WO1983003435A1 - Pulping process - Google Patents

Pulping process Download PDF

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Publication number
WO1983003435A1
WO1983003435A1 PCT/JP1983/000092 JP8300092W WO8303435A1 WO 1983003435 A1 WO1983003435 A1 WO 1983003435A1 JP 8300092 W JP8300092 W JP 8300092W WO 8303435 A1 WO8303435 A1 WO 8303435A1
Authority
WO
WIPO (PCT)
Prior art keywords
adsorbent
mixture
magnesium
cooking
adsorption
Prior art date
Application number
PCT/JP1983/000092
Other languages
English (en)
French (fr)
Japanese (ja)
Inventor
as represented by DIRECTOR-GENERAL OF ... JAPAN
Ltd. Kunimine Industries Co.
Original Assignee
Ikari, Yoshikatsu
Yokoyama, Shoichiro
Katoh, Keisuke
Inoue, Haruhiko
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Ikari, Yoshikatsu, Yokoyama, Shoichiro, Katoh, Keisuke, Inoue, Haruhiko filed Critical Ikari, Yoshikatsu
Publication of WO1983003435A1 publication Critical patent/WO1983003435A1/ja

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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
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D21C11/0085—Introduction of auxiliary substances into the regenerating system in order to improve the performance of certain steps of the latter, the presence of these substances being confined to the regeneration cycle

Definitions

  • This invention relates to the pulping method
  • the present invention has proposed a lumping method including a step of baking at least a part of the adsorbent that has adsorbed the organic component to remove the organic component by burning and regenerating the adsorbent.
  • the present invention provides an improved hopping method that overcomes the problems of the conventional method.
  • the present invention is characterized by adding an alkaline substance to a cooking waste liquid treated with a magnesia adsorbent to increase pH. This is it! ), Magnesium compounds dissolved in the waste liquid can sink and be recovered.
  • lignocellulose substance means a substance containing cellulose and lignin.
  • suitable lignocellulose materials include wood, bamboo, pagasu, straw, rice straw, and other fibrous materials.
  • the lignocellulose substance is treated with a known cooking liquor]) under known conditions and by a known method to obtain a cooking product (first mixture).
  • a suitable cooking liquor NaOH, Na 2 G0 3, Na 2 S0 4 and Na 2 S0 3, such as Na preparative imidazolium compound and 2 oxidation
  • I Saiu of Na- pace obtained was dissolved in water goods and, MgO, MgC0 3, Mg ( OH) 2,
  • the digestion product from step (a) is sent to a solid-liquid separator. And the digestion waste (strength liquor) containing a large amount of lignin and other attached substances released from lignocellulose substances in the step).
  • the cooking effluent (stronglyceric acid) obtained in step (b) is treated with a magnesium-containing adsorbent to remove organic components such as lignin by adsorption.
  • a magnesium-containing adsorbent to remove organic components such as lignin by adsorption.
  • Magnesia-containing sorbents are suitable for lignin and other organic components. While it exhibits high adsorption capacity, it does not adsorb metal ions
  • the cooking waste liquor after the treatment with the adsorbent can be circulated to the cooking step as at least a part of the cooking liquor.
  • adsorbents are: calcined magnesia, magnesia and alumina mixture, magnesia.
  • the product obtained by calcining at 450-600 for 15-45 minutes exhibits excellent adsorptivity and is a preferred adsorbent.
  • the calcined magnesia preferably has a particle size of less than 60 mesh, especially less than 200 mesh, low crystallinity and apparent specific gravity.
  • the calcined magnesia can be mixed with fillers such as iron oxide, ferric oxide, calcium oxide, alumina, perlite, zeolite, pentonites, and silicate clay.
  • the amount of filler in this case is less than 40%, preferably 2.0%, based on the total weight of filler and magnesia.
  • Such a mixed adsorbent is prepared by mixing a calcined magnesium and a filler in the form of an oxide obtained by calcining a filler in the form of a hydroxide at 400 to 700 ° C, or It can be obtained by firing the mixture of the above-described magnesium compound and filler at 400 ° C.
  • the adsorption treatment comprises adsorbing the adsorbent into the reactor.
  • the waste liquid is supplied intermittently.
  • the amount of adsorbent is 2 to 15% by weight, preferably 5 to 10% by weight.
  • a part of the obtained mixture (second mixture) is intermittently discharged from the reactor and sent to the solid-liquid separation described below.
  • the reactor may be composed of a plurality of reactors connected in series. i adsorption, under stirring, 4 0 - 7 0, favored properly about .6 0 rig two emissions content of the liquid phase of the resulting mixture at a temperature of ⁇ 5% by weight or less, preferred _ properly 2% This is done over a period of time that: The reaction time is usually within one hour.
  • the adsorbent gradually dissolves in the cooking effluent.
  • the reason is probably that magnesium forms a water-soluble complex with lignosulfate and low molecular weight organic acids in the effluent.
  • the amount of magnesium component in the liquid phase obtained by removing the solid components (adsorbent that adsorbs organic components) from the mixture obtained in the cooking process is converted to magnesium ion
  • the concentration is usually 1-5 ⁇ /, but this concentration varies depending on the type of cooking liquor and adsorption reaction conditions.
  • the pH of the digested waste liquor (second mixture) from which organic components have been removed is increased by the addition of alkaline substances, and the dissolved magnesium components precipitate due to this.
  • the alkaline substance examples include an alkali metal hydroxide and calcium hydroxide.
  • the amount of magnesium component that precipitates increases with increasing pH. It is preferred to increase the pH by at least 0.2, usually 0.2-1.2. This makes it possible to reduce the amount of magnesium component dissolved in the waste liquid to 100 P Pm or less.
  • the pH adjustment is preferably performed after the end of the adsorption treatment, at the end of the adsorption treatment, or during the step of separating the cooking waste liquid and the adsorbent.
  • the mixture is left under stirring at 40-701 C for 15- 30 minutes.
  • the precipitation of dissolved magnesium can be controlled by adjusting the pH increase. Dissolved waste liquor as it is or as required ⁇ ⁇ ⁇ It is desirable that it be reused in the digestion process after treatment
  • the control of the amount of magnesium depends on the type of cooking liquor. For example, in the case of sodium-pace steam, the concentration of magnesium dissolved in the solution should be less than 500 / pound, preferably less than 100 ppm.
  • the planned c the pH is controlled so that the dissolved magnesium concentration is 500 to 1/500 / i, depending on the product. This concentration can be reduced to traces if desired.
  • the cooking waste liquor in which the organic components are absorbed on the adsorbent is preferably due to sedimentation! ), Separated into a solid-rich layer (slurry layer) at the bottom and a liquid phase at the top. Part of the lower slurry layer is circulated to the adsorption step, and the remainder is sent to the regeneration step to regenerate the adsorbent. Due to the ⁇ ⁇ control process in the first stage! )
  • the liquid phase whose magnesium content has been reduced is circulated to the cooking liquor preparation step as it is or, if necessary, after the removal of low-molecular-weight organic components.
  • the adsorbent having a nucleated component, usually slurry, obtained in the step (d) is reduced to a cake having a water content of 30 to 70% by weight under vacuum or pressure. Dehydrated. It is preferable to wash the cake with hot water before adjusting the water content.
  • the cake is then calcined at a temperature of 400-700, preferably-450-600 ° C, usually in an oxidizing atmosphere
  • the treatment can be performed in a reducing atmosphere (oxygen concentration: 0 to 5%).
  • Organic atmosphere adsorbed on the adsorbent undergoes thermal decomposition to give tar, methane, carbon monoxide, hydrogen, and carbonaceous substances.
  • Charcoal / WIK i
  • the substance is decomposed by contact with oxygen in the subsequent process.
  • the sulfur component adsorbed on the adsorbent is also removed as sulfur dioxide by oxidation.
  • the above calcination treatment can be carried out in a moving bed, a fluidized bed calcination tower, a multi-Haas-Shash-type furnace or a monolithic-type furnace.
  • the weak liquor obtained in the step (b) can also be treated by the same method as described for the treatment of strong sugar.
  • the obtained organic matter-containing adsorbent can be subjected to a regenerating treatment together with the one obtained from stringers.
  • the liquid phase obtained from the weak liquid can be reused as the washing liquid in step (b).
  • the cooking liquor can be prepared using the liquid phase obtained in the step (d) and the carbon dioxide obtained in the step (e). If necessary, small amounts of fresh CO2 and Z or fresh digester can be used for replenishment. In order to obtain good quality pulp, the lignin content of
  • the content be 1.5% by weight or less, particularly 1.0% by weight or less.
  • FIG. 1 is a flow diagram showing a system for carrying out the halping method of the present invention
  • FIG. 2 is a flow diagram showing an example of an adsorption and sedimentation process of the present invention. is there.
  • step 2 No WIPO i It is sent to the cooking step 2, where the cooking liquor is also sent from the cooking liquor preparation step 1 via line 21.
  • step 2 the lignocell material is digested, and the resulting mixture is led through line 22 to separation step 3, where it is separated into help, digester liquor and dioxide.
  • step 5 the string glycol is mixed with the magnesia-containing adsorbent supplied via line 30 from storage tank 11.
  • alkaline substances are supplied from line 31 to precipitate magnesium components dissolved in the wastewater. Let them kill.
  • the mixture thus treated is then led through line 32 to sedimentation step 6, where sedimentation of the adsorbent occurs.7
  • the supernatant liquid phase and the lower or bottom solids are enriched Separated into phases and o.
  • the bottom layer is led to the slurry state by line 33] 9 dewatering process' 7. Weekly liquors are treated separately, similar to strong liquors.
  • the adsorbent in tank 45 is supplied via line 46 and the alkaline substance is supplied via line 38.
  • the treated mixture is sent to the line 39)) sedimentation step 10 and the bottom solids-rich layer is taken to the line 40)) dewatering step 7.
  • OMPI Cao c the supernatant liquid phase from the i after having been subjected to it or appropriate treatment is by j emission line 4 1, it is re-used as a wash purification plant and Z or w 2 -? Ru.
  • the slurry containing the adsorbent with organic components was dehydrated to a certain degree in step 7, and the mother liquor was discharged via line 36) and discharged through sedimentation step 6 through 5 lines 48. Guided to preparation step 1 together with the supernatant.
  • the dehydrated product from step 7 is led by line 34 to J baking step 8, where the organic components carried by the adsorbent are removed by decomposition or combustion, and the adsorbent is removed.
  • Regeneration produces sulfur dioxide.
  • the regenerated adsorbent is circulated through tanks 35 and 47 to tanks 11 and 45, respectively.
  • the sulfur dioxide is led to the preparation step 1 by the line 37, where the cooking liquor is prepared from the treated cooking effluent and the carbon dioxide.
  • 3 ⁇ 4 Suitable 3 ⁇ 4 New ingredients such as sodium compound, magnesium compound or carbon dioxide, are added to line 42 ?? maintain.
  • FIG. 2 shows the preferred mode of the system for the adsorption and settling processes.
  • the system (three in this example) a plurality of include ⁇ zone 3 1, 3 2 and 3 3, sedimentation zone 3 4, 3 5 and 3 6 are linked to each.
  • Cooking liquor L. (Scan collected by filtration ring or Conwy over click Li car) is sent to the first 0 adsorption zone 3 1, here, by La Lee down 4 7]? From the second settling zone 3 5 'sent the second of Mixed with adsorbent-containing slurry.
  • the mixture is introduced into the third settling zone 34, which is separated into the first upper liquid phase and the third slurry layer.
  • the first liquid phase is sent to La Lee emissions 4 9 by the second adsorption zone 3 2, whereas a portion of the third scan La Li one is by the Rai emissions 5 6 2]? To the first adsorption zone 3 1 And the other part of the third slurry It is led to the dehydration zone 39 by the in 51.
  • the dehydrate from zone 39 is sent to line 52)) to the baking zone (not shown), while the mother liquor is extracted from line 53 to line 53). It is mixed with the first liquid phase that flows through 49.
  • the cooking effluent from which a part of the organic components has been removed in the first adsorption zone 31 is then converted to the line 54 in the second adsorption zone 32]. It is treated by contact with 1 slurry supplied from the subsidence area 36.
  • the mixture in the second adsorption zone 32 is line 55! ) It is sent to the second subsidence area 35, where it is settled! 2) Separated into a second slurry layer and a second liquid phase. As described above, part of the second slurry is sent to the first adsorption zone 31. Another part of the second slurry is circulated by the line 60 to the second adsorption zone 32. The second liquid phase is led to the third adsorption zone 33 by the line 63 and further processed by the fresh adsorbent supplied by the feeder 38. The mixture in the third adsorption zone 33 is led to the line 59] 9 sedimentation zone 70, where the alkaline substance from the line 71 is mixed, and the dissolved magnesium component Sinks.
  • the mixture in the zone 70 is sent to the first settling zone 36 by the line 72 [9] and separated into the first slurry and the third liquid phase.
  • the acidic solution S is supplied from the line 73, and the pH of the mixture discharged from the precipitation zone is adjusted to a pH value suitable for adsorption in the third adsorption zone 33.
  • a part of the first slurry is circulated to the second adsorption zone 32, and another part is circulated to the third adsorption zone 33 by the line 61.
  • the third liquid phase is due] 9 discharged to the first sedimentation zone 3 6 months ⁇ Luo line 5 6, feeding into cooking liquor preparation process (not shown) as a La b by the emissions 5 7] ?, L 3 Can be If necessary, a portion of the third liquid phase is discharged from the system as line 5 8 Kakara L 5. pH power; cooking waste liquor less than 4 L 0
  • the cooking effluent is successively guided to the first, second and third -adsorption zones, where the organic components are removed by adsorption of the adsorbent] ⁇ and the amount of dissolved magnesium is removed. Gradually increases.
  • the adsorbent is sequentially guided to the third, second, and first adsorption zones, and the amount of the adsorbed organic component gradually increases.
  • 4 0, 4 1 and 4 to that shown in 2 is a Parubu, by adjusting the scan La Li one amount of circulated to the suction zone from settling zone, the adsorbent concentration of each adsorption zone a predetermined value It is intended to maintain 4 3, 4 4, 4 5 and an Parubu be that shown at 4 6, to the outside of the system part of which the flow 10 liquid, respectively L 4, L x, for drawing in and L 2 and L 5 belongs to.
  • the number of adsorption and sedimentation zones can be increased if desired.
  • Silica is compared to lignin.] 5Since it is easily adsorbed on the magnesium-containing adsorbent, silica is adsorbed without being decomposed by firing.
  • the adsorbent When the lignocell P-substance contains a silicon component, such as pagasu, bamboo, and straw, the adsorbent gradually decreases its adsorbing ability due to repeated use. In such a case, prior to the organic component removal treatment, silica removal with a magnesia-containing adsorbent should be performed.
  • Desired pre-processing is preferred.
  • the silica adsorbent used in this pretreatment is regenerated separately from the nucleated component-containing adsorbent. If most of the pretreatment adsorbent becomes magnesium silicate and loses its activity, the adsorbent is discharged out of the system and used as a building material, land conditioner, or fertilizer. It will be collected in order.
  • the cooking mixture was filtered to obtain a crude mixture.
  • a loop and a first filtrate were obtained.
  • the crude haptic was washed with 1Z15 times the weight of the first filtrate and filtered to obtain a washed pulp and a second filtrate.
  • the first and second filtrates were combined to obtain a diluted strong glycol, and the wash was further treated with water to obtain a refined Halleb and a third filtrate (a Wilikre).
  • One layer of the slurry separated from the above liquid B was dried into a cake having a water content of 35%, placed in a furnace equipped with a stirrer, and gradually reduced to 400 "C in a reducing atmosphere. After heating, the adsorbent was regenerated by burning the organic components while maintaining the mixture in an oxidizing atmosphere for 30 minutes at a temperature of 400 to 550 ° C with stirring.
  • adsorbent for
  • the pulping method is a pulp method based on the Kokuz P system, which is economically advantageous, and is an alternative to the conventional cooking wastewater treatment method.

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  • Paper (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)
PCT/JP1983/000092 1982-03-26 1983-03-26 Pulping process WO1983003435A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP57049733A JPS58169590A (ja) 1982-03-26 1982-03-26 パルプ化法
JP57/49733820326 1982-03-26

Publications (1)

Publication Number Publication Date
WO1983003435A1 true WO1983003435A1 (en) 1983-10-13

Family

ID=12839387

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP1983/000092 WO1983003435A1 (en) 1982-03-26 1983-03-26 Pulping process

Country Status (4)

Country Link
JP (1) JPS58169590A (enrdf_load_stackoverflow)
AU (1) AU545585B2 (enrdf_load_stackoverflow)
BR (1) BR8301549A (enrdf_load_stackoverflow)
WO (1) WO1983003435A1 (enrdf_load_stackoverflow)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4910870A (enrdf_load_stackoverflow) * 1972-05-30 1974-01-30
JPS55137287A (en) * 1979-04-05 1980-10-25 Kogyo Gijutsuin Sodium base pulping method
JPS55137286A (en) * 1979-04-05 1980-10-25 Kogyo Gijutsuin Magnesium base pulping method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4910870A (enrdf_load_stackoverflow) * 1972-05-30 1974-01-30
JPS55137287A (en) * 1979-04-05 1980-10-25 Kogyo Gijutsuin Sodium base pulping method
JPS55137286A (en) * 1979-04-05 1980-10-25 Kogyo Gijutsuin Magnesium base pulping method

Also Published As

Publication number Publication date
AU1373383A (en) 1983-10-24
JPH0220757B2 (enrdf_load_stackoverflow) 1990-05-10
BR8301549A (pt) 1983-12-06
AU545585B2 (en) 1985-07-18
JPS58169590A (ja) 1983-10-06

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