JPS628148B2 - - Google Patents
Info
- Publication number
- JPS628148B2 JPS628148B2 JP55045725A JP4572580A JPS628148B2 JP S628148 B2 JPS628148 B2 JP S628148B2 JP 55045725 A JP55045725 A JP 55045725A JP 4572580 A JP4572580 A JP 4572580A JP S628148 B2 JPS628148 B2 JP S628148B2
- Authority
- JP
- Japan
- Prior art keywords
- pulp
- slurry
- value
- sample
- potassium permanganate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 238000000034 method Methods 0.000 claims description 27
- 239000013055 pulp slurry Substances 0.000 claims description 27
- 239000012286 potassium permanganate Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000010411 cooking Methods 0.000 claims description 13
- 239000002002 slurry Substances 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 11
- 239000000835 fiber Substances 0.000 claims description 9
- 238000010790 dilution Methods 0.000 claims description 7
- 239000012895 dilution Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000004448 titration Methods 0.000 claims description 6
- 239000002699 waste material Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 238000002834 transmittance Methods 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000000691 measurement method Methods 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims 1
- 238000005259 measurement Methods 0.000 description 12
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 238000002835 absorbance Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 6
- 235000019345 sodium thiosulphate Nutrition 0.000 description 6
- 229920002472 Starch Polymers 0.000 description 5
- 235000019698 starch Nutrition 0.000 description 5
- 239000008107 starch Substances 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- 238000004061 bleaching Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000013505 freshwater Substances 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002655 kraft paper Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical class C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/34—Paper
- G01N33/343—Paper pulp
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Paper (AREA)
Description
【発明の詳細な説明】
本発明は未晒パルプの過マンガン酸カリ価(以
下、K価と略称する)の測定法に関し、特にパル
プ製造工程から連続的に試料を採取し測定する総
べての操作と測定値の算出までを自動的に実施す
る方法に係るものである。Detailed Description of the Invention The present invention relates to a method for measuring the potassium permanganate value (hereinafter abbreviated as K value) of unbleached pulp, and in particular to a method for measuring the permanganate potassium value (hereinafter abbreviated as K value) of unbleached pulp. This relates to a method for automatically performing operations up to the calculation of measured values.
パルプのK価は脱リグニン度の指標として測定
されており、K価に基づいて漂白条件が設定され
るだけでなく、蒸解工程における種々の変動、即
ち蒸解薬品添加量、蒸解温度、木材チツプに随伴
される水分などの蒸解度への影響因子の変動を把
握する手段としても有用な数値である。K価は被
検試料による硫酸酸性の一定条件下における過マ
ンガン酸カリ消費量から計算されるが、その測定
方法はJIS P8206に規定されている通りである。
一般には、この標準法に基づいて手分析で測定さ
れているが省力化を計るために自動測定装置が開
発されている。しかしながら、この自動測定装置
と雖もパルプ試料を精秤した上で測定に供する必
要があるので可成りの人手を要し、また迅速性に
も乏しいのが現状である。 The K number of pulp is measured as an index of the degree of delignification, and bleaching conditions are not only set based on the K number, but also various changes in the cooking process, such as the amount of cooking chemicals added, the cooking temperature, and the wood chips. This value is also useful as a means of understanding changes in factors that affect the degree of digestion, such as accompanying moisture. The K value is calculated from the amount of potassium permanganate consumed by the test sample under certain conditions of sulfuric acid acidity, and the measurement method is as specified in JIS P8206.
Generally, measurements are carried out by manual analysis based on this standard method, but automatic measuring devices have been developed to save labor. However, the current situation is that this automatic measuring device requires a considerable amount of manpower and is not very quick, since it is necessary to precisely weigh the pulp sample before using it for measurement.
上記実情に鑑み本発明者等はK価の測定に関し
種々の方法を検討した結果、パルプ製造工程から
連続的にパルプスラリー試料を採取して測定操作
の総べてと測定値の算出とを自動的に実施するこ
との可能な完全自動化迅速K価測定方法を完成し
た。 In view of the above circumstances, the inventors of the present invention investigated various methods for measuring the K number, and as a result, they decided to automatically collect pulp slurry samples from the pulp manufacturing process and automatically perform all measurement operations and calculate the measured values. We have completed a fully automated rapid K value measurement method that can be carried out on a daily basis.
以下にこの方法について詳細説明する。 This method will be explained in detail below.
K価測定を必要とする段階における未晒パルプ
は通常、蒸解排液と未蒸解物(所謂、ノツト粕、
綿状粕であり、以下“粕”と呼ぶこととする)を
随伴しており、K価測定用試料から之等を分離す
る必要がある。工業的には蒸解排液の分離洗浄に
は通常の場合、各種スクリーン若しくはウオータ
ー・サイクロンが用いられている。しかしK価測
定用試料の場合は試料の量が少なくてよいし、ま
た迅速に蒸解排液及び粕を分離することが望まし
く、自動的にこの操作をなし得る方法について
種々検討研究を行なつた結果、以下に示す方法な
いし装置によることが適切であることを究明し
た。 Unbleached pulp at the stage where K value measurement is required is usually made up of cooking waste and undigested material (so-called knot lees,
It is a flocculent lees (hereinafter referred to as "lees"), and it is necessary to separate it from the sample for K value measurement. Industrially, various screens or water cyclones are usually used to separate and wash the cooking waste. However, in the case of samples for K value measurement, the amount of sample may be small, and it is desirable to quickly separate the cooking waste and lees, and various research studies have been conducted on ways to automatically perform this operation. As a result, it was determined that the following method or apparatus was appropriate.
先ず蒸解後にパルプ工程から分岐して採取され
た試料をパルプ繊維が通過しない程度の目開きの
網またはスリツト上に導びき、蒸解排液を脱液し
ながら洗浄水シヤワーによつて水洗するが、自動
的にこの操作を実施するには横置した円筒若しく
は円錐台の周面が網若しくはスリツトで形成され
た回転体を用いるのが最も良い。次いで粕除去の
ためにはパルプ繊維のみが通過可能な目開きの網
若しくはスリツトを使用するのが良いが、円筒若
しくは円錐台の周面が網若しくはスリツトで形成
された回転体を使用し、しかも該回転体を横置し
て回転せしめるのが最も効果的である。更に蒸解
排液の分離、洗浄装置と粕除去装置とを連結して
回転させるのが良いことは言うまでもない。 First, a sample collected from the pulping process after cooking is guided onto a mesh or slit with openings that do not allow pulp fibers to pass through, and is washed with water using a washing water shower while removing the cooking liquid. In order to automatically carry out this operation, it is best to use a rotating body that is a horizontally placed cylinder or truncated cone whose circumferential surface is formed of a net or slits. Next, in order to remove the lees, it is better to use a mesh or slits with openings that allow only pulp fibers to pass through, but it is better to use a rotating body with a cylindrical or truncated conical surface formed of a mesh or slits, and It is most effective to rotate the rotating body horizontally. Furthermore, it goes without saying that it is better to connect and rotate the cooking waste liquid separation and washing device and the lees removing device.
即ち第1図はその一例であつて回転式洗浄・粕
除去装置の概略を示す側断面図であり、円筒状若
しくは円錐台状の装置が横置された状態に据付け
られているものであり、その周面前段1に40メツ
シユ程度の目開きの小さい網若しくはスリツト
が、また周面後段2には15〜20メツシユ程度の目
開きの大きい網若しくはスリツトが夫々配設され
ており、導入口3から未晒パルプ試料を導入し洗
浄水ライン4から洗浄水をシヤワーし、回転中心
5の周りを20〜40r.p.m.で回転させ、前段排出口
6から洗浄排液を、また後段排出口7から粕を排
出すると同時にK価測定用パルプスラリーを取出
口8から取り出すことが可能な装置を用いるのが
好適である。 That is, FIG. 1 is an example of this, and is a side sectional view showing the outline of a rotary washing and dregs removing device, in which a cylindrical or truncated conical device is installed horizontally. A net or slit with a small opening of about 40 meshes is provided on the front stage 1 of the peripheral surface, and a net or slit with a large opening of about 15 to 20 meshes is arranged on the rear stage 2 of the peripheral surface, and an inlet 3 is provided. An unbleached pulp sample is introduced from the washing water line 4, the washing water is showered from the washing water line 4, the rotation center 5 is rotated at 20 to 40 rpm, and the washing liquid is discharged from the front stage discharge port 6 and the second stage discharge port 7. It is preferable to use a device that is capable of taking out the pulp slurry for K value measurement from the outlet 8 at the same time as discharging the lees.
次に一定重量のパルプ試料の採取方法について
述べる。 Next, the method for collecting pulp samples of a certain weight will be described.
パルプは、その製造工程において通常20〜0.1
%の範囲内の濃度のスラリー状で存在している
が、そのパルプスラリーから一定重量のパルプ試
料を採取するには適当量のパルプスラリーを採取
してから之を乾燥し、所定量を秤量する方法が考
えられる。しかし、乾燥、秤量の操作を迅速、且
つ自動的に実施することは相当困難であり、また
乾燥方法によつてはパルプ繊維が角質化して後述
するK価測定時に単繊維への離解が不良となつて
過マンガン酸カリとの反応が不充分となつて正確
な測定結果が得られなくなる恐れがあり、またパ
ルプ繊維の変質により異なる測定値となる場合も
あり得る。 During the manufacturing process, pulp is usually 20 to 0.1
It exists in the form of a slurry with a concentration within the range of 1.5%, but in order to collect a certain weight of pulp sample from the pulp slurry, an appropriate amount of pulp slurry must be collected, dried, and weighed to a predetermined amount. There are possible ways. However, it is quite difficult to carry out drying and weighing operations quickly and automatically, and depending on the drying method, the pulp fibers may become keratinized, resulting in poor disintegration into single fibers during the K value measurement described below. As a result, the reaction with potassium permanganate may become insufficient and accurate measurement results may not be obtained, and there may be cases where different measurement values are obtained due to deterioration of the pulp fibers.
また一定重量のパルプ試料を採取するにはパル
プスラリーの濃度を知つて、それから逆算して一
定容量を採取する方法が考えられる。パルプスラ
リーの濃度測定方法として従来から
(i) パルプスラリーが管路を通過する時の圧力損
失とパルプ濃度との関係
(ii) パルプスラリー中で回転翼を一定速度で回転
させるのに要するトルクとパルプ濃度との関係
(iii) パルプスラリー中で一定トルクで回転してい
る円板、若しくは円錐体の回転速度とパルプ濃
度との関係
などを利用する方法が知られている。 In addition, in order to collect a pulp sample of a constant weight, it is possible to know the concentration of the pulp slurry and then calculate backwards to collect a constant volume. Conventional methods for measuring the concentration of pulp slurry include (i) the relationship between pressure loss and pulp concentration when the pulp slurry passes through a pipe, and (ii) the torque required to rotate a rotor at a constant speed in the pulp slurry. Relationship with Pulp Concentration (iii) A method is known that utilizes the relationship between pulp concentration and the rotational speed of a disk or cone rotating at a constant torque in pulp slurry.
之等の方法の中で(ii)及び(iii)の方法が実用化され
ているが、何れの方法もスラリーの力学的特性を
利用しているので測定精度は良好でなく、スラリ
ー濃度の高低にもよるが10〜30%程度の誤差が生
じることは不可避である。 Among these methods, methods (ii) and (iii) have been put into practical use, but since both methods utilize the mechanical properties of the slurry, the measurement accuracy is not good, and It is inevitable that there will be an error of about 10 to 30%, depending on the situation.
上記のために本発明者等はパルプスラリーの濃
度を高精度で測定する方法について種々検討研究
した結果、第2図で示したパルプスラリー濃度と
吸光度との関係の一例の様にパルプスラリー層を
通過する光の透過光量とパルプ濃度との間に密接
な関係の存在することを見出した。即ち一定厚み
のパルプスラリー層の一方から光を入射させた時
に入射光(Ii)及び透過光(It)とパルプ濃度(C)
との相互間に次式の関係が成立することを判明し
た。 For the purpose of the above, the present inventors have conducted various studies and research on methods for measuring the concentration of pulp slurry with high accuracy. As a result, as shown in the example of the relationship between pulp slurry concentration and absorbance shown in Figure 2, the present inventors have It has been found that there is a close relationship between the amount of transmitted light and pulp density. In other words, when light is incident from one side of a pulp slurry layer of a constant thickness, the incident light (Ii), transmitted light (It), and pulp density (C)
It was found that the following relationship holds true between .
C=k(−logIt/Ii)
ここにk:定数
上式における−log(It/Ii)は所謂、吸光度と
呼
ばれるものであつて、パルプスラリーの吸光度測
定値からパルプ濃度を正確に決定することが出来
ることを究明した。 C=k(-logIt/Ii) where k: constant In the above equation, -log(It/Ii) is what is called absorbance, and the pulp concentration can be accurately determined from the measured absorbance of the pulp slurry. We found out that it is possible.
なお茲で用いることの出来る光は任意のスペク
トルを有する光でもよいが、パルプスラリー層内
における光の散乱が少ない程良いことは言うまで
もなく、そのためには可視部における比較的高波
長の単色光を用いるのが好適であり、第2図のデ
ータはLUKPスラリーの濃度と600nmの単色光の
吸光度との関係を示したものである。 Although the light that can be used in the ink may have any spectrum, it goes without saying that the less scattering of light within the pulp slurry layer, the better. The data in FIG. 2 shows the relationship between the concentration of LUKP slurry and the absorbance of monochromatic light at 600 nm.
また透過光を検出して後述の目的のために電気
的信号に変換する必要があるが、光電管、光電子
増倍管、光検出ダイオードなどの検出器を任意に
選択して使用することが出来る。 Although it is necessary to detect the transmitted light and convert it into an electrical signal for the purpose described later, any detector such as a phototube, photomultiplier tube, or photodetection diode can be selected and used.
以上の様にしてパルプスラリー濃度を測定し、
パルプ繊維の所要重量から逆算した所定容量のパ
ルプスラリーを採取すればよいこととなるが、そ
のためには次に示す二つの方法の何れかを採用す
るのが適当である。 The pulp slurry concentration was measured as described above,
It is sufficient to collect a predetermined volume of pulp slurry calculated backward from the required weight of pulp fibers, and for this purpose, it is appropriate to adopt one of the following two methods.
第一の方法は蒸解排液と粕とを分離した精選未
晒パルプスラリーの任意量を第3図に示した装置
によつて採取する。即ち希釈槽9に精選未晒パル
プスラリーの任意量を投入し、ポンプ10で配管
系11を循環させながら配管系11の中に設置さ
れているフローセル12中で光源13からの光を
照射し検出器14で連続的に透過光を測定する一
方、別の清水ラインから希釈水を注入するが、所
定パルプ濃度、即ち所定吸光度に達した時に検出
器14からの電気的信号で清水ラインの電磁弁1
5を閉じ、希釈槽内のパルプスラリーの一定容量
を計量すればよい。この時の採取容量を或る一定
値に定めておけばK価測定用パルプ試料量は定め
られているので、採取スラリーのパルプ濃度が必
然的に定まる訳であり、之に対応するスラリーの
吸光度を予め実験的に求めておけば以上の様な操
作は極めて容易に実施することが可能である。 The first method is to collect an arbitrary amount of selected unbleached pulp slurry from which cooking waste and lees have been separated using the apparatus shown in FIG. That is, an arbitrary amount of selected unbleached pulp slurry is put into the dilution tank 9, and while circulating through the piping system 11 with the pump 10, light from the light source 13 is irradiated into the flow cell 12 installed in the piping system 11 for detection. While the transmitted light is continuously measured by the detector 14, dilution water is injected from another fresh water line, and when a predetermined pulp concentration, that is, a predetermined absorbance is reached, an electric signal from the detector 14 triggers the electromagnetic valve of the fresh water line. 1
5 and then measure a certain volume of pulp slurry in the dilution tank. If the collection volume at this time is set to a certain constant value, the amount of pulp sample for K value measurement is determined, so the pulp concentration of the collected slurry is inevitably determined, and the absorbance of the slurry corresponding to this is determined. The operations described above can be carried out extremely easily if is determined experimentally in advance.
第二の方法は第一の方法の場合と同様に第4図
に概略図を示した装置を使用し、蒸解排液と粕と
を分離した精選未晒パルプの任意量を容器16に
投入し、任意量の水で希釈してスラリーを調製
し、このスラリーをポンプ10で抜き出してフロ
ーセル12へ送り、光源13からの光を照射して
検出器14で透過光を測定し、予め実験により求
めておいた吸光度とスラリー濃度との関係から一
定重量に相当するスラリー液量を自動的に算出
し、その量を計算すればよい。 In the second method, as in the case of the first method, the apparatus shown schematically in FIG. , prepare a slurry by diluting it with an arbitrary amount of water, extract this slurry with a pump 10, send it to a flow cell 12, irradiate it with light from a light source 13, and measure the transmitted light with a detector 14, which has been determined in advance by experiment. The amount of slurry liquid corresponding to a certain weight may be automatically calculated from the relationship between the absorbance and the slurry concentration.
以上の操作を実動的に実施するには検出器14
からの電気的信号をマイクロコンピユーター17
へ導びき、予め設定しておいた条件に基づいてパ
ルプスラリー採取量を算出し計量器18で計量す
るとよい。 To actually perform the above operations, the detector 14
The electrical signal from the microcomputer 17
The amount of pulp slurry to be collected may be calculated based on preset conditions and measured using the measuring device 18.
次に過マンガン酸カリ消費量の測定操作につい
て説明する。 Next, the operation for measuring the amount of potassium permanganate consumed will be explained.
JIS P8206の規定によれば、パルプ試料を正確
に秤取してビーカーに投入し蒸留水を加え撹拌機
で充分に離解してから4N硫酸を加え恒温に保
つ。次いで所定量の0.1N過マンガン酸カリを瞬
時に加え、充分撹拌しながら5分間反応させた
後、1Nヨウ化カリ溶液を加えて反応を停止さ
せ、ビーカー中の繊維を別することなく、遊離
したヨウ素を0.1Nチオ硫酸ソーダで滴定する。
この滴定の終点にでん粉指示薬を用いる。 According to the regulations of JIS P8206, a pulp sample is accurately weighed, put into a beaker, added with distilled water, thoroughly disintegrated with a stirrer, then 4N sulfuric acid is added and kept at a constant temperature. Next, a predetermined amount of 0.1N potassium permanganate was instantly added, and the reaction was allowed to proceed for 5 minutes with sufficient stirring.The reaction was stopped by adding 1N potassium iodide solution, and the fibers in the beaker were released without separating them. The iodine obtained is titrated with 0.1N sodium thiosulfate.
A starch indicator is used at the end point of this titration.
本発明の方法でも基本的にこの操作手順に従う
が、第5図に示した測定装置のブロツクダイヤフ
ラムによつて説明する。 The method of the invention basically follows this operating procedure, but will be explained using the block diaphragm of the measuring device shown in FIG.
使用する装置には反応ビーカー19、自動ビユ
ーレツト20、蒸留水タンク21、4N硫酸タン
ク22、0.1N過マンガン酸カリタンク23、1N
ヨウ化カリタンク24、0.1Nチオ硫酸ソーダタ
ンク25、でん粉指示薬タンク26を具えてお
り、先ず反応ビーカー19に前述の方法で採取し
た精選未晒パルプ試料を送入後、上記各試薬を
夫々のタンク即ち蒸留水タンク21、4N硫酸タ
ンク22、0.1N過マンガン酸カリタンク23、
1Nヨウ化カリタンク24から所定量を所定の手
順で添加し、0.1Nチオ硫酸ソーダタンク25か
ら自動ビユーレツト20に送られているチオ硫酸
ソーダによつて滴定し、でん粉指示薬タンク26
からの指示薬を加える。この滴定の終点の判定は
ヨウ素化でん粉の着色の消失を光学的方法で検出
する方式に基づいて実施可能であるが、ヨウ素と
チオ硫酸ソーダとの酸化還元反応を電気化学的に
フオローして決めることも可能
各試薬の自動添加は各貯蔵タンクに直結して計
量槽を設け、所定容量毎に水頭を利用するか、ポ
ンプを用いてそれらの時間間隔はタイマーにより
設定することによつて容易に実施可能である。 The equipment used includes a reaction beaker 19, an automatic brewet 20, a distilled water tank 21, a 4N sulfuric acid tank 22, a 0.1N potassium permanganate tank 23, and a 1N potassium permanganate tank.
It is equipped with a potassium iodide tank 24, a 0.1N sodium thiosulfate tank 25, and a starch indicator tank 26. First, the selected unbleached pulp sample collected in the above-mentioned manner is fed into the reaction beaker 19, and then each of the above reagents is poured into the respective tanks. Namely, distilled water tank 21, 4N sulfuric acid tank 22, 0.1N potassium permanganate tank 23,
A predetermined amount is added according to a predetermined procedure from the 1N potassium iodide tank 24, titrated with sodium thiosulfate sent from the 0.1N sodium thiosulfate tank 25 to the automatic brewet 20, and then added to the starch indicator tank 26.
Add the indicator from. The end point of this titration can be determined by optically detecting the disappearance of the coloration of iodinated starch, but it can also be determined by electrochemically following the redox reaction between iodine and sodium thiosulfate. Automatic addition of each reagent can be easily done by installing a metering tank directly connected to each storage tank and using a water head for each predetermined volume, or by using a pump and setting the time intervals using a timer. It is possible to implement.
また計量槽を設けずに貯蔵タンクから直接定量
ポンプを用いて所定時間送液することも可能であ
り、ポンプのオン・オフ操作にはタイマーを用い
るので好適である。 It is also possible to directly feed the liquid for a predetermined period of time using a metering pump from the storage tank without providing a metering tank, and it is preferable to use a timer to turn on and off the pump.
また自動ビユーレツト20には滴定量の自動定
量機構を付設しておき、各滴定毎に滴定値をマイ
クロコンピユーター17に読み取らせ、予めイン
プツトしておいた数式に従つてK価を計算させる
ことが可能である。このK価に関する電気的信号
を他の系、例えばパルプの蒸解系若しくは漂白系
のコントロール装置へフイードすることも可能で
ある。 In addition, the automatic brewet 20 is equipped with an automatic titration amount mechanism, which allows the microcomputer 17 to read the titration value for each titration and calculate the K number according to a formula input in advance. It is. It is also possible to feed this electrical signal relating to the K number to a control device of another system, for example a pulp cooking system or a bleaching system.
本発明方法はクラフトパルプ及び亜硫酸パルプ
など任意のパルプのK価測定に適用可能なことは
言うまでもなく、また明細書に添付した図面の方
式に限定されるものでないことは勿論である。 It goes without saying that the method of the present invention is applicable to measuring the K number of any pulp such as kraft pulp and sulfite pulp, and is not limited to the method shown in the drawings attached to the specification.
以上説明した如く本発明はパルプスラリー濃度
を光透過率によつて測定し、所要試料重量を容積
によつて計量し、以下自動的にK価測定を可能な
らしめたものであり、パルプ製造工程における管
理を迅速正確に行なうことを容易ならしめたもの
であり、極めて価値の高い発明である。 As explained above, the present invention enables the pulp slurry concentration to be measured by light transmittance, the required sample weight to be measured by volume, and the K number to be automatically measured. This is an extremely valuable invention, as it has made it easy to quickly and accurately manage the system.
第1図は回転式洗浄・粕除去装置の概略を示す
側断面図、第2図はパルプスラリー濃度と吸光度
の関係を示す一例の図、第3図はパルプスラリー
試料採取装置の一例の概略図、第4図は他の例の
概略図、第5図は過マンガン酸カリ消費量自動測
定装置のブロツクダイヤグラムである。
図中、1…周面前段、2…周面後段、3…導入
口、4…洗浄水ライン、5…回転中心、6…前段
排出口、7…後段排出口、8…取出口、9…希釈
槽、10…ポンプ、11…配管系、12…フロー
セル、13…光源、14…検出器、15…電磁
弁、16…容器、17…マイクロコンピユータ
ー、18…計量器、19…反応ビーカー、20…
自動ビユーレツト、21…蒸留水タンク、22…
4N硫酸タンク、23…0.1N過マンガン酸カリタ
ンク、24…1Nヨウ化カリタンク、25…0.1N
チオ硫酸ソーダタンク、26…でん粉指示薬タン
ク。
Fig. 1 is a side cross-sectional view schematically showing a rotary washing/lees removal device, Fig. 2 is an example of the relationship between pulp slurry concentration and absorbance, and Fig. 3 is a schematic diagram of an example of a pulp slurry sampling device. , FIG. 4 is a schematic diagram of another example, and FIG. 5 is a block diagram of an automatic potassium permanganate consumption measuring device. In the figure, 1... front stage of circumferential surface, 2... rear stage of circumferential surface, 3... inlet, 4... washing water line, 5... rotation center, 6... front stage discharge port, 7... rear stage discharge port, 8... outlet, 9... Dilution tank, 10... Pump, 11... Piping system, 12... Flow cell, 13... Light source, 14... Detector, 15... Solenoid valve, 16... Container, 17... Microcomputer, 18... Meter, 19... Reaction beaker, 20 …
Automatic brewer, 21... Distilled water tank, 22...
4N sulfuric acid tank, 23...0.1N potassium permanganate tank, 24...1N potassium iodide tank, 25...0.1N
Sodium thiosulfate tank, 26... Starch indicator tank.
Claims (1)
て、パルプ製造工程中を流動している未精選パル
プの一部を連続的に分取し、随伴して来る蒸解排
液を除去洗浄することと未蒸解物の除去とを行な
つてからパルプスラリーの光透過率を測定するこ
とによつてパルプスラリーの濃度を知り、該濃度
に基づいて試料用所定パルプ重量に対応する容量
のパルプスラリー試料を採取し、該試料に対応す
る量の試薬を添加し滴定操作及び測定値より過マ
ンガン酸カリ価の計算を自動的に行なわせること
を特徴とするパルプの過マンガン酸カリ価自動測
定方法。 2 蒸解排液の除去洗浄に用いる装置が横置した
円筒状ないし円錐台状であつて、その周面にパル
プ繊維が通過不能な目開きの網、スリツトを配設
されている回転体より成るものである特許請求の
範囲第1項記載のパルプの過マンガン酸カリ価自
動測定方法。 3 未蒸解物の除去に用いる装置が横置した円筒
状ないし円錐台状であつて、その周面にパルプ繊
維の通過は可能であるが未蒸解物の通過は不可能
な目開きの網、スリツトを配設されている回転体
より成るものである特許請求の範囲第1項記載の
パルプの過マンガン酸カリ価自動測定方法。 4 洗浄装置と未蒸解物除去装置が同軸で回転す
る特許請求の範囲第1項記載のパルプの過マンガ
ン酸カリ価自動測定方法。 5 パルプスラリーを希釈槽に導入し該希釈槽内
スラリーをポンプにて吸引し再度該希釈槽に循環
させる配管系にフローセルを設けてスラリーの光
透過率を連続的に測定しながら該希釈槽に水を注
加して所定の光透過率に到達した時点において所
定容量のスラリーを採取することにより、予め測
定してある光透過率とスラリー濃度との関係から
所定重量に該当するパルプ試料を採取する方法を
用いた、特許請求の範囲第1項ないし第4項中の
何れか1項に記載のパルプの過マンガン酸カリ価
自動測定方法。[Claims] 1. In measuring permanganate potassium value of unbleached pulp, a part of the unselected pulp flowing during the pulp manufacturing process is continuously separated, and the accompanying cooking effluent is collected. After removing and washing and removing undigested materials, the concentration of the pulp slurry is determined by measuring the light transmittance of the pulp slurry, and based on the concentration, the volume corresponding to the predetermined pulp weight for the sample is determined. The potassium permanganate value of pulp is characterized in that a pulp slurry sample is taken, a corresponding amount of reagent is added to the sample, a titration operation is performed, and the potassium permanganate value is automatically calculated from the measured value. Automatic measurement method. 2. The device used for removing and cleaning cooking waste liquid is a horizontally cylindrical or truncated cone-shaped rotating body that is equipped with a mesh or slits on its circumferential surface that are so open that pulp fibers cannot pass through. A method for automatically measuring the potassium permanganate value of pulp according to claim 1. 3. The device used for removing undigested materials is horizontally placed in the shape of a cylinder or truncated cone, and has a mesh on its circumferential surface with openings that allow pulp fibers to pass through but not allow undigested materials to pass through; The method for automatically measuring the potassium permanganate value of pulp according to claim 1, which comprises a rotating body provided with slits. 4. The method for automatically measuring permanganate potassium value of pulp according to claim 1, wherein the washing device and the undigested material removal device rotate coaxially. 5. A flow cell is installed in the piping system that introduces the pulp slurry into a dilution tank, sucks the slurry in the dilution tank with a pump, and circulates it back to the dilution tank, and continuously measures the light transmittance of the slurry. By adding water and collecting a predetermined volume of slurry when a predetermined light transmittance is reached, a pulp sample corresponding to a predetermined weight is collected based on the relationship between the pre-measured light transmittance and slurry concentration. A method for automatically measuring the potassium permanganate value of pulp according to any one of claims 1 to 4, using the method.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP4572580A JPS56142458A (en) | 1980-04-09 | 1980-04-09 | Automatic measurement of permanganate number of pulp |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP4572580A JPS56142458A (en) | 1980-04-09 | 1980-04-09 | Automatic measurement of permanganate number of pulp |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS56142458A JPS56142458A (en) | 1981-11-06 |
JPS628148B2 true JPS628148B2 (en) | 1987-02-20 |
Family
ID=12727296
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP4572580A Granted JPS56142458A (en) | 1980-04-09 | 1980-04-09 | Automatic measurement of permanganate number of pulp |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS56142458A (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5720849U (en) * | 1980-07-12 | 1982-02-03 | ||
JP4592874B2 (en) * | 2000-06-08 | 2010-12-08 | 日本製紙株式会社 | Measuring method of fiber composition |
JP6239257B2 (en) * | 2013-04-24 | 2017-11-29 | 株式会社日立ハイテクノロジーズ | Filling apparatus, method, and analyzer |
-
1980
- 1980-04-09 JP JP4572580A patent/JPS56142458A/en active Granted
Non-Patent Citations (1)
Title |
---|
SYSTEMATIX AUTOMATIC TITRATOR SAT-3 OPERATION AND SERVICE=1978 * |
Also Published As
Publication number | Publication date |
---|---|
JPS56142458A (en) | 1981-11-06 |
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