JPH0218713B2 - - Google Patents

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Publication number
JPH0218713B2
JPH0218713B2 JP16653985A JP16653985A JPH0218713B2 JP H0218713 B2 JPH0218713 B2 JP H0218713B2 JP 16653985 A JP16653985 A JP 16653985A JP 16653985 A JP16653985 A JP 16653985A JP H0218713 B2 JPH0218713 B2 JP H0218713B2
Authority
JP
Japan
Prior art keywords
water
aqueous solution
powder
hydrogel
flocculant
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
JP16653985A
Other languages
Japanese (ja)
Other versions
JPS6227484A (en
Inventor
Jinichi Watanabe
Shusaku Matsumoto
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
DKS Co Ltd
Original Assignee
Dai Ichi Kogyo Seiyaku Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dai Ichi Kogyo Seiyaku Co Ltd filed Critical Dai Ichi Kogyo Seiyaku Co Ltd
Priority to JP16653985A priority Critical patent/JPS6227484A/en
Publication of JPS6227484A publication Critical patent/JPS6227484A/en
Publication of JPH0218713B2 publication Critical patent/JPH0218713B2/ja
Granted legal-status Critical Current

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Description

【発明の詳細な説明】[Detailed description of the invention]

本発明は、粉末高分子凝集剤を扱い易い粒状の
含水ゲル体にする方法に関するものである。 従来技術 従来から市販されているアニオン性及びカチオ
ン性凝集剤の大部分は粉末状であり、次のような
欠点を有している。 微粉の舞い立ち 粉末製品に含まれる微粉、特に200メツシユパ
スの微粉は、使用時における仕込みの際に、舞い
立ち易く、作業者の顔面に付着して、眼、唇、鼻
などの粘膜の水分を吸収し、その多大な吸収湿潤
性からゼリー状の濃厚液体となり、気管内壁等に
付着するなど、建康上問題となることが多い。ま
た、微粉の舞い立ちは、使用時に作業場の床面に
粉末製品の薄層を形成することとなるが、粉末製
品が作業場の漏水と混ざると、滑り易くなり、作
業者の転倒事故を起こす危険性もあつた。 ままこの発生 粉末製品は通常、水で溶解して使用するが、一
般に粉末製品はままこを生じ易く、一度発生した
ままこは、空気を内部に含有し、外表面は湿潤状
態に置かれるため、粉末製品を水に溶解し難くす
るものであり、粉末製品を30分以下の短時間で水
に均一に溶解するためは特別な装置、例えば特公
昭58−42204号公報や特開昭58−79525号公報記載
の装置などが必要であるとされていた。 このように、従来の粉末製品は、その水溶性と
高分子量に基づく優れた効能を有しながら、取り
扱い面では、多くの問題を有しており、これらの
問題の効率的な解決法が求められる。 その解決法として、凝集剤メーカーは極力200
メツシユパス分を篩選別し、比較的粗い粒子に限
り製品化しようとしているのが現状であり、まま
こを生じることなく簡単に溶解する凝集剤の開発
も試みられているが、粒状物相互の付着(ケーキ
ング)の問題があり、まだ決定的な製品は得られ
ていない。 新たな方法として、特願昭59−23356号には、
水溶性ビニルモノマーの水溶液を重合させて得ら
れた重合体ゲルを破砕したのち、平均粉砕滞留時
間が少なくとも3分以上となる竪型切断により、
これを更に細粒化し、微粉の発生を伴なわないで
粉末を製造する方法が開示される。この方法で
は、含水状態にある重合ゲル体を粉砕し、含水状
態を保つたまま乾燥させて微粉を含まない、粒径
分布の鋭い粒状物を得ることができるが、特別な
装置を必要とするため、高額な設備投資を必要と
する。 発明の目的 本発明は、粉末高分子凝集剤を、微粉の発生や
相互付着を伴うことなく、作業性よく、水に溶解
し易い微粒状の含水ゲル体に転ずる方法を提供す
ることを目的とする。 発明の構成 本発明の方法は、粉末高分子凝集剤と、ポリエ
チレングリコール、ソルビタン脂肪酸エステル及
びポリオキシエチレンソルビタン脂肪酸エステル
から選ばれる少なくとも一種の水溶性物質の0.5
〜10重量%水溶液を、重量比率で1対0.13〜3.0
の割合で、撹拌槽に連続供給し、撹拌混合して20
〜80重量%の水分を含む粒状の含水ゲル体を製造
することを特徴とする。 即ち、本発明では、粉末高分子凝集剤が撹拌槽
で特定の水溶性物質の水溶液と強制的に混合さ
れ、瞬時にして上記水溶液を吸収して、粒状の含
水ゲル体になるものであり、含水ゲル体の粒子径
は粉末高分子凝集剤の粒径及びそれと併用する上
記水溶液の量を変化させることによつて、任意に
選定できる。 粉末高分子凝集剤の粒径の増大に応じて粒径の
大きな含水ゲル体を得ることができ、また上記水
溶液の量を増すことによつても粒径の大きな含水
ゲル体を得ることができる。例えば、平均粒径
0.5mmの粉末高分子凝集剤を用いて上記水溶液の
使用量を変えることによつて、0.6〜7.0mmの粒径
の含水ゲル体が容易に製造できる。 また、上記水溶液に含まれる水溶性物質の量は
0.5〜10重量%であるが、これが過少であると、
生成した含水ゲル体が相互に付着し、撹拌に伴つ
てゲル体は塊状となり、目的とする製品を得るこ
とはできない。逆に、水溶性物質の量が過多であ
ると、不経済なだけでなく、使用時に水溶性物質
の存在が弊害を伴うこともあり、好ましくない。
本発明で使用する水溶液の水溶性物質濃度は通常
1〜5重量%であるのが好ましい。 また、ゲル体の含水率が20重量%未満では、粉
体となり、本発明の目的とする含水ゲル体を得る
ことはできず、80重量%を越えると溶解性の優れ
た安定した含水ゲル体を形成することはできな
い。 なお、本発明において生成した含水ゲル体は、
可能な限り速やかに撹拌槽から取り出されるのが
望ましく、滞留時間が長くなると含水ゲル体相互
の付着をもたらす危険性がある。一般に含水ゲル
体の滞留時間は1〜10秒であるのが望ましい。 このような本発明は、一般的な粉末高分子凝集
剤すべてに効果的に適用できるが、代表的な粉末
高分子凝集剤としては、ポリアクリルアミド、ポ
リアクリルアミド部分加水分解物、及びポリアク
リルアミドと他のビニルモノマーとの水溶性共重
合体等が挙げられ、ポリアクリルアミドと共重合
されるビニルモノマーとしては、ジメチルアミノ
エチルアクリレート、ジメチルアミノエチルメタ
クリレート、ジエチルアミノエチルアクリレー
ト、ジエチルアミノエチルメタクリレート、ジメ
チルアミノヒドロキシプロピルアクリレート、ジ
メチルアミノヒドロキシプロピルメタクリレー
ト、ジメチルアミノエチルアクリルアミド等の陽
イオン性ビニルモノマー、前記陽イオン性ビニル
モノマーをアルキルハライド、ジアルキル硫酸な
どの四級化剤で第四級アンモニウム塩化したも
の、アクリロニトリル、メタクリロニトリル、メ
チルアクリレート、エチルアクリレート、メタク
リルアミドなどの非イオン性モノマー、アクリル
酸、メタクリル酸あるいは、それらの塩などの陰
イオン性モノマーどが挙げられる。 また、粉末高分子凝集剤と併用される水溶液に
含まれる水溶性物質としては、平均分子量300〜
50000、特に平均分子量1000〜10000のポリエチレ
ングリコール、又はHLB10以上のポリオキシエ
チレンソルビタン脂肪酸エステルを使用するのが
好ましい。 次に、実施例に従つて本発明を更に詳しく説明
するが、実施例では図面に示す撹拌装置を使用し
た。 この撹拌装置は水門式排出上部板4及び下部板
5を有する水門式排出口9を円筒型容器1の側部
に有するものであつて、円筒型容器1の下方中央
には、垂直駆動モータ7によつて回転する駆動軸
8が存在し、この駆動軸8に長短2種の回転翼
2,3が上下に取りつけられており、更に、撹拌
槽1上方には水溶液貯蔵槽6が設けられ、ポリエ
チレングリコールなどの水溶液がこの水溶液貯蔵
槽6から供給管10から円筒型容器1に導入され
るようになつている。なお、当該水溶液の導入速
度はバルブ11によつて調整され、また粉末凝集
剤は直接円筒型容器1に投入されるようになつて
いるものである。 実施例 (1) 図面に示す直径50cm、高さ60cmの円筒型容器1
に、回転翼2,3を400r/mの速度で回転させな
がら、分子量2000万で、1N−NaC水溶液中30
℃で測定した固有粘度〔η〕が24.2であるポリア
クリルアミド凝集剤(加水分解率20モル%で、
200メツシユパス分1%を含む平均粒子径0.55mm
の粉末)を20.1Kg/hrの速度で円筒型容器1の上
部より供給し、同時に水溶液貯蔵槽4から分子量
6000のポリエチレングリコールの5%水溶液を
16.3Kg/hrの速度で供給した。この方法を23分間
連続的に実施したが、投入されたポリアクリルア
ミド凝集剤は短時間でポリエチレングリコールの
5%水溶液を吸収して膨潤し、平均粒子径0.75mm
の粒状の含水ゲル体が連続的に得られた(収量:
14.1Kg)。 この含水ゲル体は固形分50.6%(含水率49.4
%)で、適当な水分を含むため、しつとりした外
観を有し粉塵を生じることなく、しかも粒子間の
付着をケーキング現象のない扱い易い製品であ
り、水への溶解性も原料の粉末状ポリアクリルア
ミドの溶解性とほぼ同様に良好であつた。 ポリエチレングリコール水溶液の添加速度を表
に示す通り変化させて上記と同様の実験を行
い、含水率の異なるゲル体を得た。各種ゲル体の
水に対する溶解速度を測定した結果を、未処理の
凝集剤の測定値(No.1)と共に表示す。
The present invention relates to a method of forming a powdered polymer flocculant into a granular hydrogel that is easy to handle. Prior Art Most of the conventionally commercially available anionic and cationic flocculants are in powder form and have the following drawbacks. Flying of fine powder The fine powder contained in powdered products, especially the fine powder of 200 mesh powder, tends to fly when preparing for use, and it adheres to the face of the worker and removes moisture from the mucous membranes of the eyes, lips, nose, etc. It absorbs and becomes a jelly-like thick liquid due to its high absorption and wettability, which often causes health problems such as adhesion to the inner wall of the trachea. In addition, the flight of fine powder will form a thin layer of powder product on the floor of the workplace during use, but if the powder product mixes with water leakage in the workplace, it will become slippery and there is a risk of falling accidents for workers. The sex was also hot. Powder products are usually used after being dissolved in water, but powder products are generally prone to forming lumps. , which makes powder products difficult to dissolve in water, and in order to uniformly dissolve powder products in water in a short time of 30 minutes or less, special equipment is required, such as Japanese Patent Publication No. 58-42204 and Japanese Patent Application Laid-open No. 58-42204. It was believed that the equipment described in Publication No. 79525 was required. As described above, although conventional powder products have excellent efficacy based on their water solubility and high molecular weight, they have many problems in terms of handling, and there is a need for efficient solutions to these problems. It will be done. As a solution, flocculant manufacturers are trying to
At present, we are trying to sort out the mesh pass through a sieve and commercialize only relatively coarse particles. Attempts have also been made to develop flocculants that can be easily dissolved without forming lumps, but Due to the problem of caking, a definitive product has not yet been obtained. As a new method, Japanese Patent Application No. 59-23356 describes
After crushing the polymer gel obtained by polymerizing an aqueous solution of a water-soluble vinyl monomer, vertical cutting is performed such that the average crushing residence time is at least 3 minutes or more.
Disclosed is a method for producing powder by further refining the powder without generating fine powder. In this method, a hydrated polymer gel is crushed and dried while maintaining the hydrated state to obtain granules that do not contain fine particles and have a sharp particle size distribution, but special equipment is required. Therefore, large capital investment is required. Purpose of the Invention The purpose of the present invention is to provide a method for converting a powdered polymer flocculant into a fine-grained hydrogel that is easily soluble in water and has good workability without the generation of fine powder or mutual adhesion. do. Structure of the Invention The method of the present invention comprises a powdered polymer flocculant and 0.5% of at least one water-soluble substance selected from polyethylene glycol, sorbitan fatty acid ester, and polyoxyethylene sorbitan fatty acid ester.
~10% by weight aqueous solution at a weight ratio of 1:0.13~3.0
Continuously feed into the stirring tank at a ratio of 20
It is characterized by producing a granular hydrogel containing ~80% water by weight. That is, in the present invention, a powdered polymer flocculant is forcibly mixed with an aqueous solution of a specific water-soluble substance in a stirring tank, and instantaneously absorbs the aqueous solution to form a granular hydrogel. The particle size of the hydrogel can be arbitrarily selected by changing the particle size of the powdered polymer flocculant and the amount of the aqueous solution used together with it. A hydrogel with a large particle size can be obtained by increasing the particle size of the powdered polymer flocculant, and a hydrogel with a large particle size can also be obtained by increasing the amount of the aqueous solution. . For example, average particle size
By using a 0.5 mm powdered polymer flocculant and changing the amount of the aqueous solution used, a hydrogel having a particle size of 0.6 to 7.0 mm can be easily produced. Also, the amount of water-soluble substances contained in the above aqueous solution is
0.5 to 10% by weight, but if this is too low,
The produced hydrogels adhere to each other and become lumpy with stirring, making it impossible to obtain the desired product. On the other hand, if the amount of the water-soluble substance is too large, it is not only uneconomical, but also the presence of the water-soluble substance may cause harmful effects during use, which is not preferable.
The concentration of water-soluble substances in the aqueous solution used in the present invention is generally preferably 1 to 5% by weight. Furthermore, if the water content of the gel body is less than 20% by weight, it becomes a powder and it is impossible to obtain the hydrogel body which is the object of the present invention, and if it exceeds 80 weight%, it becomes a stable hydrogel body with excellent solubility. cannot be formed. In addition, the hydrogel body produced in the present invention is
It is desirable to remove the gel from the stirring tank as quickly as possible; if the residence time is too long, there is a risk that the hydrogels will adhere to each other. Generally, it is desirable that the residence time of the hydrogel is 1 to 10 seconds. Although the present invention can be effectively applied to all general powder polymer flocculants, representative powder polymer flocculants include polyacrylamide, polyacrylamide partial hydrolyzate, polyacrylamide, and others. Examples of vinyl monomers copolymerized with polyacrylamide include dimethylaminoethyl acrylate, dimethylaminoethyl methacrylate, diethylaminoethyl acrylate, diethylaminoethyl methacrylate, and dimethylaminohydroxypropyl acrylate. , dimethylaminohydroxypropyl methacrylate, dimethylaminoethyl acrylamide, etc., cationic vinyl monomers converted into quaternary ammonium salts with a quaternizing agent such as alkyl halides and dialkyl sulfates, acrylonitrile, methacrylamide, etc. Examples include nonionic monomers such as nitrile, methyl acrylate, ethyl acrylate, and methacrylamide, and anionic monomers such as acrylic acid, methacrylic acid, and salts thereof. In addition, the water-soluble substances contained in the aqueous solution used in combination with the powdered polymer flocculant have an average molecular weight of 300~
It is preferable to use polyethylene glycol having an average molecular weight of 50,000, particularly from 1,000 to 10,000, or polyoxyethylene sorbitan fatty acid ester having an HLB of 10 or more. Next, the present invention will be explained in more detail with reference to Examples, in which a stirring device shown in the drawings was used. This stirring device has a sluice-type discharge port 9 having a sluice-type discharge upper plate 4 and a lower plate 5 on the side of a cylindrical container 1, and a vertical drive motor 7 is installed in the lower center of the cylindrical container 1. There is a drive shaft 8 which is rotated by a rotor, and rotary blades 2 and 3 of two types, long and short, are attached above and below to this drive shaft 8, and an aqueous solution storage tank 6 is provided above the stirring tank 1. An aqueous solution such as polyethylene glycol is introduced from the aqueous solution storage tank 6 into the cylindrical container 1 through a supply pipe 10. The introduction speed of the aqueous solution is adjusted by a valve 11, and the powder flocculant is directly introduced into the cylindrical container 1. Example (1) Cylindrical container 1 with a diameter of 50 cm and a height of 60 cm shown in the drawing
While rotating the rotor blades 2 and 3 at a speed of 400 r/m, a
A polyacrylamide flocculant whose intrinsic viscosity [η] measured at °C is 24.2 (with a hydrolysis rate of 20 mol%,
Average particle size 0.55mm including 1% of 200 mesh passes
powder) is supplied from the top of the cylindrical container 1 at a rate of 20.1 Kg/hr, and at the same time the molecular weight is supplied from the aqueous solution storage tank 4.
6000 polyethylene glycol 5% aqueous solution
It was supplied at a rate of 16.3Kg/hr. This method was carried out continuously for 23 minutes, but the polyacrylamide flocculant added absorbed a 5% aqueous solution of polyethylene glycol and swelled in a short period of time, with an average particle size of 0.75 mm.
A granular hydrogel was continuously obtained (yield:
14.1Kg). This hydrogel body has a solid content of 50.6% (water content of 49.4%).
%), and contains an appropriate amount of moisture, so it has a moist appearance and does not generate dust, and is easy to handle with no caking phenomenon between particles. The solubility was almost as good as that of polyacrylamide. Experiments similar to those described above were conducted by changing the addition rate of the polyethylene glycol aqueous solution as shown in the table, and gel bodies with different water contents were obtained. The results of measuring the dissolution rate of various gel bodies in water are displayed together with the measured value (No. 1) of the untreated flocculant.

【表】 表から明らかなように、本発明に従つたNo.2
〜4の含水ゲル体は約20分で完全に溶解されるの
に対し、No.1の粉末状の製品は溶解に30分以上を
要するものであつた。なお、No.1の粉末状の製品
は溶解時に一時的に「ままこ」現象が生じ、均一
な溶解には時間がかかつた。 実施例 〔2〕 分子量の異なるポリエチレングリコールを使用
して実施例〔1〕と同様の方法を実施した。各製
品(含水ゲル体の性状を表に示す。
[Table] As is clear from the table, No. 2 according to the present invention
While the hydrogels No. 4 to 4 were completely dissolved in about 20 minutes, the powdered product No. 1 required more than 30 minutes to dissolve. It should be noted that the No. 1 powdered product temporarily caused a "sticky" phenomenon during dissolution, and it took time for uniform dissolution. Example [2] A method similar to Example [1] was carried out using polyethylene glycols having different molecular weights. The properties of each product (hydrogel body) are shown in the table.

【表】 いずれの製品も、含水ゲル体同志の相互付着性
はなく、手で容易にもみほぐすことが出来た。固
化(ケーキング)現象も認められなかつた。 実施例 〔3〕 ポリエチレングリコールの代わりにHLB=
16.7のポリオキシエチレンソルビタン脂肪酸エス
テル(モノウレート)を使用した以外は実施例
〔1〕と同様にして各種含水率の含水ゲル体を得
た。得られた含水ゲル体の性状を表に示すが、
いずれも水に対する溶解性の良好な相互付着性及
び固化現象のない扱い易い製品であつた。
[Table] In both products, the hydrogels did not adhere to each other and could be easily loosened by hand. No solidification (caking) phenomenon was observed. Example [3] HLB= instead of polyethylene glycol
Hydrogel bodies with various water contents were obtained in the same manner as in Example [1] except that polyoxyethylene sorbitan fatty acid ester (monourate) of 16.7 was used. The properties of the obtained hydrogel are shown in the table.
All of the products had good solubility in water, mutual adhesion, and were easy to handle without solidification.

【表】 発明の効果 本発明では、粉末高分子凝集剤を簡単に水に溶
けやすい粒状の含水ゲル体に調製できる。本発明
で得られる含水ゲル体は、微粉となつて作業場の
環境を悪化することはなく、また常温でも「まま
こ」を生じることなく約20分という短時間で水に
均一に溶解できる非常に扱い易いものであり、含
水ゲル体同志の相互付着(ケーキング)を生ずる
こともない。
[Table] Effects of the Invention In the present invention, a powdered polymer flocculant can be easily prepared into a granular hydrogel that is easily soluble in water. The water-containing gel obtained by the present invention does not become a fine powder and deteriorate the environment of the workplace, and it is extremely highly soluble and can be dissolved uniformly in water in a short time of about 20 minutes without causing "stickiness" even at room temperature. It is easy to handle and does not cause mutual adhesion (caking) of hydrogel bodies.

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

図面は本発明の実施例で使用した撹拌装置の断
面図である。 1……円筒型容器、2,3……回転翼、4……
水溶液貯蔵槽、5……水門式出上部板、6……水
門式出下部板、7……垂直駆動モータ、8……駆
動軸、9……排出口、10……供給管、11……
バルブ。
The drawing is a sectional view of a stirring device used in an example of the present invention. 1... Cylindrical container, 2, 3... Rotating blade, 4...
Aqueous solution storage tank, 5... Sluice gate type outlet plate, 6... Sluice gate type outlet plate, 7... Vertical drive motor, 8... Drive shaft, 9... Discharge port, 10... Supply pipe, 11...
valve.

Claims (1)

【特許請求の範囲】[Claims] 1 粉末高分子凝集剤と、ポリエチレングリコー
ル、ソルビタン脂肪酸エステル及びポリオキシエ
チレンソルビタン脂肪酸エステルから選ばれる少
なくとも一種の水溶性物質の0.5〜10重量%水溶
液を、重量比率で1対0.13〜3.0の割合で、同時
に、撹拌槽に連続供給し、撹拌混合して20〜80重
量%の水分を含む粒状の含水ゲル体を製造するこ
とを特徴とする粉末凝集剤を水易溶性の粒状含水
ゲル体にする方法。
1 Powdered polymer flocculant and a 0.5 to 10% aqueous solution of at least one water-soluble substance selected from polyethylene glycol, sorbitan fatty acid ester, and polyoxyethylene sorbitan fatty acid ester at a weight ratio of 1:0.13 to 3.0. At the same time, the powder flocculant is continuously supplied to a stirring tank and mixed by stirring to produce a granular hydrogel containing 20 to 80% by weight of water. Method.
JP16653985A 1985-07-27 1985-07-27 Method of converting powdery high-molecular coagulant into easily water-soluble particulate hydrous gel Granted JPS6227484A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP16653985A JPS6227484A (en) 1985-07-27 1985-07-27 Method of converting powdery high-molecular coagulant into easily water-soluble particulate hydrous gel

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP16653985A JPS6227484A (en) 1985-07-27 1985-07-27 Method of converting powdery high-molecular coagulant into easily water-soluble particulate hydrous gel

Publications (2)

Publication Number Publication Date
JPS6227484A JPS6227484A (en) 1987-02-05
JPH0218713B2 true JPH0218713B2 (en) 1990-04-26

Family

ID=15833156

Family Applications (1)

Application Number Title Priority Date Filing Date
JP16653985A Granted JPS6227484A (en) 1985-07-27 1985-07-27 Method of converting powdery high-molecular coagulant into easily water-soluble particulate hydrous gel

Country Status (1)

Country Link
JP (1) JPS6227484A (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6323966A (en) * 1986-07-17 1988-02-01 Wakunaga Pharmaceut Co Ltd Granulated paste and production thereof
US4799962A (en) * 1987-12-24 1989-01-24 Aqualon Company Water-soluble polymer dispersion

Also Published As

Publication number Publication date
JPS6227484A (en) 1987-02-05

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