JPH0819636B2 - Paper making - Google Patents
Paper makingInfo
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- JPH0819636B2 JPH0819636B2 JP61144545A JP14454586A JPH0819636B2 JP H0819636 B2 JPH0819636 B2 JP H0819636B2 JP 61144545 A JP61144545 A JP 61144545A JP 14454586 A JP14454586 A JP 14454586A JP H0819636 B2 JPH0819636 B2 JP H0819636B2
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- paper
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- pulp
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Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明はカチオン性の紙力増強剤を用いた紙の製法に
関するものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing paper using a cationic paper strengthening agent.
部分的に加水分解されたポリＮ−ビニルアセトアミド
は、分子内にポリビニルアミンの構造を有する安定性の
良いカチオン性の水溶性高分子であり、中性抄紙用にお
ける紙力増強剤として有効である。The partially hydrolyzed poly N-vinylacetamide is a cationic water-soluble polymer having a polyvinylamine structure in the molecule and having good stability, and is effective as a paper strength enhancer for neutral papermaking. .
従来、酸性抄紙法においては、紙力増強剤として用い
るアニオン性ポリアクリルアミドの定着剤として硫酸バ
ンドを用いるため、抄紙機の損耗、成紙の保存中の劣
化、排水の問題等があった。このため、これらの問題を
回避し、さらには、填料として安価な炭酸カルシウムを
用いることのできる中性または、弱塩基性条件下の抄紙
法が検討されつつある。Conventionally, in the acidic papermaking method, since a sulfuric acid band is used as a fixing agent for anionic polyacrylamide used as a paper strength enhancer, there have been problems such as wear of a paper machine, deterioration of papermaking during storage, and drainage. Therefore, a papermaking method under neutral or weakly basic conditions is being studied, which avoids these problems and can use inexpensive calcium carbonate as a filler.
このような条件下で使用される紙力増強剤としては、
それ自身、パルプに対して優れた定着性を有するカチオ
ン性の水溶性高分子からなる紙力増強剤が必要であり、
定着性に優れ、安定性の良いカチオン性の紙力増強剤が
望まれている。As a paper strength agent used under such conditions,
As such, a paper-strengthening agent composed of a cationic water-soluble polymer having excellent fixability for pulp is required,
A cationic paper strengthening agent having excellent fixability and good stability is desired.
分子中にポリビニルアミンの構造単位を有するポリア
クリルアミドのホフマン分解物は興味ある紙力増強効果
を示すことが知られている。しかし、製造時に強塩基性
の条件を経るため、副反応による両性化が避け難く、性
能に問題がある上、製造時に使用した次亜ハロゲン酸塩
の影響により、水溶液状における安定性に問題があっ
た。It is known that a Hoffman degradation product of polyacrylamide having a structural unit of polyvinylamine in the molecule exhibits an interesting paper-strengthening effect. However, since it undergoes a strongly basic condition during production, amphoteric conversion due to side reactions is unavoidable, and there is a problem in performance, and there is a problem in stability in aqueous solution due to the effect of the hypohalite used during production. there were.
本発明は、分子内にポリビニルアミンの構造単位を有
し、パルプに対して優れた定着性を示すカチオン性の紙
力増強剤を用いた紙の製法を提供することにある。そし
て、本発明の上記目的は下記一般式、〔Ｉ〕および〔I
I〕で表される構造単位からなり、 構造単位〔Ｉ〕：〔II〕のモル比が5:95〜90:10の範囲
であり、１規定食塩水中0.1g/dl溶液として25℃で測定
した還元粘度が0.1〜10dl/gである水溶性重合体をパル
プの乾燥重量に対して0.3〜２重量％の量で、パルプス
ラリーに添加して抄紙する、あるいは、紙に塗布するこ
とを特徴とする紙の製法により達せられる。An object of the present invention is to provide a method for producing paper using a cationic paper strengthening agent having a polyvinylamine structural unit in the molecule and exhibiting excellent fixability to pulp. The above object of the present invention is to provide the following general formulas [I] and [I]
I] consisting of structural units The molar ratio of structural units [I]: [II] is in the range of 5:95 to 90:10, and the reduced viscosity measured at 25 ° C as a 0.1 g / dl solution in 1N saline is 0.1 to 10 dl / g. The water-soluble polymer is added to the pulp slurry in an amount of 0.3 to 2% by weight based on the dry weight of the pulp to make a paper, or the paper is applied by a paper manufacturing method.
以下、本発明を詳細に説明する。 Hereinafter, the present invention will be described in detail.
前記の水溶性重合体の構造単位〔Ｉ〕式中、X-は陰イ
オンを表し、具体的には、水酸化物イオン、塩素イオ
ン、臭素イオン、ヨウ素イオン、硝酸イオン、硫酸イオ
ン、りん酸イオン、スルフアミン酸イオン、および水溶
性のアルキル硫酸、アルカンスルホン酸、カルボン酸か
らなる有機酸イオン等が例示される。In the structural unit [I] of the above water-soluble polymer, X − represents an anion, and specifically, hydroxide ion, chloride ion, bromide ion, iodide ion, nitrate ion, sulfate ion, phosphate Examples thereof include an ion, a sulfamate ion, and an organic acid ion composed of a water-soluble alkylsulfuric acid, an alkanesulfonic acid, and a carboxylic acid.
前記の水溶性重合体はＮ−ビニルアセトアミドを重合
して得られる重合体を酸または塩基性の条件下変性する
ことにより製造される。The water-soluble polymer is produced by modifying a polymer obtained by polymerizing N-vinylacetamide under acid or basic conditions.
カチオン性紙力増強剤は、通常、分子中のカチオン性
構造単位の比率が高い場合や、分子量の大きい場合に、
抄紙時のパルプの地合が悪くなるという傾向がある。し
かし、本発明の紙力増強剤は、極めて広い範囲で優れた
紙力増強効果を示し、構造単位〔Ｉ〕：〔II〕の比が5:
95〜90:10、好ましくは、10:90〜70:30の範囲の重合体
が使用される。また、高分子量であっても地合むらが起
こりにくく優れた紙力増強効果を示し、重合体を１規定
食塩水中0.1g/dlの溶液として25℃で測定した還元粘度
の値が0.1〜10dl/g、好ましくは0.5〜5dl/gの範囲のも
のが使用される。Cationic strength agents are usually used when the ratio of cationic structural units in the molecule is high or when the molecular weight is high.
There is a tendency that the formation of pulp during papermaking becomes poor. However, the paper-strengthening agent of the present invention exhibits an excellent paper-strengthening effect in an extremely wide range, and the ratio of structural units [I]: [II] is 5:
Polymers in the range 95-90: 10, preferably 10: 90-70: 30 are used. In addition, even when the polymer has a high molecular weight, uneven texture is unlikely to occur and an excellent paper-strengthening effect is exhibited, and the polymer has a reduced viscosity value of 0.1 to 10 dl measured at 25 ° C as a solution of 0.1 g / dl in 1N saline. / g, preferably in the range of 0.5-5 dl / g is used.
本発明で用いるカチオン性紙力増強剤は、たとえば、
Ｎ−ビニルアセトアミドの５〜60重量％の水溶液をラジ
カル重合開始剤の存在下、40〜80℃の温度で重合して得
られた高分子量の水溶性重合体を酸または、塩基性の条
件下、変性して得られる。The cationic strength agent used in the present invention is, for example,
A high molecular weight water-soluble polymer obtained by polymerizing a 5-60 wt% aqueous solution of N-vinylacetamide in the presence of a radical polymerization initiator at a temperature of 40-80 ° C. under acid or basic conditions , Obtained by denaturation.
ラジカル重合開始剤としては、通常、水溶性のビニル
モノマーに用いられる一般的な開始剤が使用されるが、
重合体を収率よく合成するためには、水溶性のアゾ化合
物を用いることが好ましい。好ましい重合開始剤の例と
しては、2,2′−アゾビス−２−アミジノプロパンの塩
酸塩または酢酸塩、4,4′−アゾビス−４−シアノ吉草
酸のナトリウム塩、アゾビス−N,N′−ジメチレンイソ
ブチルアミジンの塩酸塩、硫酸塩が例示される。その使
用量は、通常、Ｎ−ビニルアセトアミドの重量に対して
0.01〜１％の範囲である。得られた重合体の変性反応
は、加水分解、加アルコール分解などアミド基をアミノ
基に変えるいずれの反応も利用することができるが、水
溶液状の製品を得るためには、重合体水溶液を加水分解
する方法が用いられる。加水分解反応は塩基性でも酸性
でもよい。塩基性の加水分解物はそのまま使用すること
ができるが、反応終了後、酸を添加して中和することに
より、より安定に保存することができる。酸加水分解物
は、変性物をそのまま使用することができるが、酸を過
剰に用いた場合には、過剰の酸を中和しておくことが望
ましい。加水分解反応は、通常、重合体の濃度が５〜30
重量％の濃度で実施される。塩基または、酸の使用量
は、重合体中のアミド基の当量に対し、0.05〜２倍モル
の範囲で適宜目的とする変性率に応じて選択される。加
水分解反応は、40〜100℃の温度で実施される。かくし
て得られたカチオン性の重合体の水溶液は、極めて安定
であり、長期の保存後もその性能は低下せず、優れた紙
力増強効果を示す。As the radical polymerization initiator, a general initiator used for water-soluble vinyl monomers is usually used.
In order to synthesize the polymer in high yield, it is preferable to use a water-soluble azo compound. Examples of preferable polymerization initiators include 2,2′-azobis-2-amidinopropane hydrochloride or acetate, 4,4′-azobis-4-cyanovaleric acid sodium salt, azobis-N, N′- Examples include dimethylene isobutylamidine hydrochloride and sulfate. The amount used is usually based on the weight of N-vinylacetamide.
It is in the range of 0.01 to 1%. For the modification reaction of the obtained polymer, any reaction such as hydrolysis or alcoholysis that changes an amide group into an amino group can be utilized. A method of disassembling is used. The hydrolysis reaction may be basic or acidic. The basic hydrolyzate can be used as it is, but it can be more stably stored by adding an acid and neutralizing it after the reaction. As the acid hydrolyzate, a modified product can be used as it is, but when an acid is used in excess, it is desirable to neutralize the excess acid. The hydrolysis reaction usually has a polymer concentration of 5 to 30.
It is carried out at a concentration of% by weight. The amount of the base or acid used is appropriately selected in the range of 0.05 to 2 times the molar amount of the amide group in the polymer according to the desired modification ratio. The hydrolysis reaction is carried out at a temperature of 40-100 ° C. The aqueous solution of the cationic polymer thus obtained is extremely stable, does not deteriorate in its performance even after long-term storage, and exhibits an excellent paper-strengthening effect.
本発明の紙の製法におけるカチオン性紙力増強剤の使
用方法としては、従来公知の紙力増強方法のいずれをも
用いることができる。内添剤としてパルプスラリーに添
加して抄紙してもよく、湿紙または、乾燥紙にロールコ
ーター、サイズプレス、および浸漬機により塗布を行っ
てもよいが、内添剤として使用する場合その効果は顕著
である。As a method of using the cationic strength enhancer in the paper manufacturing method of the present invention, any conventionally known strength strengthening method can be used. Paper may be added to the pulp slurry as an internal additive, and wet paper or dry paper may be applied with a roll coater, size press, and dipping machine, but when used as an internal additive, its effect Is remarkable.
カチオン性紙力増強剤の使用量はパルプの乾燥重量に
対して0.3〜２重量％であって、内添剤として使用する
場合は、例えば、１〜３重量％のパルプスラリー中に、
その所定量を0.5〜２重量％の水溶液状で添加したのち
抄紙する。必要に応じ、硫酸バンドやアニオン性紙力増
強剤を併用してもよい。パルプの種類には限定されず、
グランドパルプ、サルフアイドパルプ、クラフトパル
プ、離解した古紙などいずれにも使用される。また、サ
イズ剤、填料の種類にも制約されない。The amount of the cationic strength agent used is 0.3 to 2% by weight based on the dry weight of the pulp, and when used as an internal additive, for example, in a pulp slurry of 1 to 3% by weight,
The predetermined amount is added in the form of an aqueous solution of 0.5 to 2% by weight, and then paper is made. If necessary, a sulfuric acid band or an anionic strength enhancer may be used in combination. Not limited to the type of pulp,
It is also used for ground pulp, sulfaid pulp, kraft pulp, and disintegrated waste paper. Further, there is no restriction on the type of sizing agent and filler.
本発明で用いるカチオン性紙力増強剤は、溶解水の水
質によらず希薄な水溶液状であっても極めて安定であ
る。また、炭酸カルシウムを填料として用いる弱アルカ
リ性の抄紙条件下でも安定でその効力を失わず中性、ま
たは、弱アルカリ性の抄紙条件に優れた紙力増強剤であ
る。The cationic strength enhancer used in the present invention is extremely stable even in the form of a dilute aqueous solution regardless of the quality of the dissolved water. Further, it is a paper strength enhancer which is stable under weak alkaline papermaking conditions using calcium carbonate as a filler and does not lose its efficacy, and is excellent in neutral or weak alkaline papermaking conditions.
以下、本発明を実施例により更に具体的に説明する
が、本発明は、その要旨を越えない限り以下の実施例に
限定されるものではない。Hereinafter, the present invention will be described more specifically by way of examples, but the present invention is not limited to the following examples unless it exceeds the gist.
（部分加水分解ポリＮ−ビニルアセトアミドの製造） 撹拌機、窒素導入下、冷却管を備えた200mlの四口フ
ラスコに、10gのＮ−ビニルアセトアミドと39.7gの脱塩
水を入れた。窒素ガス気流中、撹拌しつつ60℃に昇温し
たのち、10重量％の2,2′−アゾビス−２−アミジノプ
ロパン２塩酸塩水溶液0.3gを添加して、60℃にて６時間
保持した。得られた重合体水溶液に濃塩酸を所定量加え
て均一に混合後、６時間加熱還流し、加水分解物を得
た。生成物の一部に脱塩水および水酸化ナトリウムを添
加して希釈し、pH5の１重量％の重合体水溶液を調製
し、抄紙試験に供した。(Production of partially hydrolyzed poly-N-vinylacetamide) 10 g of N-vinylacetamide and 39.7 g of demineralized water were put into a 200 ml four-necked flask equipped with a stirrer and nitrogen, equipped with a cooling tube. After the temperature was raised to 60 ° C. with stirring in a nitrogen gas stream, 0.3 g of a 10% by weight 2,2′-azobis-2-amidinopropane dihydrochloride aqueous solution was added, and the mixture was kept at 60 ° C. for 6 hours. . A predetermined amount of concentrated hydrochloric acid was added to the obtained polymer aqueous solution, and the mixture was uniformly mixed and then heated under reflux for 6 hours to obtain a hydrolyzate. A part of the product was diluted by adding demineralized water and sodium hydroxide to prepare a 1 wt% polymer aqueous solution having a pH of 5 and subjected to a papermaking test.
生成物の一部をイソプロパノール中で脱水析出させた
のち、真空乾燥して固体状重合体を得た。これを用いて
組成および水溶液の粘度の測定に供した。A part of the product was dehydrated and precipitated in isopropanol and then vacuum dried to obtain a solid polymer. This was used to measure the composition and viscosity of the aqueous solution.
注１）還元粘度の測定 固体状の重合体を１規定の食塩水に0.1g/dlの濃度に
溶解し、25℃の条件下、オストワルドの粘度計を用いて
測定した。Note 1) Measurement of reduced viscosity A solid polymer was dissolved in 1N saline at a concentration of 0.1 g / dl and measured at 25 ° C using an Ostwald viscometer.
還元粘度ηsp/C＝（ｔ−to）/to/0.1〔dl/g〕 to:食塩水の下降速度 t:重合体溶液の下降速度 注２）加水分解率の測定 固体状の重合体を0.1重量％の濃度に蒸留水に溶解し
た。この水溶液5.0gを脱塩水を用いて200mlに希釈し希
塩酸を用いて溶液のpHを３に調整したのち、1/400規定
のポリビニル硫酸カリウムを用い、トルイジンブルーを
指示薬としたコロイド滴定法により得られた滴定値より
算出した。Reduced viscosity ηsp / C = (t-t o ) / t o /0.1 [dl / g] t o : Saline descent rate t: Polymer solution descent rate Note 2) Hydrolysis rate measurement Solid weight The coalescence was dissolved in distilled water to a concentration of 0.1% by weight. 5.0 g of this aqueous solution was diluted to 200 ml with demineralized water, the pH of the solution was adjusted to 3 with dilute hydrochloric acid, and then obtained by colloid titration using toluidine blue as an indicator using 1/400 normal potassium potassium sulfate. It was calculated from the measured titration value.
実施例１〜４、比較例１〜３ カナダ標準法で測定した、濾水度435mlを有するLBKP
の１％スラリーを500mlのビーカーに入れ、撹拌しつ
つ、前記方法で製造した重合体よりなるカチオン性紙力
増強剤を１重量％の水溶液状で対パルプ0.4重量％を添
加し１分間保持した。これをTAPPIスタンダード角型抄
紙機を用いて坪量60gの紙を抄いた。得られた湿紙を120
℃のドラムドライヤーを用いて３分間乾燥した。20℃、
相対湿度60％の条件下、成紙を放置したのち、JIS−P81
12およびJIS−P8113に従い、比破裂度および裂断長を測
定した。Examples 1-4, Comparative Examples 1-3 LBKP having a freeness of 435 ml as measured by the Canadian Standard Method.
1% slurry was placed in a 500 ml beaker and, while stirring, 0.4% by weight of a cationic paper-strengthening agent composed of the polymer prepared by the above method was added to the pulp in an aqueous solution of 1% by weight and held for 1 minute. . A TAPPI standard square paper machine was used to make a paper having a basis weight of 60 g. The obtained wet paper is 120
It was dried for 3 minutes using a drum dryer at ℃. 20 ° C,
After leaving the paper under conditions of 60% relative humidity, JIS-P81
12 and JIS-P8113, the specific bursting degree and the breaking length were measured.
ここで、 S1:破断強さ 〔kg/cm2〕 W :試験紙の坪量 〔g/m2〕 S2:引っ張り強さ 〔kg〕 B :試験片の巾 〔mm〕 使用した重合体の種類、組成および物性と、得られた
紙の紙力増強効果を第１表に示した。 Here, S 1 : breaking strength [kg / cm 2 ] W: basis weight of test paper [g / m 2 ] S 2 : tensile strength [kg] B: width of test piece [mm] Polymer used Table 1 shows the type, composition, and physical properties of paper, and the paper-strengthening effect of the obtained paper.
〔発明の効果〕 部分的に加水分解された、ポリＮ−ビニルアセトアミ
ドからなる本発明で用いるカチオン性紙力増強剤は、安
定性および紙力増強効果に優れ、自己定着性を有し、中
性条件および弱アルカリ性の条件下の抄紙法に寄与する
ことが大である。 [Effect of the Invention] The cationic paper strength enhancer used in the present invention, which is partially hydrolyzed and comprises poly N-vinylacetamide, has excellent stability and paper strength increasing effect, and has self-fixing property. It largely contributes to the papermaking method under the oxidative condition and the slightly alkaline condition.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 佐藤 耕一 神奈川県横浜市緑区鴨志田町1000番地 三 菱化成工業株式会社総合研究所内 (56)参考文献 特開 昭58−23809（ＪＰ，Ａ) 特開 昭61−118406（ＪＰ，Ａ) ─────────────────────────────────────────────────── ─── Continuation of front page (72) Koichi Sato Inventor, Koichi Sato 1000 Kamoshida-cho, Midori-ku, Yokohama-shi, Sanritsu Kasei Co., Ltd. (56) References Kaisho 61-118406 (JP, A)
Claims (1)
構造単位からなり、 構造単位〔Ｉ〕：〔II〕のモル比が5:95〜90:10の範囲
であり、１規定食塩水中0.1g/dl溶液として25℃で測定
した還元粘度が0.1〜10dl/gである水溶性重合体をパル
プの乾燥重量に対して0.3〜２重量％の量で、パルプス
ラリーに添加して抄紙する、あるいは、紙に塗布するこ
とを特徴とする紙の製法。1. A structural unit represented by the following general formulas [I] and [II]: The molar ratio of structural units [I]: [II] is in the range of 5:95 to 90:10, and the reduced viscosity measured at 25 ° C as a 0.1 g / dl solution in 1N saline is 0.1 to 10 dl / g. A method for producing a paper, which comprises adding a water-soluble polymer to the pulp slurry in an amount of 0.3 to 2% by weight based on the dry weight of the pulp to make a paper, or coating the paper.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61144545A JPH0819636B2 (en) | 1986-06-20 | 1986-06-20 | Paper making |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61144545A JPH0819636B2 (en) | 1986-06-20 | 1986-06-20 | Paper making |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS636198A JPS636198A (en) | 1988-01-12 |
| JPH0819636B2 true JPH0819636B2 (en) | 1996-02-28 |
Family
ID=15364786
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61144545A Expired - Fee Related JPH0819636B2 (en) | 1986-06-20 | 1986-06-20 | Paper making |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0819636B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2913756B2 (en) * | 1990-04-25 | 1999-06-28 | 三菱化学株式会社 | How to size paper |
| US5853636A (en) * | 1995-11-29 | 1998-12-29 | Matsumoto Yushi-Seiyaku Co., Ltd. | Fiber treatment composition |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3128478A1 (en) * | 1981-07-18 | 1983-02-03 | Basf Ag, 6700 Ludwigshafen | METHOD FOR PRODUCING LINEAR, BASIC POLYMERISATS |
| JPS61118406A (en) * | 1984-11-14 | 1986-06-05 | Mitsubishi Chem Ind Ltd | Production of water-soluble polyvinylamine |
-
1986
- 1986-06-20 JP JP61144545A patent/JPH0819636B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS636198A (en) | 1988-01-12 |
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| LAPS | Cancellation because of no payment of annual fees |