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JPS6011963B2 - Manufacturing method of acrylamide polymer - Google Patents
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JPS6011963B2 - Manufacturing method of acrylamide polymer - Google Patents

Manufacturing method of acrylamide polymer

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Publication number
JPS6011963B2
JPS6011963B2 JP15158879A JP15158879A JPS6011963B2 JP S6011963 B2 JPS6011963 B2 JP S6011963B2 JP 15158879 A JP15158879 A JP 15158879A JP 15158879 A JP15158879 A JP 15158879A JP S6011963 B2 JPS6011963 B2 JP S6011963B2
Authority
JP
Japan
Prior art keywords
polymer
acrylamide
weight
gel
water content
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
JP15158879A
Other languages
Japanese (ja)
Other versions
JPS5674107A (en
Inventor
禎三 大浜
修二 坂口
幸一 田原
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.)
Mitsubishi Chemical Corp
Original Assignee
Mitsubishi Chemical Industries 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 Mitsubishi Chemical Industries Ltd filed Critical Mitsubishi Chemical Industries Ltd
Priority to JP15158879A priority Critical patent/JPS6011963B2/en
Publication of JPS5674107A publication Critical patent/JPS5674107A/en
Publication of JPS6011963B2 publication Critical patent/JPS6011963B2/en
Expired legal-status Critical Current

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  • Processes Of Treating Macromolecular Substances (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Description

【発明の詳細な説明】 本発明はアクリルアミド系ポリマーの製造法に関するも
のである。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing an acrylamide polymer.

アクリルアミド系ポリマーは凝集剤として広く利用され
ており、通常、アクリルアミド含有水溶液を触媒の存在
下、重合させることにより容易に製造される。
Acrylamide-based polymers are widely used as flocculants, and are usually easily produced by polymerizing an acrylamide-containing aqueous solution in the presence of a catalyst.

ところが、アクリルアミドの重合は発熱反応であり、モ
ノマー水溶液の濃度をあまり高くすると重合系内の温度
が高くなりすぎ、生成したポリマーが熱劣化を起す欠点
がある。そのため、モノマ−水溶液の濃度は通常、10
〜35重量%の範囲であり、これを重合して得たポリマ
ーは含水量が90〜65重量%のゲル状物である。通常
、このゲル状ポリマーは押出造粒機で平均粒径2〜5仇
′仇の粒状物に粒状化したのち乾燥して製品とするが、
ゲル状ポリマーは粘着性が高いため、粒状化が難しいこ
と及び粒状化後の移送工程、乾燥工程などで粒状物同志
又は粒状物と装置壁との付着が激しいこと等の難点があ
った。本発明者は上記実情に鑑み、水溶液重合で得た含
水ゲル状ポリマーを粒状化する際に、粘着性の比較的に
少ない粒状物を得るため種々検討した結果、ある特定の
含水量及び粒径を有するアクリルアミド系ポリマーを添
加して上記粒状化を行うことにより、上記難点が改善さ
れることを知り、本発明を完成した。
However, the polymerization of acrylamide is an exothermic reaction, and if the concentration of the aqueous monomer solution is too high, the temperature within the polymerization system will become too high, resulting in thermal deterioration of the produced polymer. Therefore, the concentration of the monomer aqueous solution is usually 10
-35% by weight, and the polymer obtained by polymerizing this is a gel-like material with a water content of 90-65% by weight. Usually, this gel-like polymer is granulated into granules with an average particle size of 2 to 5 mm using an extrusion granulator, and then dried to produce a product.
Since gel-like polymers have high adhesiveness, they have problems such as difficulty in granulating them and severe adhesion of granules to each other or to the walls of the apparatus during the transfer process, drying process, etc. after granulation. In view of the above circumstances, the present inventor conducted various studies in order to obtain granules with relatively low stickiness when granulating a hydrogel polymer obtained by aqueous solution polymerization, and found that a specific water content and particle size was obtained. The present invention was completed based on the knowledge that the above-mentioned drawbacks can be improved by adding an acrylamide-based polymer having the following properties to perform the above-mentioned granulation.

すなわち、本発明の要旨は、モノマ‐濃度10〜35重
量%のアクリルアミド含有水溶液を触媒の存在下重合さ
せて得られる、含水量90〜65重量%のゲル状ポリマ
ーを、押出造粒機で平均粒径2〜5m/mの粒状物に粒
状化するに当り、前記ゲル状ポリマーに対し、含水量が
15重量%以下で、しかも、粒蚤がlm/仇以下である
微粒状のアクリルアミド系ポリマーを0.5〜20重量
%添加混合することを特徴とするアクリルアミド系ポリ
マーの製造法に存する。
That is, the gist of the present invention is to polymerize an acrylamide-containing aqueous solution with a monomer concentration of 10 to 35% by weight in the presence of a catalyst, and to obtain a gel-like polymer having a water content of 90 to 65% by weight on average using an extrusion granulator. When granulating into granules with a particle size of 2 to 5 m/m, a finely divided acrylamide polymer having a water content of 15% by weight or less and a particle flea of 1 m/m or less based on the gel-like polymer. A method for producing an acrylamide polymer, which comprises adding and mixing 0.5 to 20% by weight of acrylamide-based polymers.

以下、本発明を詳細に説明する。The present invention will be explained in detail below.

本発明で対象となるモノマーはアクリルアミド単独又は
アクリルアミドと例えば、アクリル酸、アクリル酸ソー
ダ、2ーアクリルアミドプロパソスルホン酸塩あるいは
ジェチルアミノェチルメクリレートの4級塩などのアク
リルアミドと共重合可能な公知のモノマーとの混合物が
挙げられるが、共重合の場合には、通常、アクリルアミ
ドの比率が50モル%以上が好ましい。
The monomer targeted by the present invention can be copolymerized with acrylamide alone or with acrylamide, such as acrylic acid, sodium acrylate, 2-acrylamide propasosulfonate, or quaternary salt of jetylaminoethyl methacrylate. Mixtures with known monomers may be mentioned, but in the case of copolymerization, it is usually preferable that the proportion of acrylamide is 50 mol% or more.

モノマー水溶液の濃度は10〜35重量%、好ましくは
20〜3の重量%であり、この濃度があまり低いと得ら
れるゲル状ポリマーの粘着性が高くなり、また、あまり
高いと重合系内の温度が高くなりすぎ、ポリマーが熱劣
化を起すので好ましくない。重合触媒としては、例えば
、アゾビス(2ーアミジノプロパン)塩酸塩などのアゾ
化合物、過硫酸カリウム、過硫酸アンモニウム、過酸化
水素などの過酸化物、亜硫酸ナトリウム、硫酸第1鉄、
塩化第1鉄などの還元剤が挙げられ、また、これらを2
種以上併用してもよい。
The concentration of the monomer aqueous solution is 10 to 35% by weight, preferably 20 to 3% by weight; if this concentration is too low, the resulting gel-like polymer will have high stickiness, and if it is too high, the temperature in the polymerization system will increase. is undesirable because it becomes too high and causes thermal deterioration of the polymer. Examples of the polymerization catalyst include azo compounds such as azobis(2-amidinopropane) hydrochloride, peroxides such as potassium persulfate, ammonium persulfate, and hydrogen peroxide, sodium sulfite, ferrous sulfate,
Reducing agents such as ferrous chloride may be mentioned;
More than one species may be used in combination.

触媒の使用量は通常、モノマーに対して100〜100
0功血、好ましくは200〜500瓜風である。重合は
通常、上述のモノマ−水溶液をN2ガスで脱気したのち
、触媒を加えて−10〜100qoの温度に保持して実
施される。
The amount of catalyst used is usually 100 to 100% of the monomer.
0 gong blood, preferably 200-500 meadow blood. Polymerization is usually carried out by degassing the above monomer aqueous solution with N2 gas, adding a catalyst, and maintaining the temperature at -10 to 100 qo.

本発明では重合により得られたゲル状ポリマーを押出造
粒機、殊に肉挽型の押出造粒機により粒状化するが、こ
の際に乾燥処理した微粒状のアクリルアミド系ポリマー
を添加混合することを必須要件とするものである。
In the present invention, the gel-like polymer obtained by polymerization is granulated using an extrusion granulator, particularly a meat grinder type extrusion granulator, and at this time, finely granulated acrylamide polymer that has been dried is added and mixed. is an essential requirement.

添加する微粒状のアクリルアミド系ポリマーは通常、製
造しようとするポリマ−の種類と同一成分のものが好ま
しい。
The finely divided acrylamide polymer to be added preferably has the same composition as the type of polymer to be produced.

微粒状ポリマーの含水量は15重量%以下、好ましくは
1の重量%以下であり、また、その粒径はlm/の以下
、好ましくは0.5の/肌以下、特に好ましくは0.2
の/肌以下である。微粒状ポリマーの含水量があまり高
い場合には、ゲル状ポリマーの粘着性を十分に改良する
ことができない。また、粒径があまり大きい場合には、
ゲル状ポリマーを良好な粒状物に成形することができな
いので好ましくない。本発明で使用する微粒状ポリマー
は他の重合系にて調製しても良いが、通常、同じ製造工
程で得られる製品ポリマーを分級又は必要に応じて粉砕
したものをリサイクル使用するのが好ましい。
The water content of the particulate polymer is less than 15% by weight, preferably less than 1% by weight, and its particle size is less than lm/cm, preferably less than 0.5 lm/skin, particularly preferably 0.2 lm/skin.
It is below the /skin level. If the water content of the particulate polymer is too high, the tackiness of the gel polymer cannot be sufficiently improved. In addition, if the particle size is too large,
This is not preferred because the gel-like polymer cannot be formed into good granules. Although the particulate polymer used in the present invention may be prepared using other polymerization systems, it is usually preferable to classify or, if necessary, crush a product polymer obtained in the same manufacturing process and recycle it.

特に、通常の製造工程では微粒状物が副生し、その処理
に困っているので、これを利用することにより劉生した
微粒状物の処理にもなるので好ましい方法である。上述
の微粒状ポリマーの添加量はゲル状ポリマーに対し0.
5〜2の重量%、好ましくは2〜15重量%であり、あ
まり添加量が少ないとゲル状ポリマ一を粒状化した際の
粘着性を改良することができず、また、あまり多いと粒
状物に良好に成形することができなくなるので好ましく
ない。
Particularly, in the normal manufacturing process, fine particles are produced as by-products and it is difficult to dispose of them, so this method is preferable because it can also be used to treat the formed fine particles. The amount of the above-mentioned fine particulate polymer added is 0.0% relative to the gel polymer.
The amount is 5 to 2% by weight, preferably 2 to 15% by weight. If the amount added is too small, it will not be possible to improve the adhesion when the gel polymer is granulated, and if it is too large, granules will be formed. This is not preferable because it will not be possible to form the material well.

微粒状ポリマーの添加は、通常、肉挽型の押出造粒機の
ホッパー中に含水ゲル状ポリマーとともに供孫舎し、両
者をなるべく均一に混練することにより行なわれる。
The addition of the particulate polymer is usually carried out by placing the polymer together with the hydrogel polymer in the hopper of a meat grinder type extrusion granulator and kneading the two as uniformly as possible.

前記押出造粒機で得られる粒状物の平均粒径は2〜5m
/のである。このように粒状化されたゲル状ポリマーは
、次いで、乾燥機に送られ乾燥処理するが、アクリルア
ミド成分の一部を加水分解する場合には、ゲル状ポリマ
ーを蝿投下、苛性ソーダ、苛性カリ、炭酸ソーダ又は炭
酸カリの水溶液と接触させてから乾燥処理を行う。
The average particle diameter of the granules obtained with the extrusion granulator is 2 to 5 m.
/ is. The gel-like polymer granulated in this way is then sent to a dryer for drying treatment, but when a part of the acrylamide component is to be hydrolyzed, the gel-like polymer is dropped onto a fly, caustic soda, caustic potash, and soda carbonate are used. Alternatively, drying treatment is performed after contacting with an aqueous solution of potassium carbonate.

乾燥処理は通常、40〜130qo、好ましくは60〜
110qoの温度で含水量が15重量%以下、好ましく
は1の重量%以下になるまで行なわれる。
The drying process is usually 40 to 130 qo, preferably 60 to 130 qo.
It is carried out at a temperature of 110 qo until the water content is below 15% by weight, preferably below 1% by weight.

乾燥処理の途中でポリマーの粒状物同志が多少、付着す
るので、乾燥の途中又は乾燥後に付着した粒状物を軽く
粉砕するのが好ましい。乾燥後のポリマーは分級処理し
、通常、粒径0.2〜5凧/仇、好ましくは0.5〜3
の/肌の粒状物を製品とし回収され、大粒状物は再粉砕
し、また微粒状物は前記の肉挽型の押出造粒機にリサイ
クルされる。以上、本発明によれば、高含水量のゲル状
ポリマーを成形して得た粒状ポリマーの粘着性が著しく
改良されるため、粒状ポリマーの移送及び乾燥工程での
粒状ポリマ−同志の付着、粒状ポリマーの装置壁への付
着が少ないと言う効果がある。また、従来、処理に困っ
ていた副生した微粒状ポリマーの処理にも役立つので、
本発明方法を採用することによる工業的効果は大きい。
次に、本発明を実施例により更に詳細に説明するが、本
発明はその要旨を超えない限り以下の実施例に限定され
るものではない。
Since some polymer particles adhere to each other during the drying process, it is preferable to lightly crush the adhered particles during or after drying. After drying, the polymer is classified, and the particle size is usually 0.2 to 5 particles per particle, preferably 0.5 to 3 particles.
The particulate matter from the skin is recovered as a product, the large particulate matter is re-ground, and the fine particulate matter is recycled to the above-mentioned meat grinder type extrusion granulator. As described above, according to the present invention, the adhesion of the granular polymer obtained by molding a gel-like polymer with a high water content is significantly improved. This has the effect of reducing adhesion of polymer to the walls of the device. It is also useful for treating by-product fine particulate polymers, which have traditionally been difficult to treat.
The industrial effects of adopting the method of the present invention are significant.
Next, the present invention will be explained in more detail with reference to examples, but the present invention is not limited to the following examples unless it exceeds the gist thereof.

実施例 1 重合反応器に25wt%アクリルアミド水溶液900k
9を仕込み、N2ガスで脱気したのち、重合触媒として
2・2−アゾビス(2−アミジノプロパン)塩酸塩20
0■血及び酸性亜硫酸ソーダ20の岬を加え、重合開始
温度2000で5時間、重合を行なった。
Example 1 900k of 25wt% acrylamide aqueous solution in a polymerization reactor
After charging 9 and degassing with N2 gas, 2,2-azobis(2-amidinopropane) hydrochloride 20 was added as a polymerization catalyst.
0.0 ■ blood and 20 g of acidic sodium sulfite were added, and polymerization was carried out at a polymerization initiation temperature of 2,000 for 5 hours.

得られたゲル状ポリマーと含水量が1肌t%で、粒径が
0.2仇/机以下のアクリルァミドポリマ‐22.5夕
(ゲル状ポリマーに対して2.5M%)とを肉挽型の押
出造粒機のホッパーに供給し、両者を混線して粒径2〜
5m/肌の粒状物を成形した。
The obtained gel-like polymer and an acrylamide polymer with a water content of 1 t% and a particle size of 0.2 mm/mm or less (2.5 M% based on the gel-like polymer) were combined. It is fed to the hopper of a meat grinder-type extrusion granulator, and the two are mixed to produce a particle size of 2~
Granules of 5 m/skin were molded.

このようにして得た粒状ポリマーにつき、粘着性テスト
を行ない、第1表に示す結果を得た。
The granular polymer thus obtained was subjected to an adhesion test and the results shown in Table 1 were obtained.

実施例 2〜3実施例1において、途中で添加する微粒
状ポリマーの添加量を第1表に示すように変えて同様な
テストを行なった。
Examples 2 to 3 Similar tests to those in Example 1 were conducted by changing the amount of the particulate polymer added during the process as shown in Table 1.

比較例 実施例1において、途中で微粒状ポリマ−を添加するこ
となく、同様なテストを行なった。
Comparative Example A test similar to that of Example 1 was conducted without adding the particulate polymer during the process.

第1表G注)粘着性テスト 造粒したゲル状ポリマー500夕をビニール袋に採り、
上下左右よりlk9/汝の圧力にて圧縮処理したのち、
ゲル状ポリマーを取り出し、その状態を観察し下記基準
により判定した。
Table 1 G Note) Adhesion test 500 g of the granulated gel polymer was placed in a plastic bag.
After compressing with lk9/your pressure from top, bottom, left and right,
The gel-like polymer was taken out, its state was observed, and it was judged according to the following criteria.

○……殆んど粒状物が相互に粘着していない。○...Almost no granules adhere to each other.

△・…・・粒状物は相互に粘着しているが、手で握ると
容易にほぐれる。
△・・・The granules are sticky to each other, but can be easily loosened when squeezed by hand.

×・・…・粒状物が相互に粘着しており、引き離すと糸
を引いてはぐれる。
×...The granules are stuck to each other, and when pulled apart, the strings are pulled and they come apart.

Claims (1)

【特許請求の範囲】[Claims] 1 モノマー濃度10〜35重量%のアクリルアミド含
有水溶液を触媒の存在下重合させて得られる、含水量9
0〜65重量%のゲル状ポリマーを、押出造粒機で平均
粒径2〜5m/mの粒状物に粒状化するに当り、前記ゲ
ル状ポリマーに対し、含水量が15重量%以下で、しか
も、粒径が1m/m以下である微粒状のアクリルアミド
系ポリマーを0.5〜20重量%添加混合することを特
徴とするアクリルアミド系ポリマーの製造法。
1 Water content 9 obtained by polymerizing an acrylamide-containing aqueous solution with a monomer concentration of 10 to 35% by weight in the presence of a catalyst
When granulating 0 to 65% by weight of a gel-like polymer into granules with an average particle size of 2 to 5 m/m using an extrusion granulator, the water content is 15% by weight or less with respect to the gel-like polymer, Moreover, the method for producing an acrylamide polymer is characterized by adding and mixing 0.5 to 20% by weight of a finely divided acrylamide polymer having a particle size of 1 m/m or less.
JP15158879A 1979-11-22 1979-11-22 Manufacturing method of acrylamide polymer Expired JPS6011963B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP15158879A JPS6011963B2 (en) 1979-11-22 1979-11-22 Manufacturing method of acrylamide polymer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP15158879A JPS6011963B2 (en) 1979-11-22 1979-11-22 Manufacturing method of acrylamide polymer

Publications (2)

Publication Number Publication Date
JPS5674107A JPS5674107A (en) 1981-06-19
JPS6011963B2 true JPS6011963B2 (en) 1985-03-29

Family

ID=15521790

Family Applications (1)

Application Number Title Priority Date Filing Date
JP15158879A Expired JPS6011963B2 (en) 1979-11-22 1979-11-22 Manufacturing method of acrylamide polymer

Country Status (1)

Country Link
JP (1) JPS6011963B2 (en)

Also Published As

Publication number Publication date
JPS5674107A (en) 1981-06-19

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