WO2018006093A1 - Compositions d'anthraquinone et leurs préparations - Google Patents

Compositions d'anthraquinone et leurs préparations Download PDF

Info

Publication number
WO2018006093A1
WO2018006093A1 PCT/US2017/040606 US2017040606W WO2018006093A1 WO 2018006093 A1 WO2018006093 A1 WO 2018006093A1 US 2017040606 W US2017040606 W US 2017040606W WO 2018006093 A1 WO2018006093 A1 WO 2018006093A1
Authority
WO
WIPO (PCT)
Prior art keywords
composition according
microns
composition
water
water soluble
Prior art date
Application number
PCT/US2017/040606
Other languages
English (en)
Inventor
Timothy Walter ABRAHAM
John M. Zupfer
Original Assignee
Cargill, Incorporated
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 Cargill, Incorporated filed Critical Cargill, Incorporated
Publication of WO2018006093A1 publication Critical patent/WO2018006093A1/fr

Links

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
    • D21C3/222—Use of compounds accelerating the pulping processes

Definitions

  • Anthraquinone is a solid that is insoluble in water.
  • a further need is to use a larger mean particle size of AQ in the AQ compositions compared to current particle sizes for ease of handling and safety.
  • Wood and other plant materials used to make pulp generally contain three main components (apart from water): cellulose fibers (desired for papermaking), lignin (a three-dimensional polymer that binds the cellulose fibers together) and hemicelluloses (shorter branched carbohydrate polymers).
  • Fiber sources include wood fibers, e.g., soft woods and hard woods and mixtures thereof, and non-wood fibers obtained from agricultural productions, such as without limitation, bagasse, wheat straw, rice straw, corn stover (stalks, leaves and husks), soy residuals, coconut tissues, cotton stalks, palm baskets, kenaf, industrial hemp, seed flax straw, textile flax straw, sisal, hesperaloe, rye grass, and mixtures thereof.
  • agricultural productions such as without limitation, bagasse, wheat straw, rice straw, corn stover (stalks, leaves and husks), soy residuals, coconut tissues, cotton stalks, palm baskets, kenaf, industrial hemp, seed flax straw, textile flax straw, sisal, hesperaloe, rye grass, and mixtures thereof.
  • Figure 1 is a block flow diagram showing the preparation of an AQ composition according to an aspect of the disclosure.
  • Figure 2 is a visual showing the stability over 1 week of four AQ compositions prepared according to an aspect of the disclosure.
  • Figure 3 is a visual showing the stability over 1 week of AQ compositions prepared according to an aspect of the disclosure.
  • One aspect of the present disclosure relates to an AQ composition
  • an AQ composition comprising
  • the AQ composition having a mean particle size from about 0.1 micron to about 200 microns, a water soluble or water dispersible polysaccharide, and water, wherein the AQ composition is a substantially homogeneous and stable suspension at room temperature in a closed container from about 24 hours to about 1 year. Further, the AQ composition is also pumpable at temperatures from about 10 to 80°C or about 15 to 70°C, such as, for example, about 20 to 60°C, about 22 to 50 °C, about 23 to 40°C, about 25 to 30°C. Further, the AQ composition can optionally comprise one or more metal ions and additive(s).
  • an AQ composition comprising AQ having a mean particle size from about 0.1 micron to about 200 microns, a water soluble or water dispersible polysaccharide, one or more metal ions, preferably water soluble, such as calcium salts and magnesium salts, and water, wherein the composition is a substantially homogeneous and stable suspension at room temperature in a closed container from about 24 hours to about 1 year.
  • the AQ composition is also pumpable at temperatures from about 10 to 80°C or about 15 to 70°C, such as, for example, about 20 to 60°C, about 22 to 50 °C, about 23 to 40°C, about 25 to 30°C.
  • the AQ composition can optionally comprise an additive(s).
  • Yet another aspect of the disclosure is the use of the AQ composition in pulping processes.
  • Another aspect of the disclosure is paper products made from the pulping process using the AQ compositions disclosed herein.
  • the term "substantially homogeneous and stable” means the AQ in the “substantially homogeneous and stable” suspension is dispersed evenly and the AQ does not settle during extended storage for at least 24 hours to one year, even at tropical-like temperatures (i.e., at least 30°C).
  • the settling of AQ in the suspension is determined visually by tilting the container containing the composition and observing its flow properties and looking for settling of AQ at the bottom of the container.
  • a suspension is "pumpable” when it can be pumped using any pumps used for pumping liquids, such as positive displacement pumps, centrifugal pumps, diaphragm pumps, gear pumps, peristaltic pumps, piston pumps, and syringe pumps.
  • pumps used for pumping liquids such as positive displacement pumps, centrifugal pumps, diaphragm pumps, gear pumps, peristaltic pumps, piston pumps, and syringe pumps.
  • the term "about” means a range of ⁇ 10%, ⁇ 5% or ⁇ 1%.
  • polysaccharides refers to polymeric carbohydrate molecules composed of long chains of monosaccharide units bound together by glycosidic linkages and on hydrolysis give the constituent monosaccharides or oligosaccharides.
  • Polysaccharides range in structure from linear to highly-branched. Examples include storage polysaccharides such as starch and glycogen, and structural polysaccharides such as cellulose, hemicellulose, and chitin. Depending on the molecular weight and structure, polysaccharides can dissolve completely in water (i.e., water soluble) giving a clear solution, or be dispersed as a powder (i.e., dry fine particles) in water (i.e., water dispersible or not necessarily completely dissolved in water). Typically, water-dispersible polysaccharides require agitation to keep them suspended in water in the absence of other compounds, such as dispersants, that promote suspension.
  • storage polysaccharides such as starch and glycogen
  • structural polysaccharides such as cellulose, hemicellulose, and chitin.
  • polysaccharides can dissolve completely in water (i.e., water soluble) giving a clear solution, or be dispersed as a powder (i.e.,
  • the concentration of the polysaccharides in the AQ composition is from about 0.001% to about 10%, from about 0.01% to about 5%, or from about 0.1% to about 1%.
  • the mean particle size of AQ in the AQ composition is about 200 microns, 150 microns or less, about 135 microns or less, about 125 microns or less, about 100 microns or less, about 75 microns or less, about 50 microns or less, about 25 microns or less, about 20 microns or less, about 15 microns or less, about 10 microns or less, about 8 microns or less, about 5 microns or less, about 3 microns or less, about 1 micron or less, about 100 microns to about 1 micron, about 75 microns to about 2 microns, about 50 microns to about 3 microns, about 25 microns to about 4 microns, about 20 microns to about 5 microns, about 10 microns to 6 microns.
  • the AQ composition can include a concentration of AQ of at least about 40 wt % or at least about 50 wt %.
  • the AQ concentration can range from about 40 wt % to about 70 wt %, from about 40 wt % to about 60 wt %, from about 40 wt % to about 50 wt %, from about 45 wt % to about 55 wt %, from about 50 wt % to about 70 wt %, from about 50 wt % to about 65 wt %, 50 wt % to about 60 wt %, and from about 50 wt % to about 55 wt %.
  • the AQ concentration is about 40 wt %. In another aspect, it is about 50 wt %.
  • Metal ions and dispersants may be used in the AQ composition. If used, the metal ions and the dispersants are water soluble.
  • the one or more metal ions may be monovalent, divalent, trivalent, tetravalent, their salts thereof, and mixtures thereof.
  • the divalent metal ion salts include, without limitation, calcium salt(s) and magnesium salt(s), and they may be any water soluble salt, e.g. chlorides, bromides, nitrates.
  • the concentration of the one or more metal ions is from about 0.01 wt % to about 1 wt %. In one aspect, the total weight of the metal ion salts is about 1.2%. In another aspect, the molar ratio of calcium to magnesium in the AQ composition is about 1:1, about 1.1:0.9, or about 0.9:1.1.
  • the dispersant may be a cationic dispersant, an anionic dispersant, or a nonionic dispersant.
  • the anionic dispersant is, for example and without limitation, an aromatic sulfonate, such as a naphathalene sulfonate, and preferably a dialkylnaphthalene sulfonate dispersant.
  • dialkylnaphathalene sulfonate include, without limitation, sodium salts of dialkylnaphthalene sulfonic acid.
  • the dispersant is sodium diisopropylnaphthalene sulfonate, for example Naxan® DIL dispersant, purchased from the Nease Corporation.
  • the concentration of the dispersant in the AQ composition is from about 0.01% to about 5%, from about 0.05% to about 3% or from about 0.1 to about 2%.
  • the molar ratio of AQ to the total calcium in the AQ is the molar ratio of AQ to the total calcium in the AQ
  • composition is about 50:1, about 51:1 to about 49:1, or about 55:1 to about 45:1.
  • the AQ composition comprising from about 40 wt % to about 50 wt % AQ as disclosed herein has an initial viscosity at 25 °C from about 500 cP to about 50,000 cP, from about 1,000 cP to about 40,000 cP, from about 2,000 cP to about 35,000 cP, from about 2,400 cP to about 31,000 cP, and from about 2,400 cP to about 25,000 cP.
  • the initial viscosity is from about 3,000 cP to about 25,000 cP, and from 3,200 cP to about 19,000 cP.
  • the AQ composition as disclosed herein remains stable at room temperature in a closed container for at least about 24 hours, at least about 1 week, at least about 1 month, at least about 3 months, or at least about 6 months. In some aspects, the AQ composition is stable up to about a year.
  • an AQ composition comprising AQ having a mean particle size of about 200 microns or less, a polysaccharide, one or more metal ions, a dispersant, and water.
  • One aspect is a composition comprising AQ having a mean particle size of about 150 microns or less, a polysaccharide, one or more calcium salts, one or more magnesium salts, a salt of diisopropylnaphthalene sulfonate, and water.
  • the mean particle size of AQ in the AQ composition is about 200 microns or less, about 135 microns or less, about 125 microns or less, about 100 microns or less, about 75 microns or less, about 50 microns or less, about 25 microns or less, about 20 microns or less, about 15 microns or less, about 10 microns or less, 200 microns to about 1 micron, about 100 microns to about 1 micron, about 50 microns to about 1 micron, about 25 microns to about 1 micron, about 20 microns to about 1 micron, about 15 microns to about 1 micron, about 10 microns to about 1 micron, about 8 microns to about 1 micron, about 5 microns to about 1 micron, and about 3 microns to about 1 micron.
  • AQ is added slowly in small portions with agitation to enable rapid dispersion of AQ in the first solution.
  • Yet another aspect of the disclosure relates to a method for preparing the AQ composition as disclosed herein, comprising:
  • AQ composition i.e., a substantially homogenous and stable suspension of the AQ composition.
  • AQ mean particle size from 0.1 micron to 200 microns
  • agitation at a speed such that the first solution forms a substantially homogeneous and stable suspension to obtain a second solution of the AQ composition (i.e., a substantially homogenous and stable suspension of the AQ composition).
  • a second solution of the AQ composition i.e., a substantially homogenous and stable suspension of the AQ composition.
  • the metal ion salts e.g., calcium and magnesium salts
  • the dispersant e.g., a salt of diisopropylnaphthalene sulfonate
  • the metal ion salts, and the dispersant may be provided as individual solutions and then mixed together to provide the first solution. This be done prior to, or after, adding the polysaccharide.
  • the AQ composition is prepared according to the flow chart shown in Figure 1, comprising the following steps:
  • step b adding polysaccharide (e.g., scleroglucan, xanthan gum, methylcellulose, guar gum) into the water, and stirring until the polysaccharide dissolves or is dispersed well; c. optionally, adding metal ion salt(s) into the polysaccharide solution prepared in step b., and stirring until all salt(s) dissolve, wherein the metal ion salt(s) may be added together or separately;
  • polysaccharide e.g., scleroglucan, xanthan gum, methylcellulose, guar gum
  • a dispersant e.g., a dialkylnaphathalene sulfonate, such as sodium diisopropylnaphthalene sulfonate
  • a dispersant e.g., a dialkylnaphathalene sulfonate, such as sodium diisopropylnaphthalene sulfonate
  • additives e.g., a viscosifier, an emulsifier, a surfactant, an inert material
  • adding other additives e.g., a viscosifier, an emulsifier, a surfactant, an inert material
  • additives e.g., a viscosifier, an emulsifier, a surfactant, an inert material
  • step (f ) adding AQ having mean particle size from 0.1 micron to 200 microns into the solution prepared in step (e) slowly and in small portions with agitation to provide a substantially homogeneous AQ composition; and g. optionally, adding a dye or colorant into the substantially homogeneous AQ composition of step f. to provide a substantially homogeneous AQ composition with dye or colorant.
  • steps b., c, d., e., and g. can be added to the water in any order, and preferably AQ is added in the final step to avoid the formation of clumps.
  • Other compounds that can be used in a pulping process can also be added to the substantially homogeneous AQ composition.
  • AQ xanthan gum, guar gum, scleroglucan, methylcellulose, NAXAN-DIL dispersant and CaC and MgCk.ethO were purchased from commercially available sources.
  • a beaker containing the desired amount of water was placed beneath a table top mixer (Model IKA RW20DZM). Any table top mixer that enables the dispersion of AQ may be used.
  • the water-soluble or water-dispersible polysaccharide was added to the water and stirred for about 15 minutes at an appropriate speed until all of the polysaccharide completely dissolved or dispersed uniformly. Clumps of undispersed polysaccharide were avoided. If clumps formed, the solution was agitated longer.
  • the AQ powder was then added in small portions with agitation to provide a dispersed suspension, and stirred for another 10 to 15 minutes at an appropriate speed to ensure the AQ was well-dispersed.
  • the dispersion obtained was visually homogeneous.
  • Table 1 AO Composition Formulation with Scleroglucan (wt %)
  • the concentration of the AQ in Table 1 through Table 4 varied from either 40 wt % or 50 wt % (i.e., a range of from about 40 wt % to about 50 wt %) and the
  • polysaccharide ranging from 0.1 wt % to about 0.25 wt %.
  • metal ion salts were used for a total weight of 1.2%.
  • AQ with a mean particle size of 10 microns was used in all the AQ composition formulations except in the xanthan gum formulation 5X for which AQ of particle size 3 microns was used.
  • the calcium chloride and magnesium chloride used in the formulation can be anhydrous or hydrates.
  • the amount of water used in the formulation is adjusted accordingly.
  • Phase separation was observed by pouring formulations, as soon as they were prepared, into glass vials and observing them visually over several days.
  • Figures 2 and 3 are visuals showing such phase separation or lack of phase separation.
  • the formulations prepared with scleroglucan and methylcellulose exhibited syneresis after 7 days.
  • the xanthan gum formulation 5X also exhibited syneresis after 7 days.
  • Tables 1-4 The AQ composition formulations in Tables 1-4 were prepared and placed in an oven at 50°C. Two additional AQ composition formulations were prepared as controls, one containing only water and AQ, and the other water, AQ and Mg/Ca salts. Table 6 shows the stability and pourability of the samples that were observed after 1 week.

Landscapes

  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Des suspensions sensiblement homogènes et stables de compositions d'anthraquinone (AQ) et des procédés de préparation sont décrits. Les compositions d'AQ sont utilisées dans des procédés de mise en pâte.
PCT/US2017/040606 2016-07-01 2017-07-03 Compositions d'anthraquinone et leurs préparations WO2018006093A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201662357671P 2016-07-01 2016-07-01
US62/357,671 2016-07-01

Publications (1)

Publication Number Publication Date
WO2018006093A1 true WO2018006093A1 (fr) 2018-01-04

Family

ID=60787447

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US2017/040606 WO2018006093A1 (fr) 2016-07-01 2017-07-03 Compositions d'anthraquinone et leurs préparations

Country Status (1)

Country Link
WO (1) WO2018006093A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112080957A (zh) * 2020-09-18 2020-12-15 广东鼎丰纸业有限公司 烧碱蒽醌高效蒸煮助剂及其制备方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1196156A (fr) * 1982-06-02 1985-11-05 Michael S. Steltenkamp Methode de production de la pate de papier, et agent servant a cette fin
US5306392A (en) * 1990-09-14 1994-04-26 Akio Mita Process for preparing pulp using potassium-based alkaline solution
US20080168608A1 (en) * 2005-02-28 2008-07-17 Gregory Plos Dyeing of in Particular Human Keratin Materials by Dry Thermal Transfer of a Direct Anthraquinone Dye, Composition Comprising the Said Dye and Its Method of Preparation
WO2015116564A1 (fr) * 2014-01-31 2015-08-06 Cargill, Incorporated Procede et composition pour reduire l'entartrage d'un evaporateur utilisant de la silice

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1196156A (fr) * 1982-06-02 1985-11-05 Michael S. Steltenkamp Methode de production de la pate de papier, et agent servant a cette fin
US5306392A (en) * 1990-09-14 1994-04-26 Akio Mita Process for preparing pulp using potassium-based alkaline solution
US20080168608A1 (en) * 2005-02-28 2008-07-17 Gregory Plos Dyeing of in Particular Human Keratin Materials by Dry Thermal Transfer of a Direct Anthraquinone Dye, Composition Comprising the Said Dye and Its Method of Preparation
WO2015116564A1 (fr) * 2014-01-31 2015-08-06 Cargill, Incorporated Procede et composition pour reduire l'entartrage d'un evaporateur utilisant de la silice

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112080957A (zh) * 2020-09-18 2020-12-15 广东鼎丰纸业有限公司 烧碱蒽醌高效蒸煮助剂及其制备方法

Similar Documents

Publication Publication Date Title
US6967027B1 (en) Microfibrillated and/or microcrystalline dispersion, in particular of cellulose, in an organic solvent
EP0322736B1 (fr) Dispersion de polymère soluble dans l'eau
EP1135438B1 (fr) Polymeres dispersables hydrosolubles
US4772646A (en) Concentrated hydrophilic polymer suspensions
PT912633E (pt) Aditivacao de nanofibrilas de celulose com celulose carboxilada com baixo grau de substituicao
DE69432701T2 (de) Flüssige Suspension von cellulose-haltigen Polysacchariden für Pflegemittel und für Haushaltsreinigungsmittel
JP2905236B2 (ja) カルボキシメチルセルロース水性懸濁液の製造法
JPS63270786A (ja) フラクチャリング流体スラリー濃厚物および使用法
JPH04227761A (ja) 水溶性ポリマー懸濁液
CA1058050A (fr) Procede pour la formation de suspensions d'alignates solubles et produits obtenus
DE69023573T2 (de) Wässerige Hydroxyethylcellulose-Suspension.
EP0039128B1 (fr) Polymères hydrosolubles en suspension
US11059964B2 (en) Starch suspension for adhesive coatings
WO2018006093A1 (fr) Compositions d'anthraquinone et leurs préparations
EP0153206B1 (fr) Suspensions aqueuses de particules solides
DE69304986T2 (de) Fluide Polyvinylalkoholsuspensionen
US6465553B2 (en) Gum slurries
US5246490A (en) Water soluble liquid alginate dispersions
CN102007148A (zh) 含果聚糖微粒的水分散液，制备方法及其应用
JP3703845B2 (ja) 溶液の形成方法
CN113461968A (zh) 一种羧甲基壳聚糖稳定的高内相乳液及其制备方法
JP7489656B2 (ja) バクテリアセルロース複合化粉末およびその製造方法
Martins et al. Effect of bacterial cellulose on the foaming properties of egg white and soy proteins
CN116370359A (zh) 一种稳定性好的洗护、护肤产品用液晶悬浮剂
JPH01289899A (ja) 水性ゼオライトスラリー組成物

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 17821443

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 17821443

Country of ref document: EP

Kind code of ref document: A1