WO2018168620A1 - Procédé de production de pâte modifiée - Google Patents

Procédé de production de pâte modifiée Download PDF

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Publication number
WO2018168620A1
WO2018168620A1 PCT/JP2018/008896 JP2018008896W WO2018168620A1 WO 2018168620 A1 WO2018168620 A1 WO 2018168620A1 JP 2018008896 W JP2018008896 W JP 2018008896W WO 2018168620 A1 WO2018168620 A1 WO 2018168620A1
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WO
WIPO (PCT)
Prior art keywords
dehydration
pulp
modified pulp
dehydrator
modified
Prior art date
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PCT/JP2018/008896
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English (en)
Japanese (ja)
Inventor
裕亮 多田
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日本製紙株式会社
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Filing date
Publication date
Application filed by 日本製紙株式会社 filed Critical 日本製紙株式会社
Publication of WO2018168620A1 publication Critical patent/WO2018168620A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B1/00—Preparatory treatment of cellulose for making derivatives thereof, e.g. pre-treatment, pre-soaking, activation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
    • C08B15/04—Carboxycellulose, e.g. prepared by oxidation with nitrogen dioxide
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/16—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only modified by a particular after-treatment

Definitions

  • the present invention relates to a method for producing modified pulp such as oxidized pulp and metal-supported pulp.
  • Cellulose nanofibers are fibers having a nano-level fiber diameter of 1000 nm or less, and can be obtained by defibrating oxidized pulp (modified pulp) with mechanical shearing force (see, for example, Patent Document 1).
  • the manufactured product can have functions such as antibacterial and deodorant (for example, see Patent Document 2).
  • JP 2008-1728 A Japanese Patent Laying-Open No. 2015-84870
  • An object of the present invention is to provide a method for producing a modified pulp that efficiently produces a modified pulp.
  • the present invention provides the following (1) to (6).
  • the said predetermined time is the manufacturing method of the modified pulp as described in (1) prescribed
  • the dehydration and washing step includes a reaction solution dehydration for dehydrating the modified pulp dispersion obtained in the previous step, a primary dehydration for dehydrating the modified pulp dispersion after the reaction solution dehydration,
  • the modified pulp is a metal-supported pulp, the predetermined time for the reaction liquid dehydration is 1 to 3 minutes, and the predetermined time for the primary dehydration and the secondary dehydration is 3 to 5 minutes.
  • FIG. 1 is a configuration diagram of a dehydration / cleaning apparatus according to an embodiment.
  • modified pulp oxidized pulp, metal-carrying pulp
  • the pulp raw material means bleached or unbleached wood pulp, bleached or unbleached non-wood pulp, refined linter, pulp derived from herbs such as jute, manila hemp, kenaf, etc.
  • Examples include fine cellulose obtained by depolymerizing cellulose by performing mechanical treatment such as decomposition, enzymatic decomposition, blasting treatment, and vibration ball mill.
  • Oxidation process Carboxyl groups are introduced into the pulp by oxidizing the above pulp raw material in water using an oxidizing agent in the presence of a compound selected from the group consisting of N-oxyl compounds and bromides, iodides or mixtures thereof. Oxidized pulp can be obtained.
  • the N-oxyl compound is a compound capable of generating a nitroxy radical.
  • any compound can be used as long as it promotes the target oxidation reaction.
  • the amount of the N-oxyl compound used is not particularly limited as long as it is a catalyst amount capable of turning pulp into nanofibers.
  • 0.01 to 10 mmol is preferable, 0.01 to 1 mmol is more preferable, and 0.01 to 0.5 mmol is even more preferable with respect to 1 g of pulp dry.
  • Bromide is a compound containing bromine, and examples thereof include alkali metal bromide that can be dissociated and ionized in water.
  • an iodide is a compound containing iodine, and examples thereof include alkali metal iodide.
  • the amount of bromide or iodide used can be selected as long as the oxidation reaction can be promoted.
  • the total amount of bromide and iodide is, for example, preferably 0.1 to 100 mmol, more preferably 0.1 to 10 mmol, and still more preferably 0.5 to 5 mmol with respect to 1 g of an absolutely dry pulp raw material.
  • oxidizing agent known ones can be used, and for example, halogen, hypohalous acid, halous acid, perhalogen acid or salts thereof, halogen oxide, peroxide and the like can be used.
  • sodium hypochlorite which is the most widely used in industrial processes and has a low environmental load, is particularly preferable.
  • the appropriate amount of the oxidizing agent used is, for example, preferably 0.5 to 500 mmol, more preferably 0.5 to 50 mmol, still more preferably 1 to 25 mmol, and most preferably 3 to 10 mmol with respect to 1 g of the absolutely dry pulp material. preferable.
  • the dehydration / washing process is a process of washing the dispersion of oxidized pulp with water after the dehydration process.
  • the dehydration / washing process is performed three times in the dehydration / washing process. By performing this step, an oxidized pulp containing no impurities can be produced.
  • the dehydration treatment in the dehydration / washing process can use a centrifugal dehydration type, vacuum dehydration type, or pressure dehydration type dehydrator.
  • centrifugal dehydration type (Tanabe Wiltech centrifuge, Kokusan centrifuge, etc.), vacuum dehydration type (drum type vacuum dehydrator, Tsukishima Kikai horizontal belt filter, etc.), pressure dehydration type (filter) Press, tube press, screw press, belt press, horizontal belt filter, polydisc filter, vibrating screen, etc.) can be used.
  • the dispersion of oxidized pulp stored in the liquid source tank is sent to the dehydrator for dehydration.
  • the filtrate from the dehydrator is collected for a predetermined time (for example, 1 to 3 minutes) from the start of the liquid supply to the dehydrator and returned to the liquid source tank.
  • the oxidized pulp dispersion stored in the liquid supply source tank is sent to the dehydrator and dehydrated, for example, 1 to 3 minutes from the start of the liquid supply to the dehydrator, Collect the filtrate from the dehydrator and return it to the feed tank.
  • the dispersion of the oxidized pulp stored in the liquid supply source tank is sent to the dehydrator, and when dehydrating, for example, 1-3 minutes from the start of the liquid supply to the dehydrator Collect the filtrate from the machine and return it to the feed tank.
  • the dehydration is performed, for example, for 1 to 3 minutes from the start of the liquid supply to the dehydrator. Collect the filtrate from the machine and return it to the feed tank.
  • the predetermined time is defined for each type of modified pulp, and for a predetermined time, a cake of modified pulp having a predetermined thickness is formed inside the dewatering tank of the dehydrator and the like. What is necessary is just to set suitably the time when the outflow amount decreases. Therefore, different times may be used for reaction liquid dehydration, primary dehydration, and secondary dehydration.
  • the filtrate by the dehydrator is returned to the liquid supply source tank for a predetermined time after the start of the liquid supply to the dehydrator, the amount of oxidized pulp flowing out to the waste water can be reduced. Therefore, the yield of oxidized pulp can be improved and oxidized pulp can be produced efficiently while minimizing the extension of operation time.
  • the metal-supported pulp is one in which one or more metal particles selected from the group consisting of Ag, Au, Pt, Pd, Cu and Zn are supported on the oxidized pulp having a carboxyl group. It can be obtained by bringing the metal compound aqueous solution into contact with the oxidized pulp introduced with carboxyl groups into the pulp obtained in the step and bonding the carboxyl groups of the oxidized pulp with the metal compounds.
  • the metal compound aqueous solution is an aqueous solution of a metal salt or an organometallic compound.
  • metal salts include complexes (complex ions), halides, nitrates, sulfates, and acetates.
  • the metal salt is preferably water-soluble.
  • a dispersion of oxidized pulp prepared in advance and an aqueous solution of metal compound may be mixed, and a dispersion containing oxidized pulp is applied onto a substrate to form a film, and the metal compound is applied to the film.
  • An aqueous solution may be dropped and impregnated. At this time, the film may remain fixed on the substrate or may be peeled from the substrate.
  • the concentration of the aqueous metal compound solution is not particularly limited. You may adjust suitably the time which a metal compound is made to contact.
  • the temperature at the time of contact is not particularly limited, but 20 to 40 ° C. is preferable.
  • the pH of the liquid at the time of contact is preferably 2.5 to 13.
  • metal particles are formed by reducing the metal compound bound to the oxidized pulp obtained as described above.
  • the reduction reaction may be performed by a known method, but it is preferable to perform the reduction reaction so as not to cleave the bond between the metal compound and the acid group while reducing the metal compound.
  • Examples of such a reduction method include a gas phase reduction method using hydrogen and a liquid phase reduction method using a reducing agent such as an aqueous sodium borohydride solution.
  • the dehydration / washing process is a process of washing the metal-supported pulp dispersion with water after the dehydration process.
  • the dehydration / washing process is performed three times in the dehydration / washing process.
  • the same dehydrator as used in the production of oxidized pulp can be used.
  • the metal-supported pulp dispersion liquid stored in the liquid supply source tank is sent to the dehydrator.
  • the filtrate from the dehydrator is collected for a predetermined time (for example, 1 to 5 minutes) from the start of liquid supply to the dehydrator and returned to the liquid source tank.
  • the metal-supported pulp dispersion stored in the liquid supply source tank is sent to the dehydrator and dehydrated, for example, 1 starts from the start of the liquid supply to the dehydrator. Collect the filtrate from the dehydrator for ⁇ 3 minutes and return it to the liquid source tank.
  • the metal-supported pulp dispersion stored in the liquid source tank is sent to the dehydrator, and when dehydrating, for example, 3 to 5 minutes from the start of the liquid supply to the dehydrator. Collect the filtrate from the machine and return it to the feed tank.
  • the dehydration is performed, for example, for 3 to 5 minutes from the start of the liquid supply to the dehydrator. Collect the filtrate from the machine and return it to the feed tank.
  • the filtrate by the dehydrator is returned to the liquid supply source tank for a predetermined time after the start of the liquid supply to the dehydrator, the amount of the metal-supported pulp flowing out to the waste water can be reduced. Accordingly, the yield of the metal-supported pulp can be improved and the metal-supported pulp can be efficiently manufactured while minimizing the extension of the operation time.
  • the liquid supply source tank 2 in which the oxidized pulp dispersion liquid is stored is connected to a centrifugal dehydrator 6 via a liquid supply pipe 4.
  • the centrifugal dehydrator 6 is used in a state where a filter cloth is wound around the inside of the dewatering tank.
  • a filter cloth having an air permeability of 20 cm 3 / cm 2 ⁇ sec is used.
  • the liquid feeding pipe 4 is provided with a pump 8 for feeding the oxidized pulp dispersion liquid to the centrifugal dehydrator 6.
  • the centrifugal dehydrator 6 is connected to the liquid supply source tank 2 via a return pipe 10 that returns the filtrate to the liquid supply source tank 2, and is connected to a drainage pit 14 via a drainage pipe 12 that drains the filtrate. Has been. Switching of the flow path from the centrifugal dehydrator 6 to the liquid supply source tank 2 or the drain pit 14 is performed by opening and closing the first valve 16 and the second valve 18.
  • the dehydration / washing apparatus shown in FIG. 1 is provided with dedicated devices for reaction liquid dehydration, primary dehydration, and secondary dehydration, and suspended substances (oxidation) recovered by reaction liquid dehydration are provided. Pulp) is subjected to primary dehydration, and secondary dehydration is performed using a suspension of suspended matter (oxidized pulp) recovered by the primary dehydration.
  • the metal-supported pulp is 1 minute after feeding the reaction liquid dehydration, and the primary dehydration and the secondary dehydration are 3 minutes after feeding. If the filtrate is collected, then the suspended matter in the filtrate The amount was found to decrease.

Abstract

Selon l'invention, un procédé de production de pâte modifiée comprend une étape de déshydratation/lavage consistant à effectuer un traitement de déshydratation/lavage sur la pâte modifiée, où : une pluralité de cycles du traitement de déshydratation/lavage de la pâte modifiée sont effectués dans l'étape de déshydratation/lavage ; et lorsque la pâte modifiée, ayant été recueillie dans une cuve source d'envoi de solution, est déshydratée par une machine de déshydratation dans la pluralité de cycles du traitement de déshydratation/lavage, du filtrat provenant de la machine de déshydratation est recueilli et renvoyé à la cuve source d'envoi de solution pendant une durée prédéterminée à partir d'un début d'alimentation en solution de la machine de déshydratation qui a été établie pour chacun des cycles.
PCT/JP2018/008896 2017-03-17 2018-03-08 Procédé de production de pâte modifiée WO2018168620A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2017052845A JP2018154740A (ja) 2017-03-17 2017-03-17 変性パルプの製造方法
JP2017-052845 2017-03-17

Publications (1)

Publication Number Publication Date
WO2018168620A1 true WO2018168620A1 (fr) 2018-09-20

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WO (1) WO2018168620A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110174471A (zh) * 2019-05-13 2019-08-27 山东省农业科学院农业质量标准与检测技术研究所 花生油中黄曲霉毒素的前处理方法及检测方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012520944A (ja) * 2009-03-20 2012-09-10 エフピーイノベイションズ 新規の特性を有するセルロース材料
JP2013067904A (ja) * 2011-09-22 2013-04-18 Nippon Paper Industries Co Ltd 酸化パルプの洗浄及び脱水方法
JP2013067906A (ja) * 2011-09-22 2013-04-18 Nippon Paper Industries Co Ltd 酸化パルプの洗浄・脱水方法
WO2014007105A1 (fr) * 2012-07-06 2014-01-09 日本製紙株式会社 Fibre recyclée et produit moulé en fibre recyclée
JP2014125690A (ja) * 2012-12-26 2014-07-07 Oji Holdings Corp 微細セルロース繊維の製造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012520944A (ja) * 2009-03-20 2012-09-10 エフピーイノベイションズ 新規の特性を有するセルロース材料
JP2013067904A (ja) * 2011-09-22 2013-04-18 Nippon Paper Industries Co Ltd 酸化パルプの洗浄及び脱水方法
JP2013067906A (ja) * 2011-09-22 2013-04-18 Nippon Paper Industries Co Ltd 酸化パルプの洗浄・脱水方法
WO2014007105A1 (fr) * 2012-07-06 2014-01-09 日本製紙株式会社 Fibre recyclée et produit moulé en fibre recyclée
JP2014125690A (ja) * 2012-12-26 2014-07-07 Oji Holdings Corp 微細セルロース繊維の製造方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110174471A (zh) * 2019-05-13 2019-08-27 山东省农业科学院农业质量标准与检测技术研究所 花生油中黄曲霉毒素的前处理方法及检测方法

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