるい
は、ジエツト粉砕などのような装置を用いて可及
的に強力に行なうことが好ましく、降温は、でき
るだけ急激な温度低下を避けることが好ましい。 Next, after vigorously stirring the molten alkali hydroxide, the temperature is lowered while stirring.
For example, it is preferable to use a device such as a homomixer, ultrasonic pulverization, or jet pulverization to carry out the process as strongly as possible, and it is preferable to avoid lowering the temperature as rapidly as possible.
このようにして、ｍμ〜μ単位の超微粒化水酸
化アルカリが溶媒中に分散した状態で得ることが
できる。しかして、溶媒留去などによつて分離す
れば超微粒化された水酸化アルカリが得られ、こ
れは再度溶媒を添加し軽く撹拌することによつて
前と同様な分散状態とすることができる。また、
超微粒化された水酸化アルカリの使用目的によつ
ては、その目的とする用途において使用する溶媒
をこの方法における溶媒として使用すれば、この
方法によつて得た超微粒水酸化アルカリを分散し
た状態のままで用いることも可能である。 In this way, ultrafine alkali hydroxide particles in mμ to μ units can be obtained in a state dispersed in the solvent. If separated by solvent distillation etc., ultrafine alkali hydroxide can be obtained, which can be made into the same dispersion state as before by adding the solvent again and stirring lightly. . Also,
Depending on the purpose of use of the ultrafine alkali hydroxide, if the solvent used in the intended use is used as the solvent in this method, the ultrafine alkali hydroxide obtained by this method can be dispersed. It is also possible to use it as is.
添付の第１図は、本発明の一実施例を示す実施
例１において得られた超微粒化水酸化カリウムの
顕微鏡写真であつて、100mμ〜μの球状に超微
粒化されていることが明瞭に認められるものに対
し、第２図は、比較として行なつた比較例１にお
いて通常の撹拌法によつた場合の顕微鏡写真であ
つて多角形を呈しｍμ〜μ単位には超微粒化され
ていないことが明瞭であつて、本発明の優位性が
明示されている。 The attached FIG. 1 is a microscopic photograph of the ultrafine particulate potassium hydroxide obtained in Example 1 showing one example of the present invention, and it is clearly seen that the ultrafine particulates are spherical and have a size of 100 mμ to μ. In contrast, Fig. 2 is a microscopic photograph taken in Comparative Example 1, which was carried out as a comparison, using the normal stirring method, and shows a polygonal shape and is not ultra-fine in the order of mμ to μ. It is clear that there is no such problem, and the superiority of the present invention is clearly demonstrated.
なお、本発明の方法によつて得られた超微粒化
水酸化アルカリは、活性メチレンなどのアルキル
化反応にきわめて有効に使用することができる。 Incidentally, the ultrafine alkali hydroxide obtained by the method of the present invention can be used very effectively in the alkylation reaction of active methylene and the like.
このように、本発明の方法は、固形水酸化アル
カリを不活性有機溶媒および分散剤の存在下に融
解状として強撹拌した後、撹拌しながら降温させ
ることによつてｍμ〜μ単位の超微粒の水酸化ア
ルカリを得ることができたものであつて効果の大
な発明である。 As described above, the method of the present invention is to melt solid alkali hydroxide in the presence of an inert organic solvent and a dispersant, stir it vigorously, and then lower the temperature while stirring to form ultrafine particles in the order of mμ to μ. This is a highly effective invention, as it was possible to obtain alkali hydroxide of .
つぎに、実施例を述べる。 Next, an example will be described.
実施例 １
ホモミキサー装置を備えたSUS製の500ml容器
に固形水酸化カリウム（純度96％）52.08ｇ、キ
シレン200ml、Tween20（商品名）0.05ｇ（水酸
化カリウムに対して0.1重量％）を仕込み、140℃
に加熱し、（このとき水酸化カリウムは、ほぼ融
解状になつていた。）ホモミキサー装置を作動さ
せ10000r.p.mで約30分間撹拌し、撹拌しながら
順次湿温まで降温させた。Example 1 52.08 g of solid potassium hydroxide (purity 96%), 200 ml of xylene, and 0.05 g of Tween 20 (trade name) (0.1% by weight based on potassium hydroxide) were placed in a 500 ml SUS container equipped with a homomixer device. ,140℃
(At this time, the potassium hydroxide was almost in a molten state.) The homomixer was operated and stirred at 10,000 rpm for about 30 minutes, and the temperature was gradually lowered to a humid temperature while stirring.
得られたキシレン中に分散している水酸化カリ
ウムの粒径を顕微鏡を用いて測定した結果、
100mμ〜μの粒径の球状超微粒水酸化カリウム
が得られたことを認めた。顕微鏡写真を第１図に
示す。 As a result of measuring the particle size of potassium hydroxide dispersed in the obtained xylene using a microscope,
It was confirmed that spherical ultrafine potassium hydroxide particles with a particle size of 100 mμ to μ were obtained. A micrograph is shown in Figure 1.
実施例 ２
固形水酸化ナトリウムを用いて実施例１と同様
に行なつた結果、100mμ〜10μの粒径の球状超
微粒水酸化ナトリウムが得られた。Example 2 As a result of carrying out the same procedure as in Example 1 using solid sodium hydroxide, spherical ultrafine sodium hydroxide particles having a particle size of 100 mμ to 10μ were obtained.
比較例 １
固形水酸化カリウム52.08ｇ、キシレン200mlを
SUS製の500ml容器にとり、撹拌翼をもつた通常
の撹拌機で1500r.p.mで60分間撹拌した。得られ
た粒子は多角形を呈した本発明によるもののよう
に球状超微粒水酸化カリウムが得られていないこ
とが認められた。顕微鏡写真を第２図に示す。Comparative example 1 52.08g of solid potassium hydroxide and 200ml of xylene
The mixture was placed in a 500 ml container made of SUS and stirred for 60 minutes at 1500 rpm using an ordinary stirrer equipped with stirring blades. It was observed that the obtained particles were not spherical ultrafine potassium hydroxide particles like those according to the present invention, which were polygonal. A micrograph is shown in Figure 2.
比較例 ２
分散剤としてのTween20（商品名）を用いず
に実施例１と同様に、ホモミキサー装置を備えた
SUS製の500ml容器に固形水酸化カリウム（純度
96％）52.08ｇ、キレン200mlを仕込み、実施例１
と同様に行なつたが、水酸化カリウムは容器内壁
に付着し、分散超微粒化できなかつた。Comparative Example 2 A homomixer device was used in the same manner as in Example 1 without using Tween20 (trade name) as a dispersant.
Solid potassium hydroxide (purity
96%) 52.08g, Kiren 200ml, Example 1
However, the potassium hydroxide adhered to the inner wall of the container and could not be dispersed into ultra-fine particles.
第１図は、本発明の実施合一例を示す実施例１
で得られた超微粒水酸化カリウムの顕微鏡写真で
あり、第２図、比較例１で得た通常の撹拌法によ
つて得た水酸化カリウムの顕微鏡写真である。
Embodiment 1 FIG. 1 shows an example of the implementation of the present invention.
FIG. 2 is a micrograph of potassium hydroxide obtained by the usual stirring method in Comparative Example 1.
Claims (1)
分散剤の存在下に加熱融解状とし強撹拌した後、
撹拌しながら降温することを特徴とする水酸化ア
ルカリ微粒化物の製造方法。1 After heating and melting solid alkali hydroxide in the presence of an inert organic solvent and a dispersant and stirring vigorously,
A method for producing an atomized alkali hydroxide, characterized by lowering the temperature while stirring.
Priority Applications (11)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11850178A JPS5547222A (en) | 1978-09-26 | 1978-09-26 | Production of alkali hydroxide fine grain |
| US06/075,314 US4307034A (en) | 1978-09-26 | 1979-09-13 | Inert organic solvent dispersion of alkali hydroxide and reaction using the same |
| DE19792937945 DE2937945A1 (en) | 1978-09-26 | 1979-09-20 | DISPERSION OF AN ALKALINE HYDROXIDE IN INERT ORGANIC SOLVENT AND IMPLEMENTATIONS USING THE SAME |
| CA000336278A CA1142961A (en) | 1978-09-26 | 1979-09-25 | Inert organic solvent dispersion of alkali hydroxide and reaction using the same |
| CH862079A CH646615A5 (en) | 1978-09-26 | 1979-09-25 | DISPERSION OF AN ALKALINE HYDROXIDE IN INERT ORGANIC SOLVENT AND IMPLEMENTATIONS USING THE SAME. |
| NL7907113A NL193189C (en) | 1978-09-26 | 1979-09-25 | Process for alkylating the methylene group of an organic compound with an active methylene group. |
| FR797923788A FR2437240B1 (en) | 1978-09-26 | 1979-09-25 | INVERTED ORGANIC SOLVENT DISPERSION OF AN ALKALINE HYDROXIDE AND REACTION USING THE SAME |
| GB7933248A GB2033362B (en) | 1978-09-26 | 1979-09-26 | Inert organic solvent dispersion of alkaline hydroxide andreaction using the same |
| GB8131017A GB2082563B (en) | 1978-09-26 | 1979-09-26 | Preparing inert organic solvent dispersion of alkaline hydroxide |
| IT26018/79A IT1165340B (en) | 1978-09-26 | 1979-09-26 | INERT ORGANIC SOLVENT DISPERSION OF ALKALINE HYDROXIDE AND REACTION USING THE SAME |
| FR8017482A FR2455577B1 (en) | 1978-09-26 | 1980-08-07 | IMPROVEMENT IN THE PROCESS FOR THE PREPARATION OF ORGANOALKYLATED METHYLENE COMPOUNDS BY ALKYLATION OF AN ACTIVE METHYLENE COMPOUND IN THE PRESENCE OF ALKALINE HYDROXIDE |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11850178A JPS5547222A (en) | 1978-09-26 | 1978-09-26 | Production of alkali hydroxide fine grain |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5547222A JPS5547222A (en) | 1980-04-03 |
| JPS6116736B2 true JPS6116736B2 (en) | 1986-05-01 |
Family
ID=14738224
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11850178A Granted JPS5547222A (en) | 1978-09-26 | 1978-09-26 | Production of alkali hydroxide fine grain |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5547222A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02130259A (en) * | 1988-11-11 | 1990-05-18 | Nippon Denso Co Ltd | Injection quantity measuring device for fuel injection pump |
-
1978
- 1978-09-26 JP JP11850178A patent/JPS5547222A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5547222A (en) | 1980-04-03 |
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