JP2001349885A - Method for measuring content of mechanical pulp - Google Patents
Method for measuring content of mechanical pulpInfo
- Publication number
- JP2001349885A JP2001349885A JP2000171785A JP2000171785A JP2001349885A JP 2001349885 A JP2001349885 A JP 2001349885A JP 2000171785 A JP2000171785 A JP 2000171785A JP 2000171785 A JP2000171785 A JP 2000171785A JP 2001349885 A JP2001349885 A JP 2001349885A
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- pulp
- mechanical pulp
- content
- potassium permanganate
- measuring
- Prior art date
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Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明はパルプ又は紙中に含
まれている機械パルプの含有率の測定に関するものであ
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to the measurement of the content of mechanical pulp contained in pulp or paper.
【0002】[0002]
【従来の技術】従来、パルプ又は紙中に含まれている機
械パルプの含有率を測定する方法としては、主に、
(1)試料を染色液(例えば、C染色液、Herzberg染色
液、Lofton-merritt染色液、Wilson染色液、Alexander
染色液あるいはKantrowitz-Simmons染色液等)で染色し
た後に顕微鏡を用いて繊維を一本ずつ観察する方法、
(2)試料を塩酸フロログリシン溶液に浸漬し、発色し
た色を標準紙と比色して測定する比色法、(3)試料と
塩酸フロログリシンを反応させ、その消費した塩酸フロ
ログリシン量を定量することによる測定法、(4)試料
中の機械パルプに含まれているリグニンを酸処理にて単
離し、重量測定によって求める方法等、が使われてき
た。2. Description of the Related Art Conventionally, methods for measuring the content of mechanical pulp contained in pulp or paper mainly include:
(1) Samples were stained (eg, C stain, Herzberg stain, Lofton-merritt stain, Wilson stain, Alexander stain)
Stained with staining solution or Kantrowitz-Simmons staining solution), and then observe the fibers one by one using a microscope.
(2) A colorimetric method in which a sample is immersed in a phloroglysin hydrochloride solution, and the developed color is measured by colorimetry with a standard paper. A measuring method by quantification, (4) a method of isolating lignin contained in mechanical pulp in a sample by an acid treatment, and measuring the lignin by weight measurement, and the like have been used.
【0003】ただし、これらの方法にはそれぞれ以下の
ような欠点がある。However, each of these methods has the following disadvantages.
【0004】(1)の顕微鏡を用いる方法では、パルプ
は複数の細胞種から成り立っている上、繊維を一本ずつ
観察していくため膨大な時間がかかり、測定繊維数も限
られてしまい、誤差が大きく、個人差も出やすい。
(2)の塩酸フロログリシン溶液による比色法について
は、特に機械パルプの含有率が高くなると非常に正確度
が低くなることが知られている(紙パルプ製造技術シリ
ーズ9 「紙パルプの試験法」 P221、紙パルプ技
術協会編)。(3)の試料と塩酸フロログリシンを反応
させ、その消費した塩酸フロログリシン量を定量するこ
とによる測定法及び(4)の機械パルプ中に含まれてい
るリグニンを酸処理にて単離し、重量測定によって求め
る方法は、反応時間あるいは処理に一日以上かかり、ま
た、正確度が非常に低い(前記「紙パルプの試験法」、
p221)。In the method (1) using a microscope, pulp is composed of a plurality of cell types, and it takes an enormous amount of time to observe fibers one by one, and the number of measured fibers is limited. Errors are large and individual differences are easy to appear.
It is known that the accuracy of the colorimetric method (2) using a phloroglysin hydrochloride solution is extremely low particularly when the content of the mechanical pulp is high (Paper pulp production technology series 9 "Test method for paper pulp"). P221, Japan Association of Paper and Pulp Technology). The sample of (3) is reacted with phloroglysin hydrochloride to measure the consumed phloroglysin hydrochloride, and the lignin contained in the mechanical pulp of (4) is isolated by acid treatment, The method obtained by measurement requires a reaction time or a treatment of one day or more, and has extremely low accuracy (the above-mentioned “paper pulp test method”,
p221).
【0005】[0005]
【発明が解決しようとする課題】この発明は上記のごと
き従来の方法の欠点を解消すべく、簡便にかつ短時間で
正確にパルプ又は紙のような繊維集合体または該繊維集
合体原料中に含まれている機械パルプ含有率を求める方
法を提供するためになされたものである。SUMMARY OF THE INVENTION The present invention solves the above-mentioned drawbacks of the conventional method by simply, accurately and quickly preparing a fiber aggregate such as pulp or paper or a raw material of the fiber aggregate. It is intended to provide a method for determining the content of mechanical pulp contained.
【0006】[0006]
【課題を解決するための手段】本発明者らは、パルプ又
は紙のような繊維集合体または該繊維集合体原料中に含
まれている機械パルプ含有率測定方法について、鋭意研
究を重ねた。その結果、その機械パルプ中に含まれてい
るリグニンによる過マンガン酸カリウムやその他漂白薬
品の消費反応を利用することにより、その機械パルプ含
有率を簡便かつ短時間で正確に測定できることを見いだ
し、この知見にもとづいて本発明を完成するに至った。Means for Solving the Problems The present inventors have intensively studied a method for measuring the content of mechanical pulp contained in a fiber aggregate such as pulp or paper or a raw material of the fiber aggregate. As a result, it was found that by utilizing the consumption reaction of potassium permanganate and other bleaching chemicals by lignin contained in the mechanical pulp, the mechanical pulp content could be measured easily and accurately in a short time. The present invention has been completed based on the knowledge.
【0007】[0007]
【発明の実施の形態】本発明において、パルプ又は紙の
ような繊維集合体または該繊維集合体原料中に含まれて
いる機械パルプ中に含まれるリグニンとの反応に用いる
薬品としては、過マンガン酸カリウム、あるいはその他
次亜塩素酸ナトリウム、その他の薬品として塩素、亜塩
素酸、二酸化塩素及び過酸化水素がある。このうち、過
マンガン酸カリウムを用いる場合は、反応条件として、
カッパー価(ISO 302、JIS P8211、TAPPI 236)や過マ
ンガン酸カリウム価(K価と略す。JIS 8206等)に規定
されている試験方法、あるいはこれに準じた試験方法を
そのまま適用できる。本発明に使用するカッパー価と
は、絶乾質量1g相当のパルプが25℃で消費するN/10
過マンガン酸カリウム溶液のml数を、加えた過マンガン
酸カリウムの50%が消費されるときの値に補正したも
のと定義される。また、K価とは、一定条件下で絶乾試
料1gが吸収する0.1N過マンガン酸カリウム溶液の
ml数と定義される。本発明では何れの方法、あるいは
これらに準じた形で試料及び薬品の量を変更した方法
等、いずれを用いても良い。これらは、入手できる試料
の絶対量等にあわせて適宜選択すればよい。カッパー価
及びK価の測定時間はそれぞれ10分、5分と非常に短
い。BEST MODE FOR CARRYING OUT THE INVENTION In the present invention, the chemical used for the reaction with lignin contained in a fibrous aggregate such as pulp or paper or mechanical pulp contained in the fibrous aggregate raw material is permanganese. Potassium acid, or other sodium hypochlorite, and other chemicals include chlorine, chlorite, chlorine dioxide, and hydrogen peroxide. Of these, when potassium permanganate is used, the reaction conditions are as follows:
The test method specified in the kappa number (ISO 302, JIS P8211, TAPPI 236) or potassium permanganate value (abbreviated as K value; JIS 8206, etc.) or a test method based thereon can be applied as it is. The kappa number used in the present invention is defined as N / 10 that pulp equivalent to 1 g of absolute dry mass consumes at 25 ° C.
It is defined as the number of ml of potassium permanganate solution corrected to the value at which 50% of the added potassium permanganate is consumed. The K value is defined as the number of ml of a 0.1N potassium permanganate solution absorbed by 1 g of an absolutely dry sample under certain conditions. In the present invention, any method or a method in which the amounts of the sample and the chemical are changed in a form according to these methods may be used. These may be appropriately selected according to the absolute amount of the available sample and the like. The measurement times for the kappa number and the K number are very short, 10 minutes and 5 minutes, respectively.
【0008】また、過マンガン酸カリウム以外の漂白薬
品としては次亜塩素酸ナトリウム、その他の薬品、塩
素、亜塩素酸、二酸化塩素、過酸化水素等を用いること
ができるが、リグニンとの反応の選択性や、操作の簡便
性等の点で、次亜塩素酸ナトリウムが望ましい。消費量
を測定する方法としてはISO 3260またはTAPPI T253の方
法が、17分で測定が完了すること等から望ましい。As a bleaching chemical other than potassium permanganate, sodium hypochlorite, other chemicals, chlorine, chlorite, chlorine dioxide, hydrogen peroxide and the like can be used. Sodium hypochlorite is desirable in terms of selectivity and simplicity of operation. As a method of measuring the consumption, the method of ISO 3260 or TAPPI T253 is preferable because the measurement is completed in 17 minutes.
【0009】本発明に適用できるパルプ又は紙のような
繊維集合体または該繊維集合体原料はスラリー状にでき
ればどんなものでもよく、抄紙原料、未印刷用紙、印刷
用紙などが適用できる。ただし、灰分や過マンガン酸カ
リウム、漂白薬品を消費するものを含んでいるときは補
正を必要とする。補正の方法は以下の通りである。The fibrous aggregate such as pulp or paper or the raw material of the fibrous aggregate applicable to the present invention may be any material as long as it can be made into a slurry. Papermaking raw materials, unprinted paper, printing paper and the like can be used. However, when ash, potassium permanganate, and those that consume bleaching chemicals are included, correction is required. The correction method is as follows.
【0010】灰分:試料の灰分量をISO1762−19
74の方法、JIS P8204の方法およびTAPPI
T211のいずれかの方法で求め、その重量を試料重量
から差し引いて算出する。Ash content: The ash content of the sample was determined to be ISO 1762-19.
74 method, JIS P8204 method and TAPPI
It is obtained by any method of T211 and the weight is subtracted from the sample weight to calculate.
【0011】過マンガン酸カリウムや漂白薬品を消費す
るものを含んでいるもの:あらかじめ成分を分析し、そ
れに消費される分を計算して補正する。[0011] Those containing potassium permanganate or those consuming bleaching chemicals: Analyze the components in advance and calculate and correct the amount consumed.
【0012】ただし、通常、パルプ又は紙のような繊維
集合体または該繊維集合体原料中には機械パルプ中に含
まれているリグニン以外過マンガン酸カリウムや漂白薬
品を消費するものはほとんどなく、補正で重要なのは灰
分だけである。However, in general, there is almost no fiber aggregate such as pulp or paper or raw material of the fiber aggregate that consumes potassium permanganate or bleaching chemicals other than lignin contained in mechanical pulp. Only the ash is important in the correction.
【0013】また、鋭意研究した結果、機械パルプの樹
種、製造法の差は、晒または未晒化学パルプと機械パル
プとの差に比べれば非常に少ないことが分かり、従っ
て、上記方法はどの機械パルプがどのように配合されて
いても測定可能である。Further, as a result of diligent research, it has been found that the difference in mechanical pulp tree species and manufacturing method is very small compared to the difference between bleached or unbleached chemical pulp and mechanical pulp. It can be measured no matter how the pulp is blended.
【0014】機械パルプ含有率とカッパー価、K価、P
N、漂白薬品消費量等との関係は、過マンガン酸カリウ
ムおよび漂白薬品の消費がない広葉樹漂白クラフトパル
プに機械パルプを混入し、その混合パルプを測定するこ
とにより簡単に検量線を作成することができる。以下
に、カッパー価を例にとった結果を示す。[0014] Mechanical pulp content and kappa number, K number, P
The relationship with N, bleaching chemical consumption, etc. is to create a calibration curve easily by mixing mechanical pulp with hardwood bleached kraft pulp that does not consume potassium permanganate and bleaching chemicals, and measuring the mixed pulp. Can be. The results obtained by taking the kappa number as an example are shown below.
【0015】カッパー価は、機械パルプの種類を問わ
ず、 (カッパー価)=a ×(機械パルプの含有率 %) a:1.4〜1.7 従って、この式に試料のカッパー価を代入することによ
り、機械パルプの配合率を求めることができる。Regarding the kappa number, irrespective of the type of mechanical pulp, (kappa number) = a × (content ratio of mechanical pulp%) a: 1.4 to 1.7 Therefore, the kappa number of the sample is substituted into this equation. By doing so, the blending ratio of the mechanical pulp can be determined.
【0016】また、過マンガン酸カリウム以外の漂白薬
品を用いた場合においても、これと同様に広葉樹クラフ
トパルプに機械パルプを混入し、その混合パルプを測定
することにより、簡便に検量線を作成することができ、
容易に上式のaに相当する値を求めることができる。When a bleaching chemical other than potassium permanganate is used, a mechanical curve is similarly mixed with hardwood kraft pulp, and the mixed pulp is measured to easily prepare a calibration curve. It is possible,
A value corresponding to a in the above equation can be easily obtained.
【0017】[0017]
【発明の効果】本発明による方法ではカッパー価、K
価、PN、漂白薬品消費量の測定を利用することにより、
簡便かつ正確に機械パルプ含有率を求めることができ
る。According to the method of the present invention, kappa number, K
By using measurements of price, PN, and bleaching chemical consumption,
The content of the mechanical pulp can be obtained simply and accurately.
【0018】[0018]
【実施例】以下に実施例を挙げて本発明をより具体的に
示すが、本発明は勿論かかる実施例に限定されるもので
はない。 [実施例1]広葉樹漂白クラフトパルプと機械パルプと
を重量比9:1に配合したパルプについて、JIS P 8
211に従ってカッパー価を測定し、メカニカルパルプ
の含有率を測定した。測定は異なる2人(測定者A、及
びB)によっておこなった。灰分をJISP8204の方法
で求めた後、カッパー価を補正し、機械パルプの含有率
を以下の式に従って求めた。EXAMPLES The present invention will be described in more detail with reference to the following Examples, but it should be understood that the present invention is by no means restricted to such Examples. [Example 1] A pulp obtained by blending a hardwood bleached kraft pulp with a mechanical pulp at a weight ratio of 9: 1 was applied to JIS P8.
The kappa number was measured according to 211, and the mechanical pulp content was measured. The measurement was performed by two different persons (measures A and B). After the ash content was determined by the method of JISP8204, the kappa number was corrected, and the content of the mechanical pulp was determined according to the following equation.
【0019】 (カッパー価)=a ×(機械パルプの含有率 %) a:1.4〜1.7 aには範囲があるので、機械パルプの含有率も範囲をも
った値となる。測定時間を含めて結果を表1に示した。 [実施例2]測定試料を広葉樹漂白クラフトパルプと機
械パルプとを重量比6:4に配合したパルプとした以外
は実施例1と同様な操作を行った。結果を表1に示し
た。 [実施例3]測定試料を広葉樹漂白クラフトパルプと機
械パルプとを重量比4:6に配合したパルプとした以外
は実施例1と同様な操作を行った。結果を表1に示し
た。 [実施例4]測定試料を広葉樹漂白クラフトパルプと機
械パルプとを重量比1:9に配合したパルプとした以外
は実施例1と同様な操作を行った。結果を表1に示し
た。 [実施例5]測定試料を広葉樹漂白クラフトパルプと機
械パルプとを重量比5:3に配合したパルプに炭酸カル
シウム20重量%加えた物とした以外は実施例1と同様
な操作を行った。結果を表1に示した。 [実施例6]測定試料を広葉樹漂白クラフトパルプと機
械パルプとを重量比5:4に配合したパルプに炭酸カル
シウム5重量%及びタルク5重量%加えた物とした以外
は実施例1と同様な操作を行った。結果を表1に示し
た。 [比較例1]比較例1に用いたパルプをTAPPI標準法T
401に従って測定した。結果を表1に示した。 [比較例2]比較例2に用いたパルプをTAPPI標準法T
401に従って測定した。結果を表1に示した。 [比較例3]比較例3に用いたパルプをTAPPI標準法T
401に従って測定した。結果を表1に示した。 [比較例4]比較例4に用いたパルプをTAPPI標準法T
401に従って測定した。結果を表1に示した。 [比較例5]比較例5に用いたパルプをTAPPI標準法T
401に従って測定した。結果を表1に示した。 [比較例6]比較例6に用いたパルプをTAPPI標準法T
401に従って測定した。結果を表1に示した。(Kappa number) = a × (mechanical pulp content%) a: Since 1.4 to 1.7 a has a range, the content of the mechanical pulp also has a value having a range. Table 1 shows the results including the measurement time. [Example 2] The same operation as in Example 1 was performed except that the measurement sample was pulp in which the hardwood bleached kraft pulp and the mechanical pulp were mixed at a weight ratio of 6: 4. The results are shown in Table 1. [Example 3] The same operation as in Example 1 was performed except that the measurement sample was pulp in which the hardwood bleached kraft pulp and the mechanical pulp were mixed at a weight ratio of 4: 6. The results are shown in Table 1. Example 4 The same operation as in Example 1 was performed, except that the measurement sample was pulp in which a hardwood bleached kraft pulp and a mechanical pulp were mixed at a weight ratio of 1: 9. The results are shown in Table 1. Example 5 The same operation as in Example 1 was carried out except that the measurement sample was a mixture of bleached hardwood kraft pulp and mechanical pulp in a weight ratio of 5: 3, and 20% by weight of calcium carbonate was added. The results are shown in Table 1. [Example 6] The same as Example 1 except that the measurement sample was a pulp obtained by mixing a hardwood bleached kraft pulp and a mechanical pulp at a weight ratio of 5: 4 and adding 5% by weight of calcium carbonate and 5% by weight of talc. The operation was performed. The results are shown in Table 1. [Comparative Example 1] The pulp used in Comparative Example 1 was prepared using TAPPI standard method T.
Measured according to 401. The results are shown in Table 1. [Comparative Example 2] The pulp used in Comparative Example 2 was prepared using TAPPI standard method T.
Measured according to 401. The results are shown in Table 1. [Comparative Example 3] The pulp used in Comparative Example 3 was prepared using TAPPI standard method T.
Measured according to 401. The results are shown in Table 1. Comparative Example 4 The pulp used in Comparative Example 4 was prepared using TAPPI standard method T.
Measured according to 401. The results are shown in Table 1. [Comparative Example 5] The pulp used in Comparative Example 5 was prepared using TAPPI standard method T.
Measured according to 401. The results are shown in Table 1. Comparative Example 6 The pulp used in Comparative Example 6 was prepared using TAPPI standard method T
Measured according to 401. The results are shown in Table 1.
【0020】[0020]
【発明の効果】本発明の方法は、実際の機械パルプの含
有率と測定した機械パルプの含有率との誤差は非常に少
なく、また、個人差もなかった。一方、従来法では測定
誤差が非常に大きく、また、個人差も大きかった。また
測定時間も本発明方法の方が遙かに短かった。According to the method of the present invention, the error between the actual mechanical pulp content and the measured mechanical pulp content was very small, and there was no individual difference. On the other hand, in the conventional method, the measurement error was very large, and individual differences were also large. The measurement time was much shorter in the method of the present invention.
【0021】[0021]
【表1】 [Table 1]
───────────────────────────────────────────────────── フロントページの続き (72)発明者 田部井 宏一 東京都北区王子5丁目21番1号 日本製紙 株式会社内 Fターム(参考) 4L055 DA03 DA04 ────────────────────────────────────────────────── ─── Continued on the front page (72) Inventor Koichi Tabei 5-21-1, Oji, Kita-ku, Tokyo Nippon Paper Industries Co., Ltd. F-term (reference) 4L055 DA03 DA04
Claims (5)
含まれている機械パルプの含有量を測定するにあたり、
前記繊維集合体または該繊維集合体原料の試料をスラリ
ー状にした後、過マンガン酸カリウムまたは漂白薬品を
添加し、添加した過マンガン酸カリウムまたは漂白薬品
の消費を測定することにより、前記試料中の機械パルプ
の含有率を測定することを特徴とする方法。In measuring the content of mechanical pulp contained in a fiber aggregate or a raw material of the fiber aggregate,
After the sample of the fiber aggregate or the raw material of the fiber aggregate is slurried, potassium permanganate or a bleaching agent is added, and the consumption of the added potassium permanganate or the bleaching agent is measured. Measuring the content of the mechanical pulp.
にあたり、カッパー価測定法を用いることを特徴とする
請求項1の方法。2. The method according to claim 1, wherein in measuring the consumption of potassium permanganate, a kappa number measuring method is used.
にあたり、JIS法K価測定法またはTappi法PN測定法を用
いることを特徴とする請求項1の方法。3. The method according to claim 1, wherein in measuring the consumption of potassium permanganate, a JIS K value measurement method or a Tappi method PN measurement method is used.
トリウムを用い、塩素消費量を測定することを特徴とす
る請求項1の方法。4. The method according to claim 1, wherein chlorine or sodium hypochlorite is used as a bleaching chemical, and chlorine consumption is measured.
用い、塩素消費量を測定するにあたり、ISO3260またはT
APPI T253の方法で定量することを特徴とする請求項1
の方法。5. When measuring chlorine consumption using sodium hypochlorite as a bleaching chemical, ISO 3260 or T
The amount is determined by the method of APPI T253.
the method of.
Priority Applications (1)
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JP2000171785A JP2001349885A (en) | 2000-06-08 | 2000-06-08 | Method for measuring content of mechanical pulp |
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CN104459089A (en) * | 2014-12-12 | 2015-03-25 | 东北大学 | Soft measurement method of freeness of high-consistency pulp grinding system |
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CN104459089A (en) * | 2014-12-12 | 2015-03-25 | 东北大学 | Soft measurement method of freeness of high-consistency pulp grinding system |
CN104459089B (en) * | 2014-12-12 | 2016-05-11 | 东北大学 | A kind of flexible measurement method of high consistency refining system freedom |
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