JP4788983B2 - Method for preventing slime failure in water system of paper and pulp manufacturing process - Google Patents
Method for preventing slime failure in water system of paper and pulp manufacturing process Download PDFInfo
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Description
【０００１】
【発明の属する技術の分野】
この発明は、紙・パルプ製造工程水系におけるスライム障害防止方法に関する。さらに詳しくは、この発明は、紙・パルプ製造工業における工程水系、主に抄紙工程水（白水）系におけるスライム障害防止方法に関する。
【０００２】
【従来の技術】
紙・パルプ製造工業における抄紙工程水系などでは、スライムによる障害が発生しやすい。スライムは、細菌や真菌のような微生物が水系内の管壁や器壁に付着し、粘着性物質を分泌することにより形成される。このスライムが管壁や器壁から剥離し、抄紙原料に混入したり配管を閉塞させたりして、生産品の品質低下や生産効率の低下などの障害が引き起こされる。
【０００３】
このようなスライムによる障害を防止するため、従来から種々の殺菌剤が使用されてきた。しかしながら、これらの殺菌剤には環境に悪影響を及ぼすもの、あるいは悪影響が懸念されるものが多く、薬剤の使用自体が規制されてきている。特に、優れた殺菌効果を発揮する薬剤ほど環境面では好ましくない性質を有する傾向がある。そこで、スライムによる障害を防止するために、より安全性の高い薬剤が求められている。
【０００４】
この発明の有効成分であるジカルボン酸またはポリホスフィノカルボン酸の重合体は、公知の防食剤、スケール防止剤としては知られているが、スライム障害防止効果を有することは知られていない。
【０００５】
【発明が解決しようとする課題】
この発明は、より安全性の高い薬剤を使用して、紙・パルプ製造工程水系におけるスライムの障害を効果的に防止することを課題とする。
【０００６】
【課題を解決するための手段】
この発明の発明者らは、かかる状況より、製品となる紙原料のパルプを含み、スライムによる障害が直接、製品の品質に悪影響を及ぼすことが懸念される、いわば特殊なスライム発生水系である紙・パルプ製造工程水系におけるスライムの障害防止効果について鋭意研究を行った。
その結果、従来スライム防止剤を含む添加剤として紙・パルプ製造工程水系には使用されたことのない特定のジカルボン酸またはポリホスフィノカルボン酸の重合体を、この水系に添加することにより、環境に悪影響を与えることなく、管壁、器壁、ワイヤーあるいはロールなどにスライムが付着するのを防止し、スライム障害防止効果が得られることを意外にも見出し、この発明を完成するに到った。
【０００７】
かくしてこの発明によれば、（Ａ）マレイン酸重合物（分子量８００〜１０００）、
（Ｂ）一般式（Ｉ）：
【０００８】
【化４】
［式中、Ｘは
【００１０】
【化５】
（式中、Ｚは−ＣＯＮＨＣ(ＣＨ3)2ＣＨ2ＳＯ3Ｈ基、ａ＋ｂは４〜１６である）で表される２つの繰り返し単位が規則的またはランダムに結合した基、Ｙは水素原子、−ＳＯ4Ｈ基または−ＨＰＯＨ基、Ｗは水素原子または−Ｘ−Ｙ基である］
で表されるアクリル酸−２−アクリロイルアミノ−２−メチル−１−プロパンスルホン酸・次亜リン酸付加重合物およびその塩、ならびに
（Ｃ）一般式（II）：
【００１２】
【化６】
（式中、ｍ＋ｎは４または１６である）
で表されるビス（ポリ−２−カルボキシエチル）ホスフィン酸およびその塩
から選択されるジカルボン酸またはポリホスフィノカルボン酸の重合体
［但し、グルタルジアルデヒド、一般式（１）および（２）：
【化９】
【化１０】
で表わされるハロゲン化脂肪族ニトロアルコールから選択される殺菌剤または殺藻剤を含まない］の１種以上の有効量を、紙・パルプ製造工程水系に添加することを特徴とする紙・パルプ製造工程水系におけるスライム障害防止方法が提供される。
【００１４】
【発明の実施の形態】
この発明で用いられる（Ａ）マレイン酸重合物は、分子量が８００〜１０００程度のものであり、比重（２０℃）が１．１〜１．２程度、動粘度（２５℃）が１０〜４０ｍｍ2／秒程度の琥珀色透明または微濁液体のものが好ましい。このような化合物は公知のスケール防止剤であり、市販のもの、例えばBioLab社製のBelclene（登録商標）２００を好適に用いることができる。
【００１５】
この発明で用いられる（Ｂ）アクリル酸−２−アクリロイルアミノ−２−メチル−１−プロパンスルホン酸・次亜リン酸付加重合物は、一般式（Ｉ）で表され、式中のホスフィニコ基の（リン原子に結合する）ヒドロキシル基の水素原子の一部または全部がアルカリ金属原子で置き換えられた塩であってもよい。また、カルボキシル基の水素原子や置換基Ｚのスルホン酸基の水素原子の一部またはその全部がアルカリ金属原子で置き換えられていてもよい。なかでも、一般式（Ｉ）におけるＺが−ＣＯＮＨＣ(ＣＨ3)2ＣＨ2ＳＯ3Ｎａ基であるアクリル酸−２−アクリロイルアミノ−２−メチル−１−プロパンスルホン酸ナトリウム・次亜リン酸付加重合物のナトリウム塩がスライム障害防止効果の点で特に好ましい。この化合物は公知のスケール防止剤であり、市販のもの、例えばBioLab社製のBelclene（登録商標）４００を好適に用いることができる。
【００１６】
この発明で用いられる（Ｃ）ビス（ポリ−２−カルボキシエチル）ホスフィン酸は、一般式（II）で表され、式中のホスフィニコ基の（リン原子に結合する）ヒドロキシル基の水素原子の一部または全部がアルカリ金属原子で置き換えられた塩であってもよい。また、カルボキシル基の水素原子の一部またはその全部がアルカリ金属原子で置き換えられていてもよい。なかでも、ビス（ポリ−２−カルボキシエチル）ホスフィン酸が、スライム障害防止効果の点で特に好ましい。このような化合物は公知の防食剤、スケール防止剤であり、市販のもの、例えばBioLab社製のBelclene（登録商標）５００［一般式（II）のｍ＋ｎが４である］およびBioLab社製の（Ｄ）Belsperse（登録商標）１６４［一般式（II）のｍ＋ｎが１６である］を好適に用いることができる。
【００１７】
この発明の方法においては、有効成分となる（Ａ）、（Ｂ）、（Ｃ）から選択されるジカルボン酸またはポリホスフィノカルボン酸の重合体の１種以上の有効量を、紙・パルプ製造工程水系に添加する。その有効量は、紙・パルプ製造工程水系の状態や有効成分の種類によって異なるが、通常、水系に対する有効成分濃度で３〜２５０ｍｇ／ｌ、好ましくは２０〜１００ｍｇ／ｌである。
有効成分濃度が３〜２５０ｍｇ／ｌの範囲であれば、優れたスライム障害防止効果が得られる。
【００１８】
この発明の方法においては、この発明の効果を阻害しない範囲で、公知の殺菌・静菌剤などを併用することができる。
【００１９】
この発明の方法における有効成分の添加形態は、特に限定されず、有効成分自体をそのままか、あるいは任意に水で希釈した水溶液として添加することができる。なお、前述の市販品は３５〜５０重量％の水溶液であり、これをそのままか、さらに水で希釈して用いることができる。
【００２０】
一般に紙・パルプ製造工程水系は循環系であるので、有効成分の添加場所は特に限定されないが、有効成分が水系中に均一に分散するように、添加場所を選定することが好ましい。また、有効成分を添加するための新たな設備を導入することなしに、既設の薬剤添加設備をそのまま転用してもよい。
【００２１】
【実施例】
この発明を以下の試験例により具体的に説明するが、この発明はこれらの試験例により限定されるものではない。
【００２２】
試験例において用いた薬剤を以下に示す。
薬剤Ａ：マレイン酸重合物の５０重量％水溶液（前述のBelclene２００）、
薬剤Ｂ：アクリル酸−２−アクリロイルアミノ−２−メチル−１−プロパンスルホン酸ナトリウム・次亜リン酸付加重合物のナトリウム塩の５０重量％水溶液（前述のBelclene４００）
薬剤Ｃ：ビス（ポリ−２−カルボキシエチル）ホスフィン酸の３５重量％水溶液（前述のBelclene５００）
薬剤Ｄ：ビス（ポリ−２−カルボキシエチル）ホスフィン酸の４０重量％水溶液（前述のBelsperse１６４）
【００２３】
薬剤Ｅ：ポリアクリル酸ナトリウムの４０重量％水溶液（比較例で使用）
薬剤Ｆ：２−メチル−５−クロロ−１，２−イソチアゾリン−３−オンと２−メチル−１，２−イソチアゾリン−３−オンとの３：１の混合物２５重量部、２−ブロモ−２−ニトロ−１，３−ジアセトキシプロパン２５重量部およびジエチレングリコール５０重量部からなる組成物（参考例で使用）
上記の薬剤のうち、薬剤Ｅはスケール防止剤として用いられている化合物であり、薬剤Ｆは殺菌剤として用いられている組成物である。
【００２４】
試験例１（スライム障害防止効果確認試験）
Ｌ字管に入れた液体標準培地に、某製紙工場白水系から採取したスライムより培養したスライム形成菌液０．１ｍｌ（生菌数：１．０×１０5 個／ｍｌ以上）を添加し、次いで表２に示される所定濃度の供試薬剤を添加した。この供試薬剤の添加時を試験開始時とした。Ｌ字管を４日間振とうした後、スライムの付着量を目視により観察し、表１に示す評価基準に基づいてスライム付着量を３段階で評価すると共に、生菌数も測定した。
それらの結果を供試薬剤名およびその添加量と共に表２に示す。
【００２５】
【表１】
【表２】
試験例２（製紙工程白水におけるスライム障害防止効果確認試験）
５００ｍｌのビーカーの内壁に沿わせて、寸法２８０ｍｍ×１００ｍｍのプラスチックワイヤーを固定し、某製紙工場白水系から採取し、予め濾過した白水（ｐＨ：７．０、ＳＳ：３５３ｐｐｍ）４００ｍｌを入れ、これを恒温槽付ジャーテスターで３０℃、５０ｒｐｍで攪拌した。次いで、表４に示される所定濃度の供試薬剤を添加した。この供試薬剤の添加時を試験開始時とした。
【００２８】
１日１回白水を交換するものとし、白水交換直後に、試験開始時に添加したものと同種、同量の供試薬剤を添加した。試験開始時、試験開始３０分後および白水交換直前における白水中の生菌数を測定した。
また、試験開始から２日後、プラスチックワイヤーに付着したスライムを目視により観察し、表３に示す評価基準に基づいてスライム付着量とスライム付着面積率をそれぞれ５段階で評価した（実施例１〜６）。
それらの結果を供試薬剤名およびその添加量と共に表４および表５に示す。
【００２９】
薬剤Ａ〜Ｄの代わりに薬剤Ｆを用い、その添加を白水交換３０分前とする以外は実施例１〜６と同様にして、スライム障害防止効果確認試験を行った。（参考例）。
試験開始時、薬剤Ｆの添加直前および白水交換直前における白水中の生菌数を測定した。また試験開始から２日後、プラスチックワイヤーに付着したスライムを目視により観察し、実施例１〜６と同様にして評価した（参考例）。
得られた結果を供試薬剤名およびその添加量と共に表４および表５に示す。
【００３０】
【表３】
【表４】
【表５】
【発明の効果】
この発明の方法によれば、より安全性の高いジカルボン酸またはポリホスフィノカルボン酸の重合体を紙・パルプ製造工程水系に添加することにより、殺菌効果が得られなくとも、優れたスライム障害防止効果が得られる。したがって、この発明のスライム障害防止方法は環境面から非常に有用な方法であるといえる。[0001]
[Field of the Invention]
The present invention relates to a method for preventing slime failure in a paper / pulp manufacturing process water system. More particularly, the present invention relates to a method for preventing slime damage in a process water system in the paper and pulp manufacturing industry, mainly in a papermaking process water (white water) system.
[0002]
[Prior art]
In the papermaking process water system in the paper and pulp manufacturing industry, failures due to slime are likely to occur. The slime is formed by microorganisms such as bacteria and fungi adhering to the tube wall and vessel wall in the water system and secreting an adhesive substance. The slime is peeled off from the pipe wall or the vessel wall, mixed into the papermaking raw material, or clogging the piping, causing problems such as a reduction in the quality of the product or a reduction in production efficiency.
[0003]
Various fungicides have been used in the past to prevent such slime damage. However, many of these bactericides have an adverse effect on the environment or are concerned about adverse effects, and the use of drugs has been regulated. In particular, a drug that exhibits an excellent bactericidal effect tends to have properties that are undesirable in terms of environment. Therefore, a safer drug is required in order to prevent damage caused by slime.
[0004]
A polymer of dicarboxylic acid or polyphosphinocarboxylic acid, which is an active ingredient of the present invention, is known as a known anticorrosive and scale inhibitor, but is not known to have a slime damage preventing effect.
[0005]
[Problems to be solved by the invention]
An object of the present invention is to effectively prevent a slime failure in a paper / pulp manufacturing process water system by using a safer chemical.
[0006]
[Means for Solving the Problems]
From this situation, the inventors of the present invention include a paper-based pulp as a product, and there is a concern that a failure caused by slime may directly adversely affect the quality of the product.・ We conducted extensive research on the prevention effect of slime in the pulp production process water system.
As a result, by adding a polymer of a specific dicarboxylic acid or polyphosphinocarboxylic acid, which has not been used in the paper / pulp manufacturing process water system as an additive containing an anti-slime agent, to this water system, The present invention has been completed by surprisingly finding that slime can be prevented from adhering to the tube wall, vessel wall, wire, roll, etc. without adversely affecting the surface, and that the slime failure prevention effect can be obtained. .
[0007]
Thus, according to this invention, (A) maleic acid polymer (molecular weight 800-1000),
(B) General formula (I):
[0008]
[Formula 4]
[Where X is
[Chemical formula 5]
Wherein Z is a —CONHC (CH 3 ) 2 CH 2 SO 3 H group, and a + b is 4 to 16, and Y is a hydrogen atom, which is regularly or randomly bonded to each other. , -SO 4 H group or -HPOH group, W is a hydrogen atom or -X-Y group]
Acrylic acid-2-acryloylamino-2-methyl-1-propanesulfonic acid / hypophosphorous acid addition polymer and its salt, and (C) general formula (II):
[0012]
[Chemical 6]
(Where m + n is 4 or 16)
A polymer of dicarboxylic acid or polyphosphinocarboxylic acid selected from bis (poly-2-carboxyethyl) phosphinic acid and salts thereof represented by
[However, glutaraldehyde, general formulas (1) and (2):
[Chemical 9]
[Chemical Formula 10]
1 or more effective amount selected from the halogenated aliphatic nitroalcohol represented by the above formula is added to the paper / pulp production process water system. A method for preventing slime failure in a process water system is provided.
[0014]
DETAILED DESCRIPTION OF THE INVENTION
The maleic acid polymer (A) used in this invention has a molecular weight of about 800 to 1000, a specific gravity (20 ° C.) of about 1.1 to 1.2, and a kinematic viscosity (25 ° C.) of 10 to 40 mm. Preferred is an amber transparent or slightly turbid liquid of about 2 / sec. Such a compound is a known scale inhibitor, and a commercially available product such as Belclene (registered trademark) 200 manufactured by BioLab can be suitably used.
[0015]
The (B) acrylic acid-2-acryloylamino-2-methyl-1-propanesulfonic acid / hypophosphorous acid addition polymer used in the present invention is represented by the general formula (I), and the phosphinico group in the formula A salt in which some or all of the hydrogen atoms of the hydroxyl group (bonded to the phosphorus atom) are replaced with alkali metal atoms may be used. Further, some or all of the hydrogen atoms of the carboxyl group and the sulfonic acid group of the substituent Z may be replaced with alkali metal atoms. Among them, sodium 2-acryloylamino-2-methyl-1-propanesulfonate / hypophosphite addition of acrylic acid in which Z in the general formula (I) is a —CONHC (CH 3 ) 2 CH 2 SO 3 Na group The sodium salt of the polymer is particularly preferred from the viewpoint of the slime damage prevention effect. This compound is a known scale inhibitor, and a commercially available product such as Belclene (registered trademark) 400 manufactured by BioLab can be suitably used.
[0016]
The (C) bis (poly-2-carboxyethyl) phosphinic acid used in the present invention is represented by the general formula (II), and is one of the hydrogen atoms of the hydroxyl group (bonded to the phosphorus atom) of the phosphinico group in the formula. A salt in which part or all of them are replaced with alkali metal atoms may be used. Further, some or all of the hydrogen atoms of the carboxyl group may be replaced with alkali metal atoms. Of these, bis (poly-2-carboxyethyl) phosphinic acid is particularly preferable from the viewpoint of the slime damage prevention effect. Such compounds are known anticorrosives and scale inhibitors, and are commercially available, for example, Belclene (registered trademark) 500 manufactured by BioLab (m + n of general formula (II) is 4) and ( D) Belsperse (registered trademark) 164 [m + n of general formula (II) is 16] can be preferably used.
[0017]
In the method of the present invention, at least one effective amount of a dicarboxylic acid or polyphosphinocarboxylic acid polymer selected from (A), (B), and (C) as an active ingredient is used for paper / pulp production. Add to process water system. The effective amount varies depending on the state of the paper / pulp production process water system and the type of the active ingredient, but is usually 3 to 250 mg / l, preferably 20 to 100 mg / l as the active ingredient concentration with respect to the water system.
When the active ingredient concentration is in the range of 3 to 250 mg / l, an excellent slime damage prevention effect can be obtained.
[0018]
In the method of the present invention, known sterilizing / bacteriostatic agents and the like can be used in combination as long as the effects of the present invention are not impaired.
[0019]
The form of addition of the active ingredient in the method of the present invention is not particularly limited, and the active ingredient itself can be added as it is or as an aqueous solution arbitrarily diluted with water. In addition, the above-mentioned commercial item is 35 to 50 weight% aqueous solution, and this can be used as it is or further diluted with water.
[0020]
Generally, since the paper / pulp production process water system is a circulation system, the addition location of the active ingredient is not particularly limited, but it is preferable to select the addition location so that the active ingredient is uniformly dispersed in the aqueous system. Moreover, you may divert the existing chemical | medical agent addition equipment as it is, without introducing the new equipment for adding an active ingredient.
[0021]
【Example】
The present invention will be specifically described with reference to the following test examples, but the present invention is not limited to these test examples.
[0022]
The drugs used in the test examples are shown below.
Agent A: 50% by weight aqueous solution of maleic acid polymer (the aforementioned Belclene 200),
Agent B: 50% by weight aqueous solution of sodium salt of 2-acryloylamino-2-methyl-1-propanesulfonate / sodium hypophosphite addition polymer of acrylic acid (the aforementioned Belclene 400)
Agent C: 35% by weight aqueous solution of bis (poly-2-carboxyethyl) phosphinic acid (the aforementioned Belclene 500)
Drug D: 40% by weight aqueous solution of bis (poly-2-carboxyethyl) phosphinic acid (Belsperse 164 described above)
[0023]
Agent E: 40% by weight aqueous solution of sodium polyacrylate (used in comparative examples)
Drug F: 25 parts by weight of a 3: 1 mixture of 2-methyl-5-chloro-1,2-isothiazolin-3-one and 2-methyl-1,2-isothiazolin-3-one, 2-bromo-2 A composition comprising 25 parts by weight of nitro-1,3-diacetoxypropane and 50 parts by weight of diethylene glycol (used in Reference Examples)
Among the above drugs, the drug E is a compound used as a scale inhibitor, and the drug F is a composition used as a bactericide.
[0024]
Test Example 1 (Slime damage prevention effect confirmation test)
To a liquid standard medium placed in an L-shaped tube, 0.1 ml of a slime-forming bacterial solution cultivated from slime collected from a white paper system of a smoked paper factory (number of viable bacteria: 1.0 × 10 5 cells / ml or more) is added, Next, reagent reagents having predetermined concentrations shown in Table 2 were added. The time when the reagent was added was designated as the start of the test. After shaking the L-shaped tube for 4 days, the amount of slime adhered was visually observed, the amount of slime adhered was evaluated in three stages based on the evaluation criteria shown in Table 1, and the number of viable bacteria was also measured.
The results are shown in Table 2 together with the reagent names and the amounts added.
[0025]
[Table 1]
[Table 2]
Test Example 2 (Slime damage prevention effect confirmation test in papermaking process white water)
Along the inner wall of a 500 ml beaker, a plastic wire with a size of 280 mm × 100 mm is fixed, taken from a white paper system of a paper mill, and 400 ml of pre-filtered white water (pH: 7.0, SS: 353 ppm) is added. Was stirred at 30 ° C. and 50 rpm with a jar tester with a thermostatic bath. Next, reagent reagents having predetermined concentrations shown in Table 4 were added. The time when the reagent was added was designated as the start of the test.
[0028]
The white water was exchanged once a day, and immediately after the white water exchange, the same kind and the same amount of reagent as those added at the start of the test were added. The number of viable bacteria in white water was measured at the start of the test, 30 minutes after the start of the test and immediately before the white water exchange.
In addition, two days after the start of the test, the slime adhered to the plastic wire was visually observed, and the slime adhesion amount and the slime adhesion area ratio were evaluated in five stages based on the evaluation criteria shown in Table 3 (Examples 1 to 6). ).
The results are shown in Tables 4 and 5 together with the reagent names and the amounts added.
[0029]
A slime failure prevention effect confirmation test was conducted in the same manner as in Examples 1 to 6, except that the medicine F was used in place of the medicines A to D and the addition was performed 30 minutes before the white water exchange. (Reference example).
At the start of the test, the number of viable bacteria in white water immediately before the addition of drug F and immediately before white water exchange was measured. Two days after the start of the test, the slime adhered to the plastic wire was visually observed and evaluated in the same manner as in Examples 1 to 6 (Reference Example).
The obtained results are shown in Tables 4 and 5 together with the reagent names and the amounts added.
[0030]
[Table 3]
[Table 4]
[Table 5]
【The invention's effect】
According to the method of the present invention, by adding a safer polymer of dicarboxylic acid or polyphosphinocarboxylic acid to a paper / pulp manufacturing process water system, even if a bactericidal effect is not obtained, excellent slime damage prevention An effect is obtained. Therefore, it can be said that the slime failure prevention method of the present invention is a very useful method from the environmental viewpoint.
Claims (2)
（Ｂ）一般式（Ｉ）：
で表される２つの繰り返し単位が規則的またはランダムに結合した基、Ｙは水素原子、−ＳＯ4Ｈ基または−ＨＰＯＨ基、Ｗは水素原子または−Ｘ−Ｙ基である］
で表されるアクリル酸−２−アクリロイルアミノ−２−メチル−１−プロパンスルホン酸・次亜リン酸付加重合物およびその塩、ならびに
（Ｃ）一般式（II）：
で表されるビス（ポリ−２−カルボキシエチル）ホスフィン酸およびその塩
から選択されるジカルボン酸またはポリホスフィノカルボン酸の重合体
［但し、グルタルジアルデヒドおよびその誘導体、一般式（１）および（２）：
で表わされるハロゲン化脂肪族ニトロアルコールから選択される殺菌剤または殺藻剤を含まない］の１種以上の有効量を、紙・パルプ製造工程水系に添加することを特徴とする紙・パルプ製造工程水系におけるスライム障害防止方法。(A) Maleic acid polymer (molecular weight 800-1000),
(B) General formula (I):
A group in which two repeating units represented by formulas are regularly or randomly bonded, Y is a hydrogen atom, —SO 4 H group or —HPOH group, and W is a hydrogen atom or —X—Y group]
Acrylic acid-2-acryloylamino-2-methyl-1-propanesulfonic acid / hypophosphorous acid addition polymer and its salt, and (C) general formula (II):
A polymer of dicarboxylic acid or polyphosphinocarboxylic acid selected from bis (poly-2-carboxyethyl) phosphinic acid and salts thereof represented by
[However, glutaraldehyde and its derivatives, general formulas (1) and (2):
1 or more effective amount selected from the halogenated aliphatic nitroalcohol represented by the above formula is added to the paper / pulp production process water system. Slime failure prevention method in process water system.
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| JP2000067294A JP4788983B2 (en) | 2000-03-10 | 2000-03-10 | Method for preventing slime failure in water system of paper and pulp manufacturing process |
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| JP2000067294A JP4788983B2 (en) | 2000-03-10 | 2000-03-10 | Method for preventing slime failure in water system of paper and pulp manufacturing process |
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| JPH0790639A (en) * | 1993-09-16 | 1995-04-04 | Akuasu Kk | One pack type water treating agent and water treating method |
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