JP4748724B2 - Pitch control agent or coagulant evaluation method - Google Patents
Pitch control agent or coagulant evaluation method Download PDFInfo
- Publication number
- JP4748724B2 JP4748724B2 JP2006161857A JP2006161857A JP4748724B2 JP 4748724 B2 JP4748724 B2 JP 4748724B2 JP 2006161857 A JP2006161857 A JP 2006161857A JP 2006161857 A JP2006161857 A JP 2006161857A JP 4748724 B2 JP4748724 B2 JP 4748724B2
- Authority
- JP
- Japan
- Prior art keywords
- pitch
- particles
- papermaking
- control agent
- pitch particles
- 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.)
- Active
Links
- 239000003795 chemical substances by application Substances 0.000 title claims description 21
- 239000000701 coagulant Substances 0.000 title claims description 9
- 238000011156 evaluation Methods 0.000 title description 5
- 239000002245 particle Substances 0.000 claims description 102
- 238000000034 method Methods 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 3
- 230000000087 stabilizing effect Effects 0.000 claims description 3
- 230000005722 itchiness Effects 0.000 claims description 2
- 239000011295 pitch Substances 0.000 description 95
- 239000000835 fiber Substances 0.000 description 12
- 239000000853 adhesive Substances 0.000 description 9
- 230000001070 adhesive effect Effects 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- 238000000691 measurement method Methods 0.000 description 6
- 239000006228 supernatant Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 239000000945 filler Substances 0.000 description 5
- 230000002209 hydrophobic effect Effects 0.000 description 5
- 238000003703 image analysis method Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000010893 paper waste Substances 0.000 description 5
- 229920001131 Pulp (paper) Polymers 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 238000011002 quantification Methods 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 3
- 125000000129 anionic group Chemical group 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 230000005653 Brownian motion process Effects 0.000 description 1
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000005537 brownian motion Methods 0.000 description 1
- 229920006317 cationic polymer Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 210000000038 chest Anatomy 0.000 description 1
- BHDFTVNXJDZMQK-UHFFFAOYSA-N chloromethane;2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound ClC.CN(C)CCOC(=O)C(C)=C BHDFTVNXJDZMQK-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- -1 etc. Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000025 natural resin Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000013055 pulp slurry Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Paper (AREA)
Description
本発明は、製紙工程上、紙の汚れや断紙等様々なトラブルの要因となる抄紙前の製紙原料中あるいは白水中のピッチ粒子を含む粒子の分析および定量化をする方法、およびピッチコントロール剤および又は凝結剤の評価をする方法、並びにピッチ粒子を含む粒子の分析および定量化により抄紙系内をモニタリングすることを特徴とする抄紙系内の操業安定化方法に関する。 The present invention relates to a method for analyzing and quantifying particles containing pitch particles in a papermaking raw material before papermaking or white water which causes various troubles such as paper stains and paper breaks in the papermaking process, and a pitch control agent The present invention also relates to a method for evaluating a coagulant and a method for stabilizing an operation in a papermaking system, wherein the inside of the papermaking system is monitored by analyzing and quantifying particles including pitch particles.
一般に、パルプ及び紙の製造工程でピッチと言われているものは、木材、パルプ及び古紙、損紙などから遊離した天然樹脂やガム物質、更にはパルプ及び紙の製造工程で使用される添加薬品などに由来する有機物を主成分とする疎水性、非水溶性の粘着物質である。ピッチは、パルプ及び紙の製造工程中、特に白水中では、コロイド状になって分散しており、コロイド状ピッチはスクリーン等での除去も困難である。これらのピッチが系内を循環して高濃度化すると、何らかの外的作用、例えば大きなせん断力、ｐHの急激な変化、硫酸バンドの過剰添加などにより、コロイド状態が破壊されて凝集、巨大化すると考えられている。凝集、巨大化したピッチは、その粘着性によりパルプや紙へ付着し、またファンポンプ、配管内、チェスト、ワイヤー、フェルト、ロールなどの製造装置類へ付着した後剥離して、パルプや紙へ再付着し、紙の汚点・欠点の発生による品質の低下や、断紙の発生による、生産製、作業性の低下などのピッチ障害を引き起こす。近年、紙の多様化による使用薬品類の増加と、工程で使用する水のクローズド化が進みにつれて従来にも増してピッチ障害が多発するとともに、複雑化している。 In general, what is said to be pitch in the pulp and paper manufacturing process is a natural resin or gum substance released from wood, pulp and waste paper, waste paper, etc., as well as additive chemicals used in the pulp and paper manufacturing process. It is a hydrophobic and water-insoluble adhesive substance mainly composed of organic substances derived from the above. The pitch is colloidal and dispersed during the pulp and paper manufacturing process, particularly in white water, and the colloidal pitch is difficult to remove with a screen or the like. When these pitches circulate in the system and become high concentration, colloidal state is destroyed due to some external action such as large shearing force, sudden change in pH, excessive addition of sulfuric acid band, and so on. It is considered. Agglomerated and enlarged pitch adheres to pulp and paper due to its adhesiveness, and adheres to manufacturing equipment such as fan pumps, piping, chests, wires, felts, rolls, etc., and then peels off to pulp and paper. Re-adhering causes deterioration in quality due to the occurrence of paper stains and defects, and pitch failures such as production and workability deterioration due to the occurrence of paper breaks. In recent years, as the number of chemicals used has increased due to diversification of paper and the use of water in the process has become more closed, pitch obstacles have become more frequent and complicated than ever before.
なお、ここでいうピッチとは、製紙工程中に存在する疎水性物質の総称として広義に用いており、いわゆる粘着物（スティッキー）と呼ばれるものも含んで使用している。 In addition, the pitch here is used in a broad sense as a general term for the hydrophobic substances present in the papermaking process, and includes the so-called adhesive (sticky).
これらピッチトラブルを防止するため、様々なピッチコントロール処方が開発されている。例えば、ピッチが付着し易い個所へピッチコントロール剤をシャワ−水として使用することにより、ピッチの付着を防止させる方法。ピッチが粗大化しないように、活性剤等を添加し、ミクロな状態で安定化させる方法。また、カチオン性高分子を使用することで、ミクロなピッチを繊維に定着させ、系外に抄き出す方法などが代表的である。 Various pitch control formulations have been developed to prevent these pitch problems. For example, a method of preventing the adhesion of pitch by using a pitch control agent as shower water in a place where the pitch easily adheres. A method in which an activator or the like is added and stabilized in a microscopic state so that the pitch does not become coarse. In addition, a typical method is to fix the micro pitch to the fiber by using a cationic polymer, and to make a paper out of the system.
これらのピッチトラブル防止のため、またピッチコントロール剤の評価をするために、製紙工程中のピッチを的確に定量、分析することが重要である。製紙工程中の製紙原料、インレット、白水紙料中のピッチ分析法については、ピッチ分抽出法、濁度測定法、アニオン量測定法、ヘマサイトメーターによる粒子カウント法（非特許文献１）、また ＪＩＳＰ８２３１−２００６に定められた古紙パルプ粘着物及びプラスチックの評価方法−画像解析法などがある。 In order to prevent these pitch troubles and to evaluate the pitch control agent, it is important to accurately quantify and analyze the pitch during the papermaking process. Regarding the pitch analysis method in papermaking raw materials, inlets, and white water stocks during the papermaking process, pitch extraction method, turbidity measurement method, anion amount measurement method, particle count method using hemacytometer (Non-patent Document 1), There is a waste paper pulp adhesive and plastic evaluation method-image analysis method defined in JISP8231-2006.
しかしながら、ピッチ分抽出法は有機溶剤が必要で手間が掛かる上、複合的な要因で生成するピッチ分を日常的に解析するのは困難である。また、濁度測定法は迅速かつ容易に行なえ、操業管理に向いてはいるが、濁度成分全てを測定するため、濁度成分の内訳、粒子の個数、粒子面積の変化を正確に反映できないときがある。アニオン量を測定する方法は、ピッチがアニオン性を帯びることから利用されるが、製紙工程中にはピッチ以外のアニオン性物質も多く存在し、また、疎水性ピッチの中にはアニオン性が弱いものも存在するため、ピッチ測定の代表的方法とするには不十分である。ＪＩＳＰ８２３１−２００６に定められた古紙パルプ粘着物及びプラスチックの評価方法−画像解析法は、粗大粘着物の測定に向いているが、粘着物と結束繊維または他の付着物との分離が困難かつ工数がかかる。また、製紙工程中のミクロな（コロイダルな）ピッチの濃度分析は不可能である。 However, the pitch extraction method requires an organic solvent and takes time, and it is difficult to routinely analyze the pitch generated due to multiple factors. The turbidity measurement method can be performed quickly and easily and is suitable for operation management. However, since all turbidity components are measured, the details of the turbidity components, the number of particles, and changes in the particle area cannot be accurately reflected. There is a time. The method for measuring the amount of anion is used because the pitch is anionic, but there are many anionic substances other than pitch during the papermaking process, and the hydrophobic pitch is weak in anionic properties. Some of them are inadequate for a typical pitch measurement method. Waste paper pulp adhesive and plastic evaluation method defined in JISP 8231-2006-Image analysis method is suitable for measuring coarse adhesives, but it is difficult to separate adhesives from bundling fibers or other adherents and man-hours. It takes. Further, it is impossible to analyze the concentration of micro (colloidal) pitch during the paper making process.
また、スラリー中の夾雑物を測定する方法としては、ワイヤーにパルプスラリーを通し、ワイヤー表面にパルプのウェットシートを形成させ、表面を平坦な透明板に押し付け、ＣＣＤカメラに取込み夾雑物を判定する方法がある。この方法は、コロイダルなピッチではなく夾雑物一般を対象とした測定法である。(特許文献１) In addition, as a method of measuring impurities in the slurry, the pulp slurry is passed through a wire, a wet sheet of pulp is formed on the surface of the wire, the surface is pressed against a flat transparent plate, and taken into a CCD camera to determine the impurities. There is a way. This method is not a colloidal pitch but a measurement method for general impurities. (Patent Document 1)
ヘマサイトメーター法による方法は、紙料液の上澄み液等を顕微鏡観察し、球形でブラウン運動を行なうミクロな粒子をカウントすることにより、系内のピッチ濃度を測定する方法である。この方法は、ミクロなピッチ粒子を直接観察できる方法であるが、目視観察のため、測定者間による誤差が大きく、客観的な値が得られず、またピッチの大きさ、形状等を区別し数値化することは困難であった。 The hemacytometer method is a method of measuring the pitch concentration in the system by observing the supernatant of the stock solution under a microscope and counting microscopic particles that are spherical and perform Brownian motion. This method allows direct observation of micro-pitch particles, but because of visual observation, there is a large error between measurers, an objective value cannot be obtained, and the pitch size, shape, etc. are distinguished. It was difficult to quantify.
また、工程中の紙料に対し、疎水性物質のみに吸着し、繊維、微細繊維、填料には親和性のない蛍光染料で処理し、その後Ｏｐｔｏｃａｌ Ｌａｓｅｒ Ｃｏｕｎｔｅｒで粒子の個数と粒径を測定する方法がある（非特許文献２）。
従来のピッチ測定法は、目視観察による場合は測定者間による誤差が大きく、客観的な値が得られず、またピッチの大きさ、形状等を区別し数値化することは困難であった。またＪＩＳＰ８２３１−２００６に定められた古紙パルプ粘着物及びプラスチックの評価方法ー画像解析法は、粗大粘着物の測定に向いているが、粘着物と結束繊維や他の付着物との分離が困難かつ工数がかかる。また、白水中のコロイダルなピッチの濃度分析は不可能である。従って本発明の課題は、測定者間の誤差が少なく、抄紙系内のコロイダルなピッチ分を含む粒子の個数、大きさ、形状等を客観的に分析、定量化する方法を開発することである。 In the conventional pitch measurement method, an error between the measurers is large in the case of visual observation, an objective value cannot be obtained, and it is difficult to distinguish and quantify the pitch size and shape. Also, the waste paper pulp adhesive and plastic evaluation method-image analysis method stipulated in JISP8231-2006 is suitable for measuring coarse adhesives, but it is difficult to separate adhesives from bundling fibers and other adhered substances. It takes man-hours. In addition, it is impossible to analyze the concentration of colloidal pitch in white water. Accordingly, an object of the present invention is to develop a method for objectively analyzing and quantifying the number, size, shape, etc. of particles containing colloidal pitch components in a papermaking system with little error between measurers. .
本発明者らは、前記目的を達成するために鋭意研究を重ねた結果、製紙工程における抄紙前製紙原料液中あるいは白水中のピッチ粒子を含む粒子の顕微鏡画像を、画像処理ソフトを用いコンピュータ画面上に表示させ特定の色成分を選択し前記ピッチ粒子を抽出することによりピッチ粒子の個数、ピッチ粒子の総面積、ピッチ粒子の平均面積、ピッチ粒子の平均いびつ度を定量化することにより、ピッチコントロール剤あるいは凝結剤の効果を評価することが可能であることが分かった。さらに分析および定量化により抄紙系内をモニタリングすることにより抄紙系内の操業を安定化する方法も可能であることを発見し本発明に到達した。 The present inventors have before Symbol result of extensive studies to achieve the object, a microscopic image of particles containing pitch particles before papermaking material solution or in the white water papermaking in the papermaking process, a computer using image processing software By quantifying the number of pitch particles, the total area of the pitch particles, the average area of the pitch particles, and the average degree of itchiness of the pitch particles by selecting the specific color component displayed on the screen and extracting the pitch particles, It was found that the effects of pitch control agents or coagulants can be evaluated. Furthermore, the present inventors have found that a method of stabilizing the operation in the papermaking system by monitoring the inside of the papermaking system by analysis and quantification has been achieved.
本発明は、製紙工程における抄紙前製紙原料液中あるいは白水中の繊維およびピッチ粒子を含む粒子の顕微鏡画像を画像処理しピッチを分析、定量する方法において、製紙工程における抄紙前製紙原料液中あるいは白水中のピッチ粒子を含む粒子の顕微鏡画像を、画像処理ソフトを用いコンピュータ画面上に表示させ特定の色成分を選択し前記ピッチ粒子を抽出することにより、ピッチ粒子の総面積、ピッチ粒子の平均面積、ピッチ粒子の平均いびつ度ピッチコントロール剤あるいは凝結剤の効果を評価することが可能であることが分かった。＠またこの分析および定量化法によって抄紙系内に添加したピッチコントロール剤あるいは凝結剤の評価が可能であり、さらにこの分析および定量化により抄紙系内をモニタリングすることによって抄紙系内の操業を安定化することが可能である。
The present invention relates to a method for image processing and analyzing and quantifying a microscopic image of particles containing fibers and pitch particles in white paper water before paper making in a paper making process, or in a paper making raw material liquid before paper making in a paper making process. A microscopic image of particles containing pitch particles in white water is displayed on a computer screen using image processing software, a specific color component is selected, and the pitch particles are extracted to obtain a total area of pitch particles, an average of pitch particles. It has been found that it is possible to evaluate the effect of the pitch control agent or the coagulant on the average degree of area and pitch particle pitch. @ The are possible evaluation of pitch control agent or coagulant is added to the papermaking system by the analysis and quantification method, stable operations in a papermaking system by further monitoring the papermaking system by the analysis and quantification It is possible to
本発明の分析および定量化法は、抄紙前製紙原料液またはその希釈液の上澄み液を採取し、１０倍から１２００倍の光学顕微鏡で観察し、水平、垂直方向に焦点をずらした複数箇所についての画像をデジタルカメラ、コンピュータあるいはビデオソフトなどのキャプチャ機能で採取し、それら画像を電子的な記録媒体としてコンピュータなどに保存する。顕微鏡の倍率は特に制限はなく、対象とするピッチ分の大きさにより調節するが、粒径が約５０μｍ以下のコロイダルなピッチを観測する場合は8００倍以上が望ましく、ピッチの凝集度合いを観察するには４００倍以下の低倍率のほうが望ましい。また画像を取り込む際に、顕微鏡画像をモニター上でさらに拡大してから取り込み、保存してもよい。 The analysis and quantification method of the present invention is to collect a supernatant of a pre-papermaking papermaking raw material liquid or a diluted liquid thereof, and observe with a 10 to 1200 times optical microscope, with respect to a plurality of positions shifted in the horizontal and vertical directions. Are captured by a capture function such as a digital camera, a computer, or video software, and the images are stored as an electronic recording medium in a computer or the like. The magnification of the microscope is not particularly limited, and is adjusted according to the size of the target pitch, but when observing a colloidal pitch with a particle size of about 50 μm or less, it is preferably 800 times or more, and the degree of pitch aggregation is observed. A lower magnification of 400 times or less is desirable. Further, when capturing an image, the microscope image may be further magnified on the monitor and then captured and stored.
その後、画像処理ソフト等を用い、特定の範囲の色成分を選択することで、ピッチ粒子が抽出されるような条件を設定して、画面上で目的とする粒子を抽出する。このとき、ピッチ粒子以外に填料、微細繊維等も同条件で抽出されるが、これらの形状はピッチ粒子と異なるため、後に形状の違いから区別することが可能である。また、ピッチ粒子以外の粒子も含めて、全粒子を測定し、形状の違いからピッチ粒子とピッチ粒子以外の粒子の存在割合等を推察することも可能である。抽出した粒子に関しては、抽出画像を直接比較するか、または粒子の個数、面積、粒径、形状、移動距離等を測定することにより、系内のピッチの濃度、粒子の種類、ピッチの自己凝集の度合いが判定できる。また、ピッチコントロール剤の未添加と添加済製紙原料中のピッチ分の抽出結果を比較することにより、ピッチコントロール剤あるいは凝結剤の効果を判定することが可能である。 Then, by using image processing software or the like, selecting a color component in a specific range, a condition for extracting pitch particles is set, and target particles are extracted on the screen. At this time, in addition to the pitch particles, fillers, fine fibers, and the like are also extracted under the same conditions. However, since these shapes are different from the pitch particles, they can be distinguished later from the difference in shape. It is also possible to measure all particles including particles other than pitch particles and infer the existence ratio of pitch particles and particles other than pitch particles from the difference in shape. For extracted particles, either directly compare the extracted images or measure the number, area, particle size, shape, distance traveled, etc. of the particles to determine the pitch concentration, particle type, pitch self-aggregation in the system. Can be determined. Moreover, it is possible to determine the effect of the pitch control agent or the coagulant by comparing the extraction result of the pitch in the papermaking raw material with no addition of the pitch control agent.
用いる画像解析ソフトは、色成分のヒストグラムから、特定の範囲を抽出することが可能で、個数、表面積等の測定が可能なものを用いる。特にソフトを限定するものではないが、解像度が高く、的確に目的粒子を抽出できるように、各色成分を表す値（Ｒ値、Ｇ値、Ｂ値等）に対して、少なくとも２５６段階のレンジ調整が可能なものを用いるのが好ましい。 The image analysis software to be used is one that can extract a specific range from a histogram of color components and can measure the number, surface area, and the like. The software is not particularly limited, but the range is adjusted in at least 256 steps with respect to the values (R value, G value, B value, etc.) representing each color component so that the target particles can be accurately extracted with high resolution. It is preferable to use one capable of
ピッチ分を抽出する方法は、例えばＲＧＢ値（赤（Ｒ）、緑（Ｇ）、青（Ｂ）の３種の色の組み合わせで全ての色を表す）やＨＳＩ値（色相（Ｈ）、彩度（Ｓ）、明度（Ｉ）の組み合わせで全ての色を表す）等のヒストグラムから、適切なレンジ設定を行なうことにより、ピッチ粒子が抽出されるような色成分のみを選択して抽出する。顕微鏡の設定、元画像の明るさにより、設定レンジは調節するが、同一試験には同一条件を用いるのが好ましい。ピッチ粒子他、填料や微細繊維等も同条件で抽出されるが、後に形状、面積を測定することにより、区別することが可能である。また、ピッチ以外の粒子も含め、全粒子として測定し、形状の違いからピッチ粒子とピッチ粒子以外の粒子の存在割合等を測定することも可能である。例えば疎水性ピッチは一般に球形であり、ピッチの凝集物はクラスター状になって観測される。また、填料等は角型やコンペイトウ型などそれぞれの填料特有の形態で観測される。微細繊維は細長い形状で観察される。 The method of extracting the pitch is, for example, an RGB value (representing all colors by a combination of three types of red (R), green (G), and blue (B)) or an HSI value (hue (H), chroma). By selecting an appropriate range from a histogram such as degrees (S) and lightness (I) representing all colors), only the color components from which pitch particles are extracted are selected and extracted. Although the setting range is adjusted depending on the setting of the microscope and the brightness of the original image, it is preferable to use the same conditions for the same test. Pitch particles, fillers, fine fibers, and the like are extracted under the same conditions, but can be distinguished later by measuring the shape and area. It is also possible to measure all particles including particles other than pitch, and to determine the existence ratio of pitch particles and particles other than pitch particles from the difference in shape. For example, the hydrophobic pitch is generally spherical, and the pitch aggregates are observed as clusters. In addition, fillers and the like are observed in a form specific to each filler such as a square type and a complex type. Fine fibers are observed in an elongated shape.
用いる顕微鏡には、特に制限はないが、デジタルカメラと接続が可能であるか、またはモニター上かコンピュータ上に画像を映し出すことが可能なものが、画像の取込みと保存の面から好ましい。拡大倍率は、ピッチ粒子の形状を十分に解析するために、１０倍〜１２００倍の倍率をカバーできることが望ましい。デジタルカメラは、解像度が高い方が、ミクロなピッチ粒子の解析に有効であり、好ましくは１００万画素以上で、粒子が鮮明に写せる画質を満たすデジタルカメラが好ましい。コンピュータは、使用する画像解析ソフトの動作環境を満たせるものであれば、特に制限はない。 Although there is no restriction | limiting in particular in the microscope to be used, The thing which can be connected with a digital camera or can display an image on a monitor or a computer is preferable from the surface of capture and preservation | save of an image. In order to sufficiently analyze the shape of pitch particles, it is desirable that the magnification can cover a magnification of 10 to 1200 times. The higher the resolution of the digital camera, the more effective it is for analyzing micro pitch particles. Preferably, the digital camera is preferably a digital camera having 1 million pixels or more and satisfying an image quality capable of clearly capturing particles. The computer is not particularly limited as long as it can satisfy the operating environment of the image analysis software to be used.
粒子面積、粒子数等の測定結果の推移は、ヒストグラムを作成することにより、容易に比較できる。また、その平均値、最大値、最小値などの代表的値で比較することができる。 The transition of measurement results such as particle area and number of particles can be easily compared by creating a histogram. In addition, comparison can be made with representative values such as an average value, a maximum value, and a minimum value.
粒子形状の判定には、例えばいびつ度、すなわち真円度（円からのズレ度合い）や、長短半径比、クラスター数などの測定値を比較することで行なうことが可能である。 The particle shape can be determined, for example, by comparing measured values such as the degree of sway, that is, the roundness (degree of deviation from the circle), the long / short radius ratio, and the number of clusters.
本発明のピッチ粒子の分析および定量化方法は、ピッチコントロール剤あるいは凝結剤を添加する前と、添加した後の比較を行なうことにより、ピッチコントロール剤の効果を評価することができる。ピッチ粒子が繊維に定着すると、測定結果で粒子数の減少が見られる。粒子数、粒子総面積が減少し、平均粒径が小さい場合は、ピッチコントロール剤が有効に働き、ピッチ粒子が繊維に定着していることを示す。粒子数が減少しても、粒子総面積の減少が見られず、１個あたりの粒子平均面積が増加している場合は、ピッチが繊維に定着せず、自己凝集を起こし粗大化していることがわかる。 In the method for analyzing and quantifying pitch particles according to the present invention, the effect of the pitch control agent can be evaluated by comparing before and after the addition of the pitch control agent or the coagulant. When the pitch particles are fixed on the fiber, the measurement results show a decrease in the number of particles. When the number of particles and the total particle area decrease and the average particle size is small, the pitch control agent works effectively, indicating that the pitch particles are fixed to the fibers. Even if the number of particles decreases, the total particle area does not decrease, and if the average particle area per particle increases, the pitch does not settle on the fibers, causing self-aggregation and coarsening. I understand.
（実施例）以下、実施例および比較例によって本発明をさらに詳しく説明するが、本発明はその要旨を超えない限り、以下の実施例に制限されるものではない。 EXAMPLES The present invention will be described in more detail with reference to the following examples and comparative examples. However, the present invention is not limited to the following examples unless it exceeds the gist.
異なるＤＩＰ（脱墨パルプ、以下ＤＩＰと略記）紙料スラリーＤＩＰ−（１）、ＤＩＰ−（２）の２種を、純水にて１０倍希釈し、上澄み液を毛細管で吸い上げ、厚さ０．２ｍｍのカウンティングチェンバー上に採取し、光学顕微鏡１２００倍で観察した。ピントを垂直方向にずらしていきながら静止画を複数枚撮影した。カウンティングチェンバー上の異なる５箇所以上で同様の操作を繰り返した。画像処理ソフト（Ｍｅｄｉａ Ｃｙｂｅｒｎｅｔｉｃｓ，ｉｎｃ． ＩＭＡＧＥ−ＰＲＯ ＰＬＵＳ Ｖｅｒ．５．０ を用い、顕微鏡画像の静止画を取込み、ＲＧＢ値のレンジ設定をＲ値（０−１９０）Ｇ値（０−１３０）Ｂ値（０−１５６）に調整することにより、目的とする粒子を抽出した。その抽出した粒子について、個数、面積、平均面積、粒径、いびつ度（円からのズレ度合い）を測定した。結果を表１に示す。 Two types of different DIP (deinked pulp, hereinafter abbreviated as DIP) paper slurry DIP- (1) and DIP- (2) were diluted 10 times with pure water, and the supernatant was sucked up by a capillary tube to obtain a thickness of 0 The sample was collected on a 2 mm counting chamber and observed with an optical microscope 1200 times. I took several still images while shifting the focus vertically. The same operation was repeated at five or more different locations on the counting chamber. Using image processing software (Media Cybernetics, inc. IMAGE-PRO PLUS Ver. 5.0), a still image of a microscopic image is captured, and the RGB value range setting is set to an R value (0-190) G value (0-130) B The target particles were extracted by adjusting the value (0 to 156), and the number, area, average area, particle size, and distorted degree (degree of deviation from the circle) of the extracted particles were measured. Is shown in Table 1.
(表１)
表１に示したように、ＤＩＰ−（１）はＤＩＰ−（２）よりも粒子数が少ないが、粒子総面積、粒子平均面積が大きく、粒子平均真円度も大きいことから、大きく、いびつな粒子が多いことがわかる。従って、ＤＩＰ−（１）の方はピッチが凝集して成長しているため、ピッチトラブルが発生しやすいことを示す。従来法のヘマサイトメーター法では、粒子数のみの判定であるため、ＤＩＰ−（１）の方が粒子は少なくきれいな系内であるとの結果しか得られないのに対し、本画像解析法ではヘマサイトメーター法に較べより抄紙系の現状を的確に表現し、抄紙系を管理する場合、どのようなアクションを次にとればよいのかの情報が得られ易いことを示している。 As shown in Table 1, DIP- (1) has a smaller number of particles than DIP- (2), but the particle total area, particle average area is large, and particle average roundness is large. It can be seen that there are many fine particles. Accordingly, DIP- (1) indicates that pitch trouble is likely to occur because the pitch is aggregated and growing. In the conventional hemacytometer method, since only the number of particles is determined, DIP- (1) can only obtain the result that the number of particles is in a clean system, whereas in this image analysis method, Compared to the hemacytometer method, the current state of papermaking is accurately expressed, and when managing papermaking, it is easy to obtain information on what action should be taken next.
ＤＩＰ―（３）紙料スラリーを、純水にて１０倍希釈し、上澄み液を毛細管で吸い上げ、厚さ０．２ｍｍのカウンティングチェンバー上に採取し、光学顕微鏡１２００倍で観察した。ピントを垂直方向にずらしていきながら静止画を複数枚撮影した。カウンティングチェンバー上の異なる５箇所以上で同様の操作を繰り返した。画像処理ソフト（Ｍｅｄｉａ Ｃｙｂｅｒｎｅｔｉｃｓ，ｉｎｃ． ＩＭＡＧＥ−ＰＲＯ ＰＬＵＳ Ｖｅｒ．５．０）を用い、静止画を取込み、ＲＧＢ値のレンジ設定をＲ値（０−１９０）Ｇ値（０−１３０）Ｂ値（０−１５６）に調整することにより、目的とする粒子を抽出した。その抽出した粒子について、個数、面積、平均面積、粒径、真円度（円からのズレ度合い）を測定した。その結果を表２に示す。 The DIP- (3) stock slurry was diluted 10-fold with pure water, the supernatant liquid was sucked up by a capillary tube, collected on a counting chamber having a thickness of 0.2 mm, and observed with an optical microscope 1200 times. I took several still images while shifting the focus vertically. The same operation was repeated at five or more different locations on the counting chamber. Image processing software (Media Cybernetics, inc. IMAGE-PRO PLUS Ver. 5.0) is used to capture a still image and set the RGB value range setting to an R value (0-190) G value (0-130) B value ( The target particles were extracted by adjusting to 0-156). For the extracted particles, the number, area, average area, particle size, and roundness (degree of deviation from the circle) were measured. The results are shown in Table 2.
ＤＩＰ―（３）に、ピッチコントロール剤として、メタクリル酸ジメチルアミノエチルの塩化メチル四級化物のホモ重合体（Ａ）（分子量３０万、カチオン当量、４．９５ｍｅｑ／ｇ）３００ｐｐｍを添加し、６０秒、２００ｒｐｍで攪拌する。純水で１０倍に希釈後、上澄み液を実施例１と同様な操作で測定した。その結果を表２に示す。 To DIP- (3), as a pitch control agent, 300 ppm of a homopolymer (A) of dimethylaminoethyl methacrylate methyl chloride quaternized product (molecular weight 300,000, cation equivalent, 4.95 meq / g) was added. Stir at 200 rpm for 2 seconds. After diluting 10 times with pure water, the supernatant was measured in the same manner as in Example 1. The results are shown in Table 2.
ＤＩＰ―（３）に、ピッチコントロール剤としてポチエチレンイミン（Ｂ）（分子量５万、カチオン当量、２１ｍｅｑ／ｇ）２００ｐｐｍを添加し、６０秒２００ｒｐｍで攪拌する。純水で１０倍に希釈後、上澄み液を実施例１と同様な操作で測定した。その結果を表２に示す。 To DIP- (3), 200 ppm of polyethyleneimine (B) (molecular weight 50,000, cation equivalent, 21 meq / g) is added as a pitch control agent, and stirred for 60 seconds at 200 rpm. After diluting 10 times with pure water, the supernatant was measured in the same manner as in Example 1. The results are shown in Table 2.
（表２）
実施例２のピッチコントロール剤未添加時の粒子数に比較し、ピッチコントロール剤を添加した実施例３と４の粒子数が減少した。実施例３と実施例４は、粒子数の減少割合はほぼ同程度であるが、実施例４は実施例３に比較し、粒子総面積が大きく、粒子平均面積も大きい。また、粒子平均真円度も高い値を示し、円からずれている粒子が多いことを示す。以上のことから、実施例３と比較し、実施例４のピッチコントロール剤は、ピッチを凝集、粗大化させていることがわかり、従って実施例３のピッチコントロール剤のほうが、ピッチコントロール剤として優れていることが明らかである。従来のヘマストメーター法では、粒子数のみの比較のため、実施例３と実施例４の優劣の判定は困難であったが、本画像解析法により、実施例３と実施例４の優劣の判定が可能となった。
Compared with the number of particles when the pitch control agent was not added in Example 2, the number of particles in Examples 3 and 4 to which the pitch control agent was added decreased. In Example 3 and Example 4, the reduction ratio of the number of particles is almost the same, but Example 4 has a larger total particle area and a larger average particle area than Example 3. In addition, the particle average roundness also shows a high value, indicating that there are many particles deviating from the circle. From the above, it can be seen that the pitch control agent of Example 4 agglomerates and coarsens the pitch compared to Example 3, and therefore the pitch control agent of Example 3 is superior as a pitch control agent. It is clear that In the conventional hematometer method, it was difficult to determine the superiority or inferiority of Example 3 and Example 4 because of the comparison of only the number of particles, but the superiority or inferiority of Example 3 and Example 4 was determined by this image analysis method. Judgment became possible.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006161857A JP4748724B2 (en) | 2006-06-12 | 2006-06-12 | Pitch control agent or coagulant evaluation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006161857A JP4748724B2 (en) | 2006-06-12 | 2006-06-12 | Pitch control agent or coagulant evaluation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2007332467A JP2007332467A (en) | 2007-12-27 |
| JP4748724B2 true JP4748724B2 (en) | 2011-08-17 |
Family
ID=38932212
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2006161857A Active JP4748724B2 (en) | 2006-06-12 | 2006-06-12 | Pitch control agent or coagulant evaluation method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP4748724B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2490006A4 (en) * | 2009-10-14 | 2018-05-02 | Nippon Paper Industries Co., Ltd. | Method for measuring degree of contaminant deposition |
| US9562861B2 (en) | 2011-04-05 | 2017-02-07 | Nalco Company | Method of monitoring macrostickies in a recycling and paper or tissue making process involving recycled pulp |
| JP6222173B2 (en) * | 2015-06-26 | 2017-11-01 | 栗田工業株式会社 | Pitch analysis method and pitch processing method |
| JP7172153B2 (en) * | 2018-06-12 | 2022-11-16 | 栗田工業株式会社 | Method for estimating amount of accumulated dirt on wire and/or felt in papermaking process |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61272639A (en) * | 1985-05-28 | 1986-12-02 | Kanzaki Paper Mfg Co Ltd | Detecting method for impurity in pulp |
| JPS63295946A (en) * | 1987-05-27 | 1988-12-02 | Oji Paper Co Ltd | Detection of foreign matter in pulp sheet material |
| JPH01244338A (en) * | 1988-03-25 | 1989-09-28 | Pfizer M S P Kk | Apparatus for counting number of pitch particles in raw material of paper and control apparatus for pitch particle |
| JPH03238346A (en) * | 1990-02-16 | 1991-10-24 | Nippon Kamiparupu Kenkyusho:Kk | Method for quantifying pitch in manufacturing process of pulp or paper |
| JP2621693B2 (en) * | 1991-07-08 | 1997-06-18 | 王子製紙株式会社 | How to control the degree of washing of kraft pulp |
| JPH0792438B2 (en) * | 1992-02-19 | 1995-10-09 | 本州製紙株式会社 | Liquid inspection device and inspection method |
| JPH10300680A (en) * | 1997-04-21 | 1998-11-13 | Mitsubishi Cable Ind Ltd | Method for inspecting foreign object in injected resin |
| EP1546367A4 (en) * | 2002-07-24 | 2006-08-16 | Univ Texas | Capture and detection of microbes by membrane methods |
-
2006
- 2006-06-12 JP JP2006161857A patent/JP4748724B2/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| JP2007332467A (en) | 2007-12-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4748724B2 (en) | Pitch control agent or coagulant evaluation method | |
| JP6059201B2 (en) | Method for monitoring macro-viscous substances during recycling process including recycled pulp and paper or dust paper manufacturing process | |
| US9280726B2 (en) | On-line macrocontaminant analyser and method | |
| WO2017210975A1 (en) | Method for monitoring distribution condition of sticky materials in pulping and papermaking system | |
| TWI689718B (en) | Resin analysis method and resin treatment method | |
| EP3714256B1 (en) | Method of measuring hydrophobic contaminants in a pulp slurry or a papermaking system | |
| Mayr et al. | Improved microscopy method for morphological characterisation of pulp fines | |
| JP4802156B2 (en) | Adhesive pitch analysis method | |
| WO2017210973A1 (en) | System and method for obtaining image of granular sticky materials in papermaking pulp | |
| TWI303527B (en) | Image inspecting apparatus, image inspecting method and computer-readable storage medium | |
| Zedel et al. | Automated Metal Cleanliness Analyzer (AMCA)—An Alternative Assessment of Metal Cleanliness in Aluminum Melts | |
| JP4747031B2 (en) | Method for detecting parameter value for image analysis processing, program for detecting parameter value for image processing, and method for counting target object using parameter value detected by them | |
| JP2004325358A (en) | Apparatus and method for measuring component ratio of cast iron | |
| JP2007333395A (en) | Method of quantitating pitch | |
| JP2022518245A (en) | How to Visualize and Quantify Biofilms on Solid Surfaces | |
| TW200825947A (en) | Microscopic image analysis method and system of microfluidic cells | |
| JP2016065821A (en) | Method for analyzing coal, apparatus for analyzing coal and computer program | |
| KR102676281B1 (en) | How to Measure Hydrophobic Contaminants in a Pulp Slurry or Paper Making System | |
| CN106644846A (en) | Method for quantitatively characterizing dispersity of solid particles in coating film | |
| Das et al. | REAL-TIME IN-LINE STICKIES, DIRT AND CONTAMINANT DETECTION IN RECYCLED PULP | |
| JP6229320B2 (en) | Sample structure classification method | |
| D'Avenio et al. | A software for analysing erythrocytes images under flow. | |
| JP2008092812A (en) | Method for measuring microbial count | |
| Tarzia et al. | A software for analysing erythrocytes images under flow | |
| Grubb et al. | The use of flow cytometry for managing extractives associated with pitch deposits |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20080804 |
|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20101029 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20101108 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20101206 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20110512 |
|
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20110513 |
|
| R150 | Certificate of patent or registration of utility model |
Free format text: JAPANESE INTERMEDIATE CODE: R150 Ref document number: 4748724 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20140527 Year of fee payment: 3 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |