WO2018130528A1 - Prévention des dépôts dans la production de cellulose selon le procédé au sulfate (dissolution kraft) - Google Patents

Prévention des dépôts dans la production de cellulose selon le procédé au sulfate (dissolution kraft) Download PDF

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Publication number
WO2018130528A1
WO2018130528A1 PCT/EP2018/050472 EP2018050472W WO2018130528A1 WO 2018130528 A1 WO2018130528 A1 WO 2018130528A1 EP 2018050472 W EP2018050472 W EP 2018050472W WO 2018130528 A1 WO2018130528 A1 WO 2018130528A1
Authority
WO
WIPO (PCT)
Prior art keywords
acid
monoethylenically unsaturated
acids
group
comb polymers
Prior art date
Application number
PCT/EP2018/050472
Other languages
German (de)
English (en)
Inventor
Bernd Horrer
Silvia Held-Beller
Original Assignee
CHT Germany GmbH
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 CHT Germany GmbH filed Critical CHT Germany GmbH
Priority to BR112019013116A priority Critical patent/BR112019013116A2/pt
Priority to ES18701117T priority patent/ES2845552T3/es
Priority to CA3043462A priority patent/CA3043462A1/fr
Priority to RU2019121787A priority patent/RU2746828C2/ru
Priority to AU2018207866A priority patent/AU2018207866B2/en
Priority to EP18701117.6A priority patent/EP3568519B1/fr
Priority to PL18701117T priority patent/PL3568519T3/pl
Publication of WO2018130528A1 publication Critical patent/WO2018130528A1/fr

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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
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/22—Other features of pulping processes
    • D21C3/226—Use of compounds avoiding scale formation
    • 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
    • D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
    • 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
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/02—Washing ; Displacing cooking or pulp-treating liquors contained in the pulp by fluids, e.g. wash water or other pulp-treating agents

Definitions

  • the present invention relates to the use of comb polymers as scale inhibitors in pulp production by the sulfate process (Kraft pulping).
  • the most important and most frequently used process for the production of pulp is the sulphate or kraft process.
  • C.F. Dahl patented a process using sodium sulfide or sodium sulfate, respectively.
  • the resulting sulphate pulp is preferred because of its high strength, especially for mechanically stressed paper "kraft papers” and therefore also kraft pulp.
  • the basis of the method is the partial solubility of lignin in hot solutions.
  • the alkaline process uses cooking liquors containing sodium hydroxide, sodium sulfide, sodium sulfate and sodium carbonate.
  • the chips are treated in pressure vessels for three to six hours at elevated pressure (7 to 10 bar) and at a temperature of 140 to 170 ° C.
  • sodium sulfide increases the delignification, in which the lignin is split by a nucleophilic attack of the sulfide anion and turns into the so-called black liquor (soluble alkali lignin), and on the other hand, the fiber lengths are increased.
  • carbohydrates are also degraded in the more alkaline range.
  • Polysulfide-containing lyes stabilize the polyoses. Paper made of Kraftpulp is tear-resistant, unbreakable and tensile. Advantages of the sulphate process are a good impregnation of the chips in alkaline solution and thus shorter cooking times, it can be used virtually all woods.
  • Sulfate pulps contain even larger amounts of polyoses and are darker than sulfite pulps. They do not have a sufficiently high content of ⁇ -cellulose for the production of cellulose derivatives.
  • the lignin-containing waste liquors arising from the sulphate process are concentrated and incinerated so that the energy requirement of the entire process can be met.
  • turpentine oil and about 30 to 35 kg of tall oil per 1,000 kg of pulp are produced.
  • JPH 1025684 (A) describes a terpolymer based on maleic acid, acrylic acid and 2-acrylamido-2-methylpropanesulfonic acid (AMPS) having a molecular weight of 500 to 20,000 g / mol.
  • AMPS 2-acrylamido-2-methylpropanesulfonic acid
  • No. 5,409,571 A discloses a copolymer based on maleic acid and acrylic acid which has been polymerized with the addition of hypophosphite.
  • the molecular weight is 500 to 10,000 g / mol.
  • polyitaconic acid in a mixture with phosphonic acids is known from JP 2011-052358 (A).
  • Scale inhibitor-1 polyitaconic acid and l-hydroxyethylidene-l, l-diphosphonic acid (HEDP) are mixed.
  • JP 2014-147911 discloses a mixture of two polyitaconic acid polymers having different molecular weights.
  • Polymer A has a molecular weight of 500 to 15,000 g / mol and Polymer B has a molecular weight of 15,000 to 40,000 g / mol.
  • WO 00/12436 A claims a copolymer of l, 2-dihydroxy-3-butene, and another monomer from the group of maleic acid, acrylic acid, acrylamide, methacrylic acid, itaconic acid, vinylsulfonic acid, styrenesulfonic acid, N-tert-butylacrylamide, butoxymethylacrylamide , N, N-dimethylacrylamide, 2-acrylamido-2-methylpropanesulfonic acid and salts thereof.
  • the publications listed are exclusively concerned with the inhibition of deposits of inorganic calcium carbonate.
  • WO 2010/019425 AI gives in the cited prior art a good overview of which substances can be used as a resin dispersant.
  • the application itself claims a mixture of triglyceride oil or triglyceride alkyl esters with polyalkylene glycol based surfactants and / or resin, rosin soaps, tall oil, tall oil soaps and derivatives thereof.
  • WO 2008/057492 A2 describes a copolymer of vinyl alcohol and vinyl acetate and hydrophobically modified hydroxyethyl cellulose as a detackifier. Also mentioned are enzymes which catalyze the hydrolysis of resin.
  • WO 2004/057101 A1 discloses a mixture of fatty acids and resin acids as an effective dispersant with respect to extractable substances.
  • the publications listed are exclusively concerned with the inhibition of organic resin deposits.
  • the object of the present invention is the ne gative ⁇ influencing the CaC0 3 -Ablagerungsinhibitoren by resin dispersant during the kraft cooking process effectively underbin ⁇ .
  • polymers are to be provided which effectively inhibit the deposits of CaCO 3 during the cooking process. when working with the addition of resin dispersants based on organic carboxylic acids.
  • the comb polymers used according to the invention can be obtained by a free radical polymerization of monoethylenically unsaturated monomers of the group AI) monoethylenically unsaturated acids and their salts and the group A2) monoethylenically unsaturated polyethers.
  • the invention therefore provides the use of comb polymers obtainable by a free-radical polymerization of monoethylenically unsaturated monomers
  • Examples of the monomers of group AI, the monoethylenically unsaturated acids and their salts are acrylic acid, methacrylic acid, crotonic acid, maleic acid, fumaric acid, itaconic acid, vinylsulfonic acid, allylsulfonic acid, methallylsulfonic acid, 2-acrylamido-2-methylpropanesulfonic acid, styrenesulfonic acid, vinylphosphonic.
  • the monomers of group AI can be used individually or as a mixture of different monomers.
  • acrylic acid, methacrylic acid or maleic acid in an amount of from 5 to 95% by weight, based on the polymer, acrylic acid or maleic acid being particularly preferably used in an amount of from 10 to 90% by weight, based on the polymer.
  • the monoethylenically unsaturated polyethers are polyethylene glycol monoallyl ether, polypropyleneglycol monoallyl ether and polyethylene-polypropylene monoallyl ether; these are, for example, by the company. Clariant under the product number polyglycol ® A, from Fa. BASF ® under the product number Pluriol A ... R or by the company. NOF Corporation under the product rows Uniox ® 'Unisafe ® and Unilube ® commercially available. Further examples are Polyethylenglycolmonovinylether (range from Clariant. Polyglycol ® R) Isoprenylethoxilate (product series from BASF. Pluriol ® A ... I) and Vinyloxybutylethoxilate (product series from BASF. Pluriol ® A ... V).
  • the monomers of group A2 can be OH-terminated or have an end-group bond.
  • the monomers may be used singly or as mixtures of different monomers. Preference is given to using polyalkyl glycol monoallyl ethers in an amount of from 2 to 25% by weight, based on the polymer, more preferably using polyethylene glycol monoallyl ether and polyethylene-polypropylene monoallyl ether with an amount of from 5 to 20% by weight, based on the polymer.
  • the use according to the invention can be carried out as part of pulp production by the sulphate process in a continuous or discontinuous process such that the comb polymer is added separately to a cooking liquor, or the comb polymer is introduced into the cooking liquor as a constituent of the CaC0 3 deposition inhibitor or the resin dispersant.
  • Another object of the invention is therefore a CaC0 3 deposition inhibitor containing a comb polymer according to the invention.
  • CaC0 3 deposition inhibitors and resin dispersants containing the comb polymer to be used in the present invention may contain any of the usual ingredients of such agents which do not undesirably interact therewith.
  • such a CaC0 3 deposition inhibitor contains polymers as mono-, co- and terpolymers based on monoethylenically unsaturated acids and their salts, such as acrylic acid, methacrylic acid, crotonic acid, maleic acid, fumaric acid, itaconic acid, vinylsulfonic acid, allylsulfonic acid, Methallylsulfonic acid, 2-acrylamido-2-methylpropanesulfonic acid, styrenesulfonic acid, vinylphosphonic acid, acrylamide, N-tert-butylacrylamide, butoxymethylacrylamide and N, N-dimethylacrylamide.
  • the solution was made with demineralized water.
  • the 140 ° C was maintained for a further 30 minutes.
  • the contents of the cup were then cooled to 80 ° C, the cups were opened and the hot solution filtered through black filter.
  • ⁇ 5 amorphous and crystalline deposits
  • Standard polymer acrylic acid / maleic acid copolymer, which is used as a deposit inhibitor in pulp boiling in the sulfate process in practice.
  • Experiment No. 1 clearly shows what massive crystalline deposits can be formed under pulp cooking conditions when no scale inhibitor is used.
  • the coarse-crystalline structure leads to a complete and rapid filtration of the deposits, the filtrate is clear.
  • different levels of scale inhibitors were added.
  • the test parameters are only insignificantly influenced.
  • Mainly coarse-crystalline structures are formed, which lead to rapid and complete filtration. From a concentration of 40 mg, the results change abruptly.
  • the crystal structure changes from coarse-crystalline to fine-amorphous.
  • the pores of the filter material are added quickly and there is a significant reduction in the filtration rate. From experience, the mechanism of crystal modification is necessary to practice effective to prevent CaC0 3 deposits during pulp cooking.
  • Experiment No. 5 shows the effect of tall oil on the resulting deposits. Compared to experiment # 1, the deposits on the filter have obviously increased.
  • Experiment No. 6 now discloses the whole problem known from practice that the standard polymers fail by the use of tall oil and are no longer sufficiently effective. If the standard polymer in Experiment No. 4 could still effectively modify the resulting deposits, it completely fails in Experiment No. 6. An increase in the amount used (experiments Nos. 7 and 8) does improve the situation, but it is far from having sufficient effect.

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Paper (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Polyethers (AREA)

Abstract

L'invention concerne l'utilisation de polymères en peigne qui peuvent être obtenus par une polymérisation radicalaire de monomères monoéthyléniques insaturés du groupe A1) acides monoéthyléniques insaturés et leurs sels et du groupe A2) polyéther monoéthylénique insaturé, en tant qu'inhibiteurs des dépôts dans la production de cellulose selon le procédé au sulfate (dissolution kraft).
PCT/EP2018/050472 2017-01-12 2018-01-09 Prévention des dépôts dans la production de cellulose selon le procédé au sulfate (dissolution kraft) WO2018130528A1 (fr)

Priority Applications (7)

Application Number Priority Date Filing Date Title
BR112019013116A BR112019013116A2 (pt) 2017-01-12 2018-01-09 uso de polímeros em pente e inibidor de deposição para produção de polpa de acordo com o método de sulfato (polpação kraft)
ES18701117T ES2845552T3 (es) 2017-01-12 2018-01-09 Inhibición de la sedimentación en la fabricación de celulosa de acuerdo con el procedimiento del sulfato (digestión de Kraft)
CA3043462A CA3043462A1 (fr) 2017-01-12 2018-01-09 Prevention des depots dans la production de cellulose selon le procede au sulfate (dissolution kraft)
RU2019121787A RU2746828C2 (ru) 2017-01-12 2018-01-09 Применение гребнеобразных полимеров в качестве ингибиторов отложений при производстве целлюлозы сульфатным способом (крафт-процесс)
AU2018207866A AU2018207866B2 (en) 2017-01-12 2018-01-09 Deposit prevention in pulp production according to the sulphate process (kraft process)
EP18701117.6A EP3568519B1 (fr) 2017-01-12 2018-01-09 Prévention des dépôts dans la production de cellulose selon le procédé au sulfate (dissolution kraft)
PL18701117T PL3568519T3 (pl) 2017-01-12 2018-01-09 Zapobieganie tworzeniu się osadu w produkcji pulpy w procesie siarczanowym (roztwarzanie kraft)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102017200430.4 2017-01-12
DE102017200430.4A DE102017200430A1 (de) 2017-01-12 2017-01-12 Ablagerungsverhinderung in der Zellstoff-Herstellung nach dem Sulfatverfahren (Kraft-Aufschluss)

Publications (1)

Publication Number Publication Date
WO2018130528A1 true WO2018130528A1 (fr) 2018-07-19

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2018/050472 WO2018130528A1 (fr) 2017-01-12 2018-01-09 Prévention des dépôts dans la production de cellulose selon le procédé au sulfate (dissolution kraft)

Country Status (11)

Country Link
EP (1) EP3568519B1 (fr)
AU (1) AU2018207866B2 (fr)
BR (1) BR112019013116A2 (fr)
CA (1) CA3043462A1 (fr)
CL (1) CL2019001599A1 (fr)
DE (1) DE102017200430A1 (fr)
ES (1) ES2845552T3 (fr)
PL (1) PL3568519T3 (fr)
PT (1) PT3568519T (fr)
RU (1) RU2746828C2 (fr)
WO (1) WO2018130528A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109665634A (zh) * 2019-01-30 2019-04-23 上海电力学院 一种高分子阻垢缓蚀剂及其制备方法和应用

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT202200003134A1 (it) 2022-02-21 2023-08-21 Alter Eco Pulp S R L Metodo di estrazione della cellulosa da biomasse di scarto

Citations (13)

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Publication number Priority date Publication date Assignee Title
US4500693A (en) * 1981-07-07 1985-02-19 Nippon Shokubai Kagaku Kogyo Co., Ltd. Water soluble copolymer method for manufacture therefore and use thereof
EP0537870A1 (fr) 1991-10-18 1993-04-21 W.R. Grace & Co.-Conn. Copolymères d'ethers insaturés éthyléniquement utilisables comme superplastifiants pour ciment hydraulique
US5409571A (en) 1992-08-27 1995-04-25 Hakuto Co., Ltd. Scale deposit inhibitor for kraft digesters and method for controlling scale deposition in kraft digesters
WO2000012436A1 (fr) 1998-08-31 2000-03-09 Nalco Chemical Company Procede d'inhibition d'incrustations dans des systemes a conditions severes et anti-incrustation associes
WO2002098802A1 (fr) 2001-06-06 2002-12-12 Solutia Inc. Procede empechant la formation de depots de sels de calcium
WO2002098803A1 (fr) 2001-06-06 2002-12-12 Solutia Inc. Methode pouvant inhiber l'entartrage par le sel de calcium
WO2004057101A1 (fr) 2002-12-23 2004-07-08 Arizona Chemical B.V. Aide de cuisson pour ameliorer l'enlevement de matieres extractives dans la production de pulpe, sa production et son utilisation
WO2008057492A2 (fr) 2006-11-06 2008-05-15 Hercules Incorporated Procédés permettant de lutter contre l'empoissement et l'encrassement lors de la fabrication de papier et pâte à papier
EP2020422A1 (fr) * 2007-07-31 2009-02-04 Sika Technology AG Polymères émulsifiants et leur utilisation
WO2010019425A1 (fr) 2008-08-15 2010-02-18 Hercules Incorporated Additifs de réduction en pâte pour une réduction de la quantité de résine dans de la pâte kraft
JP2011052358A (ja) 2009-09-04 2011-03-17 Hakuto Co Ltd スケール防止剤およびスケール防止方法
JP2014147911A (ja) 2013-02-04 2014-08-21 Hakuto Co Ltd スケール防止剤及びスケール防止方法
DE102013207778A1 (de) * 2013-04-29 2014-10-30 Cht R. Beitlich Gmbh Kammpolymere als Waschkraftverstärker für Wasch- und Reinigungsmittel

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US5534157A (en) * 1994-11-10 1996-07-09 Calgon Corporation Polyether polyamino methylene phosphonates for high pH scale control
JP3088085B2 (ja) * 1996-12-27 2000-09-18 株式会社日本触媒 スケール防止剤
FR2894998A1 (fr) * 2005-12-16 2007-06-22 Coatex Sas Procede de fabrication de sauces de couchage a la retention d'eau et a la viscosite brookfield ameliorees mettant en oeuvre un polymere peigne avec au moins une fonction greffee oxyde de polyalkylene.
WO2009093615A1 (fr) * 2008-01-22 2009-07-30 Lion Corporation Détergent pour pâte kraft et procédé de production de pâte kraft avec celui-ci
WO2015153349A1 (fr) * 2014-03-31 2015-10-08 Dow Global Technologies Llc Modificateur de rhéologie sous forme de polymère synthétique et agent de rétention d'eau destiné à remplacer l'éther de cellulose dans des compositions de ciment

Patent Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4500693A (en) * 1981-07-07 1985-02-19 Nippon Shokubai Kagaku Kogyo Co., Ltd. Water soluble copolymer method for manufacture therefore and use thereof
EP0537870A1 (fr) 1991-10-18 1993-04-21 W.R. Grace & Co.-Conn. Copolymères d'ethers insaturés éthyléniquement utilisables comme superplastifiants pour ciment hydraulique
US5409571A (en) 1992-08-27 1995-04-25 Hakuto Co., Ltd. Scale deposit inhibitor for kraft digesters and method for controlling scale deposition in kraft digesters
WO2000012436A1 (fr) 1998-08-31 2000-03-09 Nalco Chemical Company Procede d'inhibition d'incrustations dans des systemes a conditions severes et anti-incrustation associes
WO2002098802A1 (fr) 2001-06-06 2002-12-12 Solutia Inc. Procede empechant la formation de depots de sels de calcium
WO2002098803A1 (fr) 2001-06-06 2002-12-12 Solutia Inc. Methode pouvant inhiber l'entartrage par le sel de calcium
WO2004057101A1 (fr) 2002-12-23 2004-07-08 Arizona Chemical B.V. Aide de cuisson pour ameliorer l'enlevement de matieres extractives dans la production de pulpe, sa production et son utilisation
WO2008057492A2 (fr) 2006-11-06 2008-05-15 Hercules Incorporated Procédés permettant de lutter contre l'empoissement et l'encrassement lors de la fabrication de papier et pâte à papier
EP2020422A1 (fr) * 2007-07-31 2009-02-04 Sika Technology AG Polymères émulsifiants et leur utilisation
WO2010019425A1 (fr) 2008-08-15 2010-02-18 Hercules Incorporated Additifs de réduction en pâte pour une réduction de la quantité de résine dans de la pâte kraft
JP2011052358A (ja) 2009-09-04 2011-03-17 Hakuto Co Ltd スケール防止剤およびスケール防止方法
JP2014147911A (ja) 2013-02-04 2014-08-21 Hakuto Co Ltd スケール防止剤及びスケール防止方法
DE102013207778A1 (de) * 2013-04-29 2014-10-30 Cht R. Beitlich Gmbh Kammpolymere als Waschkraftverstärker für Wasch- und Reinigungsmittel

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109665634A (zh) * 2019-01-30 2019-04-23 上海电力学院 一种高分子阻垢缓蚀剂及其制备方法和应用

Also Published As

Publication number Publication date
AU2018207866B2 (en) 2022-04-14
AU2018207866A1 (en) 2019-05-23
ES2845552T3 (es) 2021-07-27
RU2746828C2 (ru) 2021-04-21
DE102017200430A1 (de) 2018-07-12
EP3568519A1 (fr) 2019-11-20
BR112019013116A2 (pt) 2019-12-17
RU2019121787A3 (fr) 2021-02-12
PL3568519T3 (pl) 2021-05-31
EP3568519B1 (fr) 2020-11-18
CL2019001599A1 (es) 2019-08-23
PT3568519T (pt) 2021-02-10
RU2019121787A (ru) 2021-02-12
CA3043462A1 (fr) 2018-07-19

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