JPH0299679A - Method of controlling alkaline cellulose digesting process - Google Patents
Method of controlling alkaline cellulose digesting processInfo
- Publication number
- JPH0299679A JPH0299679A JP21024589A JP21024589A JPH0299679A JP H0299679 A JPH0299679 A JP H0299679A JP 21024589 A JP21024589 A JP 21024589A JP 21024589 A JP21024589 A JP 21024589A JP H0299679 A JPH0299679 A JP H0299679A
- Authority
- JP
- Japan
- Prior art keywords
- cooking
- acid
- acetic acid
- formic acid
- cellulose
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 43
- 229920002678 cellulose Polymers 0.000 title claims abstract description 10
- 239000001913 cellulose Substances 0.000 title claims abstract description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 69
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 40
- 235000019253 formic acid Nutrition 0.000 claims abstract description 21
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000004817 gas chromatography Methods 0.000 claims abstract 2
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract 2
- 238000010411 cooking Methods 0.000 claims description 30
- 238000010025 steaming Methods 0.000 claims description 23
- 150000007513 acids Chemical class 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 6
- 239000002699 waste material Substances 0.000 claims description 5
- 238000004587 chromatography analysis Methods 0.000 claims description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 claims 1
- 159000000000 sodium salts Chemical class 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 8
- 239000003513 alkali Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000029087 digestion Effects 0.000 abstract 3
- 229920001131 Pulp (paper) Polymers 0.000 abstract 1
- 238000002419 base digestion Methods 0.000 abstract 1
- 235000011121 sodium hydroxide Nutrition 0.000 abstract 1
- 235000011054 acetic acid Nutrition 0.000 description 19
- 239000002023 wood Substances 0.000 description 13
- 239000000203 mixture Substances 0.000 description 7
- 229920005610 lignin Polymers 0.000 description 6
- 150000001720 carbohydrates Chemical class 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 4
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 4
- 235000011613 Pinus brutia Nutrition 0.000 description 4
- 241000018646 Pinus brutia Species 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- 229910052801 chlorine Inorganic materials 0.000 description 4
- 239000011121 hardwood Substances 0.000 description 4
- 239000011122 softwood Substances 0.000 description 4
- 235000018185 Betula X alpestris Nutrition 0.000 description 3
- 235000018212 Betula X uliginosa Nutrition 0.000 description 3
- 238000003776 cleavage reaction Methods 0.000 description 3
- 229920002488 Hemicellulose Polymers 0.000 description 2
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical class OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- -1 soda anthraquinone Chemical class 0.000 description 2
- 235000009109 Betula pendula Nutrition 0.000 description 1
- 241000219430 Betula pendula Species 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229920002581 Glucomannan Polymers 0.000 description 1
- 150000001243 acetic acids Chemical class 0.000 description 1
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 description 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 150000004674 formic acids Chemical class 0.000 description 1
- 150000001261 hydroxy acids Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 150000002763 monocarboxylic acids Chemical group 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229920001221 xylan Polymers 0.000 description 1
- 150000004823 xylans Chemical class 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/22—Other features of pulping processes
- D21C3/228—Automation of the pulping processes
Landscapes
- Paper (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は、木材のようなセルロースを含む材料のアルカ
リ蒸煮法、特に、硫酸塩法及びソーダ法を制御する方法
に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for controlling the alkaline cooking process of cellulose-containing materials such as wood, in particular the sulphate process and the soda process.
アルカリ蒸煮法においては、原料木材中に含まれセルロ
ース繊維を互いに結合させているリグニンは強アルカリ
性条件下で除去されるが、同時に、木材の高分子炭水化
物成分すなわち、セルロースやヘミセルロースの脂肪族
カルボン酸類への部分的開裂が起きる（Ｓｊ６ｓｔｒ６
ｍ、 Ｅ、、 ＷｏｏｄＣｈｅｍｊ、５ｔｒｙ ：
Ｆｕｎｒｌａｍｅｎｔａｌｓ ａｎｄ Ａｐｐｌ
ｉｃａｔｉｏｎｓＡｃａｄｅｍｉｃ Ｐ＋ｓｓｓ、 Ｎ
ｅｗ Ｙｏｒｋ、 １９８１）。In the alkaline cooking method, the lignin that is contained in raw wood and binds cellulose fibers to each other is removed under strongly alkaline conditions, but at the same time, the polymeric carbohydrate components of the wood, such as the aliphatic carboxylic acids of cellulose and hemicellulose, are removed. Partial cleavage to Sj6str6 occurs (Sj6str6
m, E,, WoodChemj, 5try:
Funramentals and Appl
cationsAcademic P+sss, N
ew York, 1981).
かくして、廃液中に溶解している有機物は、リグニン分
解の産物の他に、前述の炭水化物の分解産物及び少量の
木材抽出物からなる。The organic matter dissolved in the effluent thus consists, in addition to the products of lignin decomposition, of the aforementioned carbohydrate decomposition products and small amounts of wood extract.
廃液中に含まれる脂肪族カルボン酸両分自身は、揮発性
の酸（酢酸及び蟻酸）に加え、ヒドロキシモノカルボン
酸及びヒドロキシジカルボン酸の両者からなる。The aliphatic carboxylic acids themselves contained in the waste liquid consist of both hydroxymonocarboxylic acids and hydroxydicarboxylic acids in addition to volatile acids (acetic acid and formic acid).
（Ａｌｅｎ、 Ｒ，、Ｎｉｅｍｅｌａ、 Ｋ、、 ＆
５ｊＯｓｔｒ′ｏｍ、 Ｅ。(Alen, R., Niemela, K., &
5j Ostr'om, E.
Ｊ、 Ｃｈｒｏｍａｔｏｇｒ、１
（３０１（１９８４） ２７３； Ｎｉｅｍｏｌａ、
Ｋ、 ＆ Ｓｊ６ｓｔｒｉｉｍ。J, Chromatogr, 1 (301 (1984) 273; Niemola,
K, & Sj6striim.
Ｅ、 、 Ｉｌｏｌｚｆｏｒｓｃｈｕｎｇ）＋４０．１
９８６．３８１＋。E, , Ilolzforschung) +40.1
986.381+.
硬質木材の蒸煮においては、蒸煮収率が高い為に産出さ
れる酸類の総量は、軟質木材の蒸煮の場合に比較してや
や少ないが、原料の異なった炭水化物組成が、それぞれ
の酸組成の本質的な相異の原因となる。これらの相異は
さらに酸の生成速度において認められてきたが、その結
果として廃液中の酸組成は脱リグニンを行う過程で変化
する。In the case of hardwood steaming, the total amount of acids produced is slightly lower than in the case of softwood steaming due to the high steaming yield, but the different carbohydrate compositions of the raw materials contribute to the essential acid composition of each. It causes a difference. These differences have also been observed in the rate of acid production, with the result that the acid composition of the waste fluid changes during the delignification process.
軟質木材類及び硬質木材類両方のヘミセルロース類（グ
ルコマンナン類及びキシラン類）中のアセデル基は、蒸
煮の初期の段階でアルカリの作用下で容易に開裂し、そ
の結果酢酸を生成する。The acedel groups in hemicelluloses (glucomannans and xylans) of both soft and hard woods are easily cleaved under the action of alkali during the early stages of cooking, resulting in the production of acetic acid.
（Ｏｌｍ、 Ｌ、 ＆ Ｔｉ５ｔａｄ、 Ｇ、、 ５ｖ
ｅｎｓｋ Ｐａｐｐｅｒｓｔｉｄｎ８２、１９７９．３
５８１
酢酸はより緩慢に生成されるが、これは、炭水化物鎖に
おきる開裂反応の結果として、先ず第１に生成される。(Olm, L. & Ti5tad, G., 5v
ensk Paperstidn82, 1979.3
581 Acetic acid is produced more slowly, but it is produced first as a result of a cleavage reaction that occurs on the carbohydrate chain.
硬質木材類はアセチル基を多く含むので、対応する黒液
は、軟質木材の黒液よりも顕著に多量の酢酸を含む。一
方、蟻酸は、例えば、開裂反応に関連して開裂される炭
水化物末端単位の反応生成物の一つとして生成し、その
黒液中の濃度は蒸煮が進むに従って、酢酸の濃度に比べ
てより規則的に上昇する。酢酸と対照的に、黒液中の蟻
酸の量は、蒸煮工程に付される原料木材にはそれほど影
響を受けない。Since hard woods contain more acetyl groups, the corresponding black liquor contains significantly more acetic acid than the black liquor of soft woods. On the other hand, formic acid, for example, is produced as one of the reaction products of the carbohydrate end units cleaved in connection with the cleavage reaction, and its concentration in black liquor becomes more regular compared to that of acetic acid as the cooking progresses. to rise. In contrast to acetic acid, the amount of formic acid in black liquor is not significantly affected by the raw wood that is subjected to the cooking process.
許可されたフィンランド国特許（第７１．５８４号）に
よるとアルカリ蒸煮法の制御は、蒸煮液中に含まれるモ
ノカルボン酸の相対組成をクロマトグラフィーで分析す
ることにより、驚くべき正確さで行うことができる。対
応する分解産物の組成に基づいて、蒸煮に付される軟質
木材、硬質木材片の組成を決定することが可能であると
いうことが後になって判った（フィンランド国特許第８
７５２４８号）。本発明の目的は、それ故、アルカリ、
セルロース蒸煮を以前よりずっと簡単にかつより単純に
、さらには、蒸煮のそれぞれの程度に応じてより正確に
制御するための新規な方法を提供する事である。According to the granted Finnish patent (No. 71.584), the control of the alkaline cooking process can be carried out with remarkable precision by chromatographic analysis of the relative composition of the monocarboxylic acids contained in the cooking liquor. Can be done. It was later found that it was possible to determine the composition of the soft and hard wood pieces to be subjected to steaming on the basis of the composition of the corresponding decomposition products (Finnish Patent No. 8).
No. 75248). The object of the invention is therefore that an alkali,
The object is to provide a new method for cellulose cooking much easier and simpler than before, and also to control the respective degree of cooking more precisely.
本発明を特色づける背景については、請求項１を参ロベ
されたい。本発明においては新規で、かつ、予測できな
い観察がなされた。すなわち、アルカリセルロース蒸煮
法は、与えられた時間内に蒸煮によって生成される、揮
発性酸類（酢酸及び蟻酸）を含む画分の助けを借りてう
ま（制御が出来るということである。制御は脱リグニン
の過程で酢酸と蟻酸含量の比を観察することに基づいて
いる。この結果、各場合に適用されるこれらの条件下で
の脱リグニンのいかなる所望の程度にも到達する為に消
費される時間を予測することが出来るようになる。本発
明の主な特徴はここに添付した各請求項中に読むことが
できる。For background characterizing the invention, please refer to claim 1. A new and unexpected observation was made in the present invention. That is, the alkaline cellulose cooking method can be controlled with the help of the fraction containing volatile acids (acetic acid and formic acid) produced by the cooking within a given time. It is based on observing the ratio of acetic acid and formic acid contents in the process of lignin, which is consumed to reach any desired degree of delignification under these conditions applied in each case. The main features of the invention can be read in the claims appended hereto.
本発明方法が開発されるにしたがって、蒸煮中に発生す
る酢酸と蟻酸の濃度比と蒸煮の総収量（あるいは、原材
料に残存するリグニン量）との間にはある直線関係があ
るという事が判明した。この算術関係はまた、蒸煮時の
アルカリ総量や硫化度のような条件の不規則な変化によ
っても、わずかな影響を受けるのみである。もし蒸煮工
程で、一定の時間間隔をおいてサンプルを取り出したな
らば、前述の酸の比を用いて、所望の蒸煮度を達成する
のに必要な時間を決定することが出来る。As the method of the present invention was developed, it became clear that there is a linear relationship between the concentration ratio of acetic acid and formic acid generated during steaming and the total yield of steaming (or the amount of lignin remaining in the raw material). did. This arithmetic relationship is also only slightly affected by random changes in conditions such as total alkali content and sulfidity during cooking. If samples are taken at regular time intervals during the cooking process, the aforementioned acid ratios can be used to determine the time required to achieve the desired degree of cooking.
本発明においてはまた、もし必要とあれば黒液中の酢酸
及び蟻酸は、酸の揮発性を増大させる誘導体を作ること
なしにクロマトグラフィーによって、分析できるという
ことが重要である。この点については、揮発性が乏しい
ヒドロキシモノカルボン酸の監視に基づく先行の方法に
比べて著しい利点がある（フィンランド国特許第７１５
８４号）。そのうえ、本発明の方法では、数十種類のヒ
ドロキシ酸の代りに２種類の酸成分だけを分析するれば
よいという事実の故に、従来の方法よりも実質的に進歩
している。コンピューター技術によって制御情報を得る
ための必須要件である信用出来る分析データがサンプリ
ングしてすぐ得られるという事は、ちょうど上に述べた
情況からも、自明の理であり、この事はこの方法の有用
性に大きく貢献している。It is also important in the present invention that acetic and formic acids in black liquor can be analyzed by chromatography, if desired, without making derivatives that increase the volatility of the acids. In this respect, there are significant advantages compared to previous methods based on the monitoring of poorly volatile hydroxymonocarboxylic acids (Finland Patent No. 715
No. 84). Moreover, the method of the present invention is a substantial advance over conventional methods due to the fact that only two acid components need be analyzed instead of dozens of hydroxy acids. The fact that reliable analytical data, which is an essential requirement for obtaining control information using computer technology, can be obtained immediately after sampling is self-evident from the situation just described above, and this fact makes this method useful. It makes a major contribution to sexuality.
本発明によって提案された方法は、次に示す実施例によ
り詳しく述べられている。これらの例は、松や樺のチッ
プについて行われる硫酸塩蒸煮を扱っているが、当業者
にとっては、他のアルカリ蒸煮法（例えば、ソーダーア
ントラキノン蒸煮法）の場合にも、あるいは他の原料水
材種の場合（そしておそらくはまた他種のセルロース含
有の植物原料の場合にも）この方法が同様に適用できる
事は明らかである。これらの他の場合には、特定の原材
料（例えば、混合蒸煮）の質と組成な考査に入れて、蒸
煮工程の総収量やリグニンの溶解に対する酢酸・蟻酸の
濃度比の変化を、各場合に先づ測定することになる。The method proposed by the invention is explained in more detail by means of the following examples. These examples deal with sulfate steaming carried out on pine and birch chips, but it will be appreciated by those skilled in the art that they can also be used in the case of other alkaline steaming methods (e.g. soda anthraquinone steaming) or with other raw water materials. It is clear that this method is equally applicable in the case of seeds (and perhaps also in the case of other cellulose-containing plant materials). In these other cases, the changes in the acetic acid/formic acid concentration ratio for the total yield of the cooking process and the dissolution of lignin should be taken into consideration in each case, taking into account the quality and composition of the particular raw material (e.g. mixed cooking). We will measure it first.
実施例１：
棒材（Ｂｅｔｕｌａ ｖｅｒｒｕｃｏｓａ／Ｂ、 ｐｕ
ｂｅｓｃｅｎｓ、 ２−４ｍｍの篩両分）から調製さ
れたチップを用いて、実験室の蒸解がまで通常の硫酸蒸
煮を行った。Example 1: Bar material (Betula verrucosa/B, pu
Conventional sulfuric acid cooking was carried out until laboratory cooking using chips prepared from P. bescens, 2-4 mm sieve size).
蒸煮は、木の量の２０％（水酸化ナトリウムとして）の
活性アルカリを用い、硫化度３０％、液体／木材比４Ｌ
／ｋｇで行った。蒸煮温度を上げ（３０℃から１６８°
Ｃまで）最高温度で、９０分間蒸煮を続けた。蒸煮中、
廃液のサンプルを、一定の間隔（２０分）で取り出し、
酢酸及び蟻酸の量を分析した。（Ａｌｅｎ、 Ｒ，、、
Ｊａｎｎｉｒｉ、 Ｐ、 ＆ＳｊＯｓｔｒｉｉｍ、 Ｅ
、、 Ｆｉｎｎ、 Ｃｈｅｍ、 Ｌｅｔｔ、、 １９８
５．１９０１以前の知識に基づけば蒸煮中縁収量が塩素
価に依存することはよく知られている（ここでいう塩素
価はバルブ中のリグニン量を計算する事を可能にする）
ので１本件の場合、塩素価は測定しなかった。For steaming, use active alkali of 20% of the amount of wood (as sodium hydroxide), sulfidity of 30%, liquid/wood ratio of 4 L.
/kg was used. Increase the steaming temperature (from 30℃ to 168℃)
Cooking was continued for 90 minutes at the highest temperature (up to C). During steaming,
Samples of waste liquid were taken at regular intervals (20 minutes),
The amount of acetic acid and formic acid was analyzed. (Alen, R.,
Janniri, P. & SjOstriim, E.
,, Finn, Chem, Lett,, 198
Based on knowledge prior to 5.1901, it is well known that the yield of the steamed rim depends on the chlorine number (the chlorine number here makes it possible to calculate the amount of lignin in the valve).
Therefore, in this case, the chlorine value was not measured.
第１図においては、酢酸・蟻酸比の、蒸煮時間に対する
関係を、第２図においては、蒸煮中に分解した物質量に
対する上述の比の変化を示した。後者の場合、蒸煮の種
々段階で観察される酸比の屈曲点が、明らかに見られる
。温度上昇期の最中及びその直後に、それぞれの蒸解が
まを用いてなされる同様の蒸煮の充分な数のサンプルを
廃液から取り出すことによりこのようにして得られた情
報を用いることにより、所望の蒸煮度が達成出来る時間
を数学的に決定することができる。FIG. 1 shows the relationship of the acetic acid/formic acid ratio to the steaming time, and FIG. 2 shows the change in the above-mentioned ratio with respect to the amount of substances decomposed during the steaming. In the latter case, the inflection points in acid ratios observed at various stages of cooking are clearly visible. By using the information thus obtained by removing from the effluent a sufficient number of samples of similar cooks made with each digester during and immediately after the temperature rise period, the desired The time at which a degree of cooking can be achieved can be determined mathematically.
実施例２
実施例１と同様に、松（旺凹と胚旦二に且）材のチップ
を用いて、同様の硫酸蒸煮を次の条件下で行った。すな
わち、木の１の２４％（水酸化ナトリウムとして）の活
性アルカリ、硫化度３０％、液体／木材比３．５Ｌ／ｋ
ｇであった。蒸煮温度は、６０分間一定速度で、２０℃
から１７０°Ｃまで上昇させ、蒸煮な１５０分間続けた
。蒸省°時間中、一定の間隔（３０分）で廃液のサンプ
ルを抜き出したのち、実施例１の場合のように、それか
ら酢酸及び蟻酸の量を測定した。第３図及び第４図は、
それぞれの場合について、酢酸と蟻酸の比の変化を蒸煮
時間及び蒸煮過程中に溶解した材料の量に対してプロッ
トしたものを示す。この場合にもまた、総収量と塩素測
量の関係に関する、蒸煮制御の観点から必要な情報は既
知の事実である。Example 2 In the same manner as in Example 1, sulfuric acid steaming was performed under the following conditions using chips of pine wood (Wangko and Gedanji). i.e. 24% active alkali (as sodium hydroxide) of 1 of wood, sulfidity 30%, liquid/wood ratio 3.5L/k
It was g. Steaming temperature was 20°C at a constant speed for 60 minutes.
The temperature was raised to 170°C and steaming continued for 150 minutes. After drawing samples of the waste liquid at regular intervals (30 minutes) during the evaporation period, the amounts of acetic acid and formic acid were determined therefrom as in Example 1. Figures 3 and 4 are
For each case, the change in the ratio of acetic acid to formic acid is shown plotted against the cooking time and the amount of material dissolved during the cooking process. In this case too, the information necessary from the point of view of steaming control regarding the relationship between total yield and chlorine measurement is a known fact.
上記の実施例は、本発明を説明せんとするにすぎず、決
して本発明を限定するものではない。The above examples are only intended to illustrate the invention and are not intended to limit it in any way.
第１図は樺の木の硫酸蒸煮過程で、時間経過に伴う酢酸
／蟻酸濃度比の変化をグラフにしたものである。
第２図は同様の樺の木の硫酸塩蒸煮過程での蒸煮分解生
成物量と酢酸／蟻酸濃度比の関係をグラフにしたもので
ある。
第３図は松の木の硫酸塩蒸煮過程で時間経過に伴う酢酸
／蟻酸濃度比の変化をグラフにしたものである。
第４図は同様の松の木の硫酸塩蒸煮過程での蒸煮分解生
成物量と酢酸／蟻酸濃度比の関係をグラフにしたもので
ある。Figure 1 is a graph showing changes in the acetic acid/formic acid concentration ratio over time during the sulfuric acid cooking process of birch wood. FIG. 2 is a graph showing the relationship between the amount of steamed decomposition products and the acetic acid/formic acid concentration ratio in a similar sulfate steaming process of birch wood. Figure 3 is a graph showing changes in the acetic acid/formic acid concentration ratio over time during the sulfate steaming process of pine wood. FIG. 4 is a graph showing the relationship between the amount of steamed decomposition products and the acetic acid/formic acid concentration ratio during the sulfate steaming process of a similar pine tree.
Claims (1)
塩法及びソーダ法の蒸煮工程を制御する方法であって、
脱リグニン化に関連して生成する揮発性酸を、蒸煮工程
中に分析し、黒液中に存在する揮発性酸の濃度比を基に
して、所望の蒸煮度を達成するのに必要な時間を決定す
ることを特徴とする方法。 （２）脱リグニン化に関連して、酢酸及び蟻酸を分析し
、黒液中に存在する２つの酸の濃度比を基に所望の蒸煮
度を達成するのに必要な時間を決定する請求項（１）記
載の方法。（３）酢酸と蟻酸をガスクロマトグラフィー
もしくは高圧液体クロマトグラフィーに基づく、クロマ
トグラフィーによって分離、分析する請求項（１）又は
（２）記載の方法。 （４）廃液中に存在する酢酸及び蟻酸を、ナトリウム塩
、遊離酸及び／又は誘導体として分析する請求項（１）
〜（３）のいずれか１項に記載の方法。 （５）各特定の時刻における進行中の蒸煮の段階及びさ
らに必要な脱リグニン化のための時間を、黒液中に存在
する酢酸及び蟻酸の濃度比を基に決定し、該比をそれぞ
れの蒸煮法について別に決定された対応する比の関係と
比較する請求項（１）〜（４）のいずれか１項に記載の
方法。 （６）蒸煮過程で、酸の分析の為に必要な数のサンプル
を蒸煮液から抜き出す、請求項（１）〜（５）のいずれ
か１項に記載の方法。[Claims] (1) A method for controlling the alkaline steaming process of cellulose-containing materials, particularly the sulfate method and the soda method, comprising:
The volatile acids produced in connection with delignification are analyzed during the cooking process and the time required to achieve the desired degree of cooking is determined based on the concentration ratio of volatile acids present in the black liquor. A method characterized by determining. (2) A claim in which, in connection with delignification, acetic acid and formic acid are analyzed and the time required to achieve a desired degree of cooking is determined based on the concentration ratio of the two acids present in the black liquor. (1) The method described. (3) The method according to claim (1) or (2), wherein acetic acid and formic acid are separated and analyzed by chromatography based on gas chromatography or high-pressure liquid chromatography. (4) Claim (1) in which acetic acid and formic acid present in waste liquid are analyzed as sodium salts, free acids and/or derivatives.
The method according to any one of (3) to (3). (5) Determine the ongoing cooking stage and the time for further necessary delignification at each particular time based on the concentration ratio of acetic acid and formic acid present in the black liquor, and 5. A method according to any one of claims 1 to 4, wherein the comparison is made with a corresponding ratio relationship determined separately for the steaming process. (6) The method according to any one of claims (1) to (5), wherein a number of samples necessary for acid analysis are extracted from the cooking liquid during the cooking process.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FI883818 | 1988-08-17 | ||
| FI883818A FI80731C (en) | 1988-08-17 | 1988-08-17 | FOERFARANDE FOER STYRNING AV ALKALISK CELLULOSAKOK. |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0299679A true JPH0299679A (en) | 1990-04-11 |
Family
ID=8526931
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21024589A Pending JPH0299679A (en) | 1988-08-17 | 1989-08-16 | Method of controlling alkaline cellulose digesting process |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JPH0299679A (en) |
| DE (1) | DE3927183A1 (en) |
| FI (1) | FI80731C (en) |
| SE (1) | SE8902722L (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FI893830A (en) * | 1989-08-14 | 1991-02-15 | Kajaani Elektroniikka Oy | FOERFARANDE FOER STYRNING AV SYRGAS -ALKALI BLEKNING. |
| DE59005944D1 (en) * | 1990-03-05 | 1994-07-07 | Siemens Ag | Process for the production of pulp in a continuous cooker. |
-
1988
- 1988-08-17 FI FI883818A patent/FI80731C/en not_active IP Right Cessation
-
1989
- 1989-08-11 SE SE8902722A patent/SE8902722L/en not_active Application Discontinuation
- 1989-08-16 JP JP21024589A patent/JPH0299679A/en active Pending
- 1989-08-17 DE DE19893927183 patent/DE3927183A1/en not_active Withdrawn
Also Published As
| Publication number | Publication date |
|---|---|
| FI80731C (en) | 1990-07-10 |
| SE8902722L (en) | 1990-02-18 |
| FI80731B (en) | 1990-03-30 |
| SE8902722D0 (en) | 1989-08-11 |
| FI883818A0 (en) | 1988-08-17 |
| DE3927183A1 (en) | 1990-02-22 |
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