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US20070272377A1 - Fully Closed, Zero Discharge, Clean Oxidizing Pulping Technology and Process - Google Patents

Fully Closed, Zero Discharge, Clean Oxidizing Pulping Technology and Process Download PDF

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Publication number
US20070272377A1
US20070272377A1 US10/583,763 US58376303A US2007272377A1 US 20070272377 A1 US20070272377 A1 US 20070272377A1 US 58376303 A US58376303 A US 58376303A US 2007272377 A1 US2007272377 A1 US 2007272377A1
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water
materials
accordance
active oxygen
pulp
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Xiuquan Mei
Laisu Xie
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    • 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
    • D21C9/001—Modification of pulp properties
    • D21C9/002—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives
    • D21C9/004—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives inorganic compounds
    • 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

Definitions

  • the invention relates to a process for a fully closed, zero discharge, clean oxidizing pulping technology and process. It is practically a process that involves a method with close-loop, self-cycling, non-acid, non-alkali, non-chlorine, non-anthraquinone, non-cooking, non-bleaching, non-draining and non-pollution.
  • non-wood fiber materials can be categorized as: 1. the grass fiber materials 2. base fiber materials 3. cotton linters fiber materials 4. leaf fiber materials. And the holocellulose content is 48%-84%. The length of most non-wood fiber is longer than that of wood fiber and cellulose is main content used in papermaking. Cellulose extracted both from wood and non-wood materials can be used as supporting materials of paper and raw material of middle or high quality pulp. It is demonstrated that in the fiber of non-wood materials such as cotton stalk, all kinds of chemical components are similar to that of hard wood and soft wood. China is an agricultural country and also is a cotton-producing country. Annual resource that can compare favorably with wood is about 0.16 billion tons.
  • Anthraquinone belongs to the fused polycyclic hydrocardes of arenes.
  • the fused polycyclic hydrocardes have been confirmed to be the carcinogen.
  • a carcinogen structure made of anthracene is as follows:
  • Pulp bleaching with ClO 2 and O 3 invented by France liquid air company was made public at Mar. 31, 1999. Pulping of cornstalk and other non-wood fiber materials (CN1371439A) invented by America Carolina State University was made public at Sep. 25, 2002. A method that produces pulp by non-wood and its preparation system equipment (CN1407172A) invented by Japan business corporation, a pollution-free pulping method (CNI198492) invented by Shandong Weichang Normal University, a pulping method without alkali (CN1229155) and a pulp bleaching electrochemical technology of polyoxometallate (CN1458075) were made public at Apr. 2, 2003.
  • the invention overcomes the current technical shortcomings and provides a close-loop, self-cycling, zero discharge, clean oxidizing pulping technology and process.
  • Clean pulping process and preparation method of the invention are carried out by undermentioned technical projects.
  • the character of the invention is that materials of the clean pulping process and the preparation method are non-wood and wood. Preparation of the pulp can be finished according to undermentioned processes.
  • the active oxygen A is selected from O 2 , H 2 O 2 , and one or two free radicals generated from O 2 , H 2 O 2 .
  • the active oxygen B is selected from O 3 , 1 O 2 (singlet oxygen), O 2 . ⁇ /HOO. (superoxide anion radical) and one or multiform free radicals generated from O 3 , 1 O 2 , O 2 . ⁇ /HOO. in water in which organic solvent exists.
  • the organic solvent for example, is DMSO or oxalic acid.
  • a kind of pulp is obtained by above process.
  • the non-wood materials such as full cotton stalk includes cotton bast, cotton stem, cotton stalk root and full cotton holocellulose, cellulose and hemicellulose of valvular cotton, cotton short linter, cotton dregs, cottonseed, a kind of lignin or two or multi-kinds of their compounds.
  • the described wood fiber includes soft wood and hard wood such as Masson pine, longitudinal white pine, David poplar, fast-growing poplar, birch and so on.
  • the metal ions are selected from Mg 2+ , Fe 2+ , Mn 2+ , Cu 2+ , Al 3+ , Zn 2+ , Si 2+ and two or multi-kinds of their compounds.
  • the metallic ion ligands include DMD, DTPA, EDTA, alkyl-sulfonic acid sodium, poly-oxyethyl-enabkylether and two or multi-kinds of their compounds.
  • dosage of the metal ions is between 1-1000 ppm.
  • the oxidizing dipping treatment is carried out in acidic condition whose pH is between 1-4, and the best pH is between 1.5-2.5.
  • the grinding treatment is carried out in acidic condition whose pH is between 1-4, and the best pH is between 2.5-3.8.
  • the acidic condition can be obtained by active oxygen of the invention (such as HOO.) and also can be obtained by pH regulator.
  • the concentration of active oxygen A in above materials is 0.01-2.0 wt %
  • the concentration of active oxygen 8 in above materials is 0.1-50 umol/L.
  • a kind of method as stated above has undermentioned characters and advantages:
  • C Self-cycling: All water in the process from the pretreatment of raw materials till the delivery of it to the oxidation reactor is divided into two parts to accomplish the self-cycling in the process. One is the water from the process of materials cleaning pretreatment.
  • the pulps are sent to the common beating process. Water generated in the process is cycled into purification pool. 0.1%-0.15% ozonizer and acticarbon nutsch filter are installed in the purification pool to decolor the water. The water contains oxygen free radical and it is pumped into the cycling water system. The other is the water from the oxidizing process. After cleaned with centrifugal cleaner and then is concentrated with common decker, the pulp is sent to the tank for papermaking. The produced water is filtrated and placed in the water-purifying tank for self-cycling. The purified water is pumped into materials cleaning system, oxygen dipping system, oxygen grinding system and filtrating system for recycling use.
  • the present invention takes advantage of active oxygen free radicals generated by oxidation-reduction reaction of molecular oxygen in reactor to transform and separate lignin, and to change chromophoric group in the intercellular space and obtain paper pulp.
  • the conventional pulping technologies that use harmful polluting chemicals such as acid, alkaline, chlorine, anthraquinone and so on are basically changed in the present invention.
  • the cooking and bleaching process, generating severe pollution, can be avoided.
  • the abundant yearly grown fiber materials can be utilized in this process and water and energy can be saved. As a result, the cost of production can be saved.
  • the active oxygen is added in the materials and high-concentration defibrator generates grinding heat reaction by grinding, which is used to change lignin's chromophore of intercellular space.
  • the special free radicals formed by three oxygen atoms of molecule oxygen has strong attack power and internal nucleophilic attack power, the electrophilic reaction occurs between special free radicals and lignin.
  • the lignin structural element phenyl and exocyclic big ⁇ circle around (7) ⁇ -bond are broken, and then lignin is degradated and dissolved.
  • the chromophore of lignin is changed or decomposed into low-molecular, then forms achromictintless monolarboxylic acid or binary carboxylic acid.
  • the invention also includes the pulp made by above process.
  • the character of the invention is that materials of the cleaning pulping process and the preparation method is non-wood and wood. Preparation of the pulp can be finished according to undermentioned processes.
  • the active oxygen A is selected from O 2 , H 2 O 2 , and one or two free radicals generated from O 2 , H 2 O 2 .
  • the active oxygen B is selected from O 3 , 1 O 2 (singlet oxygen) O 2 . ⁇ /HOO. (superoxide anion radical) and one or multi-free radicals generated from O 3 , 1 O 2 , O 2 . ⁇ /HOO. in water in which organic solvent exists.
  • Active oxygen can be obtained when O 2 passes through process radiator in which the oxidation-reduction reaction can occur and the energy is provided, at last water is formed.
  • process radiator in which the oxidation-reduction reaction can occur and the energy is provided, at last water is formed.
  • one oxygen free radical will be generated when one electron is absorbed by O 2 .
  • hyperoxidized anion free radical is formed when O 2 is reduced by one electron and its equation is: O 2 +e ⁇ O 2 . ⁇ /HOO.
  • Hydrogen peroxide is formed when O 2 is reduced by two electrons and its equation is: O 2 +2e+2H + ⁇ H 2 O 2 .
  • Hydroxy free radical is formed when O 2 is reduced by three electrons and free radical is formed by reaction of Fe 2+ and H 2 O 2 , which are special free radicals of water treatment and their equations are: O 2 +3e+3H + ⁇ H 2 O+.OH, Fe 2+ +H 2 O 2 ⁇ Fe 3+ +.OH+OH ⁇ .
  • the metal ions are selected from Mg 2+ , Fe 2+ , Mn 2+ , Cu 2+ , Al 3+ , Zn 2+ , Si 2+ and two or multi-kinds of their compounds and the ions are in the form of salt such as FeSO 4 , MgCO 3 etc.
  • the metallic ion ligands is selected from DMD, DTPA, EDTA, alkyl-sulfonic acid sodium, poly-oxyethyl-enabkylether and two or multi-kinds of their compounds.
  • the metallic ion ligand together with the metal ion, the metallic ion ligand, hyperoxidized anion free radical (O 2 ⁇ /HOO.) and H 2 O 2 , they form a functional cellulose protection system which can not only protect cellulose but also get rid of silicon.
  • Pretreatment usually includes removing impurity, shear, fiberization and cleanout with concrete condition.
  • the oxidizing dipping treatment is carried out in acidic condition whose pH is between 1-4, and the best pH is between 1.5-2.5.
  • the grinding treatment is carried out in acidic condition whose pH is between 1-4, and the best pH is between 2.5-3.8.
  • the acidic condition can be obtained by active oxygen of the invention (such as HOO ) and also can be obtained by pH regulator.
  • active oxygen of the invention such as HOO
  • pH regulator also can be obtained by pH regulator.
  • the ions are usually used in the form of salt and its dosage range is commonly between 1-1000 ppm, the best range is between 10-100 ppm according to weight of metal ion.
  • the non-cooking involves that, the conventional cooking process can be omitted.
  • the active oxygen is dropped into the disc refiner, in which heat energy is generated through the rotation of the disc, and the energy transferred reaction is generated, then the fiber is separated from the intercellular space.
  • non-conventional bleaching process involves that: the bleaching process can be omitted.
  • the cooperation of the active oxygen A and B are used in order to transform the chromophoric group in the lignin into non-color group.
  • ⁇ , ⁇ -aldehyde or ketone group are turned to the carboxylic acid or binary acid.
  • the pretreatment system of the raw materials This is a cooperation process. In this process, materials are removed legumen, calyces by crushing engine and cut into length of 5 cm and thick of 1.5 cm. Finally materials whose forming rate is 98% are obtained. Above materials are broken into plush by roller and crushing engine, removed dust and medulla by wind power, removed impurity by cleaner. Water of the cleaner is full closed and circular water Little active oxygen free radicals and little cellulose preserver (could be brought from market) are left in the water, so active oxygen needn't be added in the pretreatment process. No any drainage is drained in the process of washing materials by circular water, which changes the traditional process with acid washing and alkali washing.
  • Oxidation reactor system (refer to the application of patent for invention of China: 200310103895.3): The main function is imbibition, softening and debonding of the materials. Active oxygen in the subacidity water whose pH is 1 to 4 generates superoxide anion radicals (O 2 ⁇ .HOO.) who have strong penetrability and can penetrate intercellular space directly to occur oxidation reaction. Agitator is installed in the oxidation reactor and the agitator connects outer power plant through the top of the reactor.
  • the agitator at least has three-process propellers, and its rotating speed can be controlled. Start the agitator and then in the reactor, positive ions are produced in the water. Materials are softened by cooperation of positive ions, pressure, temperature and shearing stress of the agitator. In the oxidation reactor, catenating layer, pectin, poly pentose are decomposed at the same time, and decolor reactions are occurred by high speed agitating of active oxygen.
  • Grinding system the best choice is disk grinder system that is made of two parts, one is model RL5OS disc refiner or high consistency defibrator and the other is oxidation reactor.
  • the process has first refining and second refining. Active oxygen A is used in the first refining and active oxygen B is used in the second refining.
  • the raw materials exported by oxidation dipping system are fed to refiner by screw feeder continuously and equally, then the materials are dipped by O 3 whose concentration is 1-15 umol/L, weight percentage concentration of water 30%, and pH 2.5. Grinding rotating speed is 600-1200 r/s and the gap between the disks is 0.2-0.15 mm.
  • active oxygen A whose weight percentage concentration is 0.1-1.5 is added in the shower water to mix grind with materials.
  • the materials are softened with grinding, and then the cellulose cladded in the intercellular space is separated.
  • Main function of the grinding thermal reaction it producing heat transfer reaction with confriction of refiner by mix grinding of active oxygen and material.
  • Chromophore of hydrocinnamic alkyl is oxidized by superoxide anion free radicals, dioxygen and hydrogen peroxide.
  • With softening temperature difference of lignin, hemicellulose and cellulose, hydrophilic groups gotten from oxidized exiguous fibers can connect fundamental chain of cellulose, as a result, yield is augmented to 8-12%.
  • Key of the invention is condition of the process (the detail instruction of the process such as sequence, pH, temperature, dosage of active oxygen, time, rotating speed, pressure and pulp concentration).
  • the process has first refining and second refining.
  • slag grinding can be grinded and screened repeatedly after screening.
  • edible citric acid whose weight percentage concentration is 0.12 and hydroxylamine whose weight percentage concentration is 0.01 are added and sprinkled to prevent dandy worm and oxidative stain.
  • routine beating process the pulp is original material with yield 76% and ISO whiteness 52-65.
  • the process described above can be applied in the village and township enterprises in the area with abundant raw materials. And the coarse pulp products can be supplied sufficiently to the consolidation pulp mills.
  • the raw materials are fed to refiner continuously and equally.
  • O 2 weight percentage concentration is 0.1
  • H 2 O 2 weight percentage concentration is 1.5
  • O 3 concentration is 10 umol/L
  • O 2 superoxide anion radicals
  • method of the invention has advantages as follows: It is practically a process which involves a method with close-loop, self-cycling, non-acid, non-alkali, non-chlorine, non-anthraquinone, non-cooking, non-bleaching, non-draining and non-pollution.
  • the method has characters of saving energy, saving water and clean pulping and it solves pollution of papermaking completely, utilizes the resource of agriculture and forest, and protects the environment.
  • the fully closed, self-cycling, zero discharge refers to: All water in the process from the pretreatment of raw materials till the delivery of it to the oxidation reactor is divided into two parts to accomplish the self-cycling in the process.
  • FIG. 1 The flow sheet of this invention that is a fully closed, self-cycling, zero discharge and clean pulping process is illustrated in FIG. 1 .
  • impregnating softness number of the materials in the reactor is 98%.
  • the materials change from deep yellow to pale white and accord with ISO whiteness 48-52° (hereinafter it is called whiteness or ISO whiteness for short).
  • Above materials are washed repeatedly and dewatered to concentrate, and weight percentage concentration of the water is 30%.
  • H 2 O 2 solution is added in the material, and weight percentage concentration of H 2 O 2 in the material is 0.2.
  • the material is fed to refiner continuously and equally to be grinded.
  • the rotating speed of refiner disc is 600-1200 r/s and the gap between the disks is 0.2-0.15 mm. slag grinding can be grinded and screened repeatedly after screening.
  • H 2 O 2 weight percentage concentration is 1-5) prepared in advance are added to pulp in 1:0.12 (according to weight ratio) and mixed with pulp in refiner at 60° C., pH 3.8 and 12-15% consistency.
  • the rotating speed of refiner is 1300 r/s and the gap between the disks is 0.15-0.1 mm.
  • the pulp whiteness can be 60-750.
  • O 3 concentration is 10umol/L
  • the rotating speed of refiner disc is 1300 r/s and the gap is 0.1 mm.
  • the ISO whiteness can reach to 75-86°.
  • the pulp is sent into the conventional screening process for fine screening.
  • the refined pulp is sent into the centrifugal cleaning process before it is condensed with decker, beaten, and then sent into the storage process.
  • the pulp can be processed again according to the process described above and pulp yield is 75%.
  • superoxide anion radicals (O 2 ⁇ /HOO.) (concentration is 10 umol/L) is added and mixed with pulp at 80° C., pH 3.8, 12-15% pulp consistency and 0.4 Mpa.
  • the rotating speed of refiner disc is 1300 r/s and the gap is 0.1 mm.
  • the ISO whiteness can reach to 75-86°.
  • the pulp is sent into the conventional screening process for fine screening.
  • the refined pulp is sent into the centrifugal cleaning process before it is condensed with decker, beaten, and then sent into the storage process. When higher whiteness is required, the pulp can be processed again according to the process described above and pulp yield is 75%.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Paper (AREA)
US10/583,763 2003-12-25 2003-12-25 Fully Closed, Zero Discharge, Clean Oxidizing Pulping Technology and Process Abandoned US20070272377A1 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2003/001121 WO2005064076A1 (fr) 2003-12-25 2003-12-25 Procede de reduction en pate par oxydation en cycle ferme sans rejet

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US (1) US20070272377A1 (fr)
EP (1) EP1707668A1 (fr)
CN (1) CN100420789C (fr)
AU (1) AU2003292884A1 (fr)
WO (1) WO2005064076A1 (fr)
ZA (1) ZA200605196B (fr)

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US8778136B2 (en) 2009-05-28 2014-07-15 Gp Cellulose Gmbh Modified cellulose from chemical kraft fiber and methods of making and using the same
CN104153228A (zh) * 2014-07-31 2014-11-19 广西三威林产工业有限公司 木片水洗及输送装置
CN105483936A (zh) * 2016-01-26 2016-04-13 天津鸿胜嘉德科技有限公司 一种水刺无纺布的生产方法
US9511167B2 (en) 2009-05-28 2016-12-06 Gp Cellulose Gmbh Modified cellulose from chemical kraft fiber and methods of making and using the same
US9512237B2 (en) 2009-05-28 2016-12-06 Gp Cellulose Gmbh Method for inhibiting the growth of microbes with a modified cellulose fiber
US9512563B2 (en) 2009-05-28 2016-12-06 Gp Cellulose Gmbh Surface treated modified cellulose from chemical kraft fiber and methods of making and using same
US9617686B2 (en) 2012-04-18 2017-04-11 Gp Cellulose Gmbh Use of surfactant to treat pulp and improve the incorporation of kraft pulp into fiber for the production of viscose and other secondary fiber products
US9719208B2 (en) 2011-05-23 2017-08-01 Gp Cellulose Gmbh Low viscosity kraft fiber having reduced yellowing properties and methods of making and using the same
US9951470B2 (en) 2013-03-15 2018-04-24 Gp Cellulose Gmbh Low viscosity kraft fiber having an enhanced carboxyl content and methods of making and using the same
US10000890B2 (en) 2012-01-12 2018-06-19 Gp Cellulose Gmbh Low viscosity kraft fiber having reduced yellowing properties and methods of making and using the same
US10138598B2 (en) 2013-03-14 2018-11-27 Gp Cellulose Gmbh Method of making a highly functional, low viscosity kraft fiber using an acidic bleaching sequence and a fiber made by the process
US10151064B2 (en) 2013-02-08 2018-12-11 Gp Cellulose Gmbh Softwood kraft fiber having an improved α-cellulose content and its use in the production of chemical cellulose products
US10865519B2 (en) 2016-11-16 2020-12-15 Gp Cellulose Gmbh Modified cellulose from chemical fiber and methods of making and using the same
CN114808519A (zh) * 2022-04-22 2022-07-29 山东大汶河农业发展集团有限公司 一种姜秸秆高值化利用的方法

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US20090090478A1 (en) * 2007-10-05 2009-04-09 Hollomon Martha G Selectivity improvement in oxygen delignification and bleaching of lignocellulose pulp using singlet oxygen
KR102421357B1 (ko) * 2013-12-19 2022-07-18 쓰리엠 이노베이티브 프로퍼티즈 컴파니 재순환된 폐수를 사용하여 오염 제어 장치에 또는 방화재에 사용하기에 적합한 부직 섬유질 재료를 제조하는 방법
CN108547079B (zh) * 2018-06-08 2023-10-10 北京鹏盛天纤科技有限公司 一种脱脂棉绿色连续式生产集成装置和工艺
CN110295507A (zh) * 2019-06-06 2019-10-01 安徽盛林环保科技有限公司 秸秆提取纤维工艺

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US10731293B2 (en) 2009-05-28 2020-08-04 Gp Cellulose Gmbh Modified cellulose from chemical kraft fiber and methods of making and using the same
US9777432B2 (en) 2009-05-28 2017-10-03 Gp Cellulose Gmbh Modified cellulose from chemical kraft fiber and methods of making and using the same
US11111628B2 (en) 2009-05-28 2021-09-07 Gp Cellulose Gmbh Modified cellulose from chemical kraft fiber and methods of making and using the same
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US9512561B2 (en) 2009-05-28 2016-12-06 Gp Cellulose Gmbh Modified cellulose from chemical kraft fiber and methods of making and using the same
US9511167B2 (en) 2009-05-28 2016-12-06 Gp Cellulose Gmbh Modified cellulose from chemical kraft fiber and methods of making and using the same
USRE49570E1 (en) 2009-05-28 2023-07-04 Gp Cellulose Gmbh Modified cellulose from chemical kraft fiber and methods of making and using the same
US9970158B2 (en) 2009-05-28 2018-05-15 Gp Cellulose Gmbh Modified cellulose from chemical kraft fiber and methods of making and using the same
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US9512563B2 (en) 2009-05-28 2016-12-06 Gp Cellulose Gmbh Surface treated modified cellulose from chemical kraft fiber and methods of making and using same
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US8778136B2 (en) 2009-05-28 2014-07-15 Gp Cellulose Gmbh Modified cellulose from chemical kraft fiber and methods of making and using the same
US9719208B2 (en) 2011-05-23 2017-08-01 Gp Cellulose Gmbh Low viscosity kraft fiber having reduced yellowing properties and methods of making and using the same
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US10597819B2 (en) 2012-01-12 2020-03-24 Gp Cellulose Gmbh Low viscosity kraft fiber having reduced yellowing properties and methods of making and using the same
US10995453B2 (en) 2012-01-12 2021-05-04 Gp Cellulose Gmbh Low viscosity kraft fiber having reduced yellowing properties and methods of making and using the same
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CN100420789C (zh) 2008-09-24
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AU2003292884A1 (en) 2005-07-21
WO2005064076A1 (fr) 2005-07-14

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