[go: up one dir, main page]

EP1058713A1 - Compositions colloidales a base de lignine - Google Patents

Compositions colloidales a base de lignine

Info

Publication number
EP1058713A1
EP1058713A1 EP99906000A EP99906000A EP1058713A1 EP 1058713 A1 EP1058713 A1 EP 1058713A1 EP 99906000 A EP99906000 A EP 99906000A EP 99906000 A EP99906000 A EP 99906000A EP 1058713 A1 EP1058713 A1 EP 1058713A1
Authority
EP
European Patent Office
Prior art keywords
bitumen
lignin
spent
pulping liquor
colloidal dispersion
Prior art date
Legal status (The legal status 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 status listed.)
Withdrawn
Application number
EP99906000A
Other languages
German (de)
English (en)
Inventor
Zhi-Zhong Liang
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Polyphalt Inc
Original Assignee
Polyphalt Inc
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 Polyphalt Inc filed Critical Polyphalt Inc
Publication of EP1058713A1 publication Critical patent/EP1058713A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L97/00—Compositions of lignin-containing materials
    • C08L97/005—Lignin
    • 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
    • D21C11/0007—Recovery of by-products, i.e. compounds other than those necessary for pulping, for multiple uses or not otherwise provided for

Definitions

  • the present invention relates to the processing of black liquor and the preparation of bitumen compositions containing black liquor.
  • Black liquor is an aqueous alkaline pulping residue produced in Kraft pulping of wood chips in a pulp mill to provide wood fibers for paper-making.
  • Black liquor generally contains about 55 to 65% solids comprising lignin, sodium salts of poly-saccharinic acids, organic and inorganic sulfides and carbonates and many other compounds.
  • the lignin in the black liquor is the main organic component and is present as a high mass colloid stabilized by ionized phenolic groups.
  • Lignin is a phenylpropane polymer of amorphous structure comprising about 17 to about 30% of wood.
  • Lignin is so closely associated with the cellulosic fibres and hemi-cellulose that makes up the balance of woody material that lignin can be separated from wood only by chemical reaction at high temperature, such as that used in the Kraft pulping process, wherein wood chips are digested with an aqueous alkaline solution of sodium hydroxide and hydrogen sulfide, known as white liquor. Normally, the black liquor, after separation of the wood fibers, is processed to remove organic materials and to recover and regenerate pulping chemicals. Lignin can be recovered from wood-processing wastes only in limited quantities.
  • the lignin is a natural binder derivative of wood. Alkali lignin from both softwoods and hardwoods are useful in many products.
  • Alkali lignin can also be used as adhesives for plywood, molding powers and formed insulating resins and as a reinforcing agent for rubber.
  • Asphalt binders are widely used in different applications, such as asphalt-aggregate blends for road paving, asphalt fiber reinforced membranes for roofing and asphalt-water emulsions in surface treating both for paving and roofing. Problems for straight-run asphalt in those applications are the tendency to become brittle at low temperatures and to become soft at high temperatures, the tendency to flow under constant load at service temperatures and the tendency to phase separation during storage when mixed with other components .
  • the present invention relates to compositions and methods for combining black liquor with selected petroleum-derived products. More specifically, this invention provides two separate processes for preparing lignin-based colloidal dispersions in lubricating or other petroleum-based oils.
  • the lignin-oil colloidal dispersions prepared by either of such processes may be blended with bitumen to produce novel bituminous composition. Two embodiments of such procedures are described herein.
  • the black liquor used in the invention may be that resulting from cooking wood in an alkaline solution in the soda or sulfate (Kraft) paper-making process.
  • the asphalt employed in this invention can be any of the well known bituminous substances derived from petroleum, shale oil, coal tar and the like.
  • the asphalt is prepared by vacuum distillation of a topped crude oil.
  • the asphalt has a penetration at 25°C (as determined by ASTM D5) ranging for about 20 to about 400.
  • the procedure involves essentially two steps.
  • the black liquor is converted from its aqueous colloidal system to an anhydrous colloidal dispersion in a lubricating oil medium in which a surfactant, which may be an anionic surfactant, such as DDBSA (dodecylbenzene sulfuric acid) , is used to promote the provision of the anhydrous colloidal dispersion.
  • a surfactant which may be an anionic surfactant, such as DDBSA (dodecylbenzene sulfuric acid)
  • DDBSA dodecylbenzene sulfuric acid
  • the anhydrous colloidal dispersion of lignin in oil may be mixed, in a second step, with asphalt bitumen, producing a unique combination, which is a novel bituminous composition.
  • bitumen is treated with an inorganic acid, such as sulfuric acid, at elevated temperature to provide an acid-treated bitumen.
  • the black alkaline liquor is then added slowly to the acid-treated bitumen under agitation for de-watering the black liquor at a controlled rate to form a stable, substantially anhydrous, colloidal dispersion of lignin in the bitumen, also to provide a novel bituminous composition.
  • a lubricating oil is mixed with black liquor at temperatures below the water boiling point.
  • a surfactant which may be DDBSA (dodecylbenzene sulfuric acid)
  • DDBSA dodecylbenzene sulfuric acid
  • the lubricating oil used in the first embodiment of the invention may be a re-refined waste motor oil or other convenient petroleum-based oil. Contaminants of waste motor oil, such as dirt, lead, arsenic and other harmful metals and chemicals, are removed from the waste motor oil to produce a clean base lubricating oil by the re-refining process.
  • the lubricating oil may be a selected fraction of refined mineral oil used for lubrication of moving surfaces. Such fraction may range in consistency from thin liquid to grease-like substances. Usually, lubricating oils contain small amounts of additives to impart special properties, such as viscosity index and detergency.
  • the surfactant or dispersing agent used in the process may typically be dodecylbenzene sulfuric acid (DDBSA) , although other anionic surfactants may be employed, if desired, such as fatty acid, linear alkyl sulfonates having 10 or more carbon atoms in the chain.
  • DDBSA is benzene with dodecene, and the resulting dodecylbenzene is sulfonated.
  • DDBSA may be neutralized with caustic soda from the alkaline black liquor or other convenient source to promote the detergency of the lubricating oil and to reduce surface tension in the mixture .
  • a surfactant need not always be necessary, if the lubricating oil employed has a detergency high enough to ensure that a colloidal dispersion of the solid residue from the black liquor is achieved in the lubricating oil medium.
  • the lignin-oil dispersion produced by either of these procedures may be smoothly blended with bitumen to provide the desired lignin-asphalt composition.
  • bitumen first is treated with a strong mineral acid, such as sulfuric acid, at elevated temperature and then the alkaline black liquor is added to the treated bitumen at a controlled rate under agitation to effect de-watering of the black liquor to form a stable, substantially anhydrous, colloidal dispersion in the bitumen.
  • a strong mineral acid such as sulfuric acid
  • An inorganic acid is contacted with, or added to, the asphalt to form an acid treated asphalt.
  • the acid addition shifts the asphalt structure from a sol to a gel, lowers the temperature susceptibility of the asphalt and improves the stability of the additive dispersion in the treated asphalt.
  • black liquor is an aqueous alkaline system, it is critical that the acid not be added to the asphalt after addition of or with the black liquor.
  • the acid is added slowly to the asphalt to avoid foaming, which may occur if all the acid were added at one time.
  • the inorganic acid content of the asphalt resulting from the acid treatment is not critical, but normally is in the range between about 0.2 and about 3.5 wt%, preferably between about 0.5 and about 2.5 wt% of the asphalt.
  • the inorganic acid is preferably selected from the group consisting of sulfuric acid, phosphoric acid, poly-phosphoric acid, phosphorous pentoxide, hydrochloric acid, and mixtures thereof.
  • the sulfuric acid, phosphoric acid or poly-phosphoric acid are preferred inorganic acids, with the sulfuric acid being particularly preferred.
  • the alkaline black liquor is then added slowly to the acid-treated bitumen at an elevated temperature, typically around 100°C, under agitation for a certain period of time to permit dewatering of the black liquor to occur while the solids are incorporated into the bitumen.
  • the temperature of the final composition next is increased above the boiling point of water, typically up to around 160°C until residual water is completely evaporated off to 7
  • Example 1 This Example illustrates the first embodiment of the invention in which black liquor first dispersed in a lubricating oil and then in bitumen.
  • Mass of analyzed sample of reclaimed lube oil was determined following the test method of ASTM 4124-92.
  • Base asphalt (or bitumen) used in the present invention were selected from three different degrades: AC-5 having an absolute viscosity of around 500 poises, 185/100 having a 25°C penetration range from 85 dmm to 100 dmm and 1120/150 having a 25°C penetration range from 120 dmm to 150 dmm.
  • the non-aqueous dispersing system of black liquor/lube-oil produced as described in the Table 1 was dispersed into hot liquid asphalt at about 160°C respectively to form a very fine dispersion mixture.
  • the stability of these lignin based bituminous mixtures during hot storage at elevated temperature was evaluated using a conditioned tube test.
  • the conditioning procedure consists of placing approximately 70g of the mixture in H" aluminum tubes and storing such tubes in a vertical position at 165°C in an oven for 48 hrs. Following hot storage, a viscosity ratio was determined by comparing the viscosity of the mixture tested at 135°C from the bottom section of the sample and from the top section of the sample in the tube. A ratio in the range of 0.80 to 1.20 is generally considered acceptable with respect to separation of the dispersed phase.
  • the testing results on eight compositions are shown in the following Table 2. The results indicate that the lignin based solid dispersion in asphalt binder are quite stable.
  • This Example illustrates the second embodiment of the invention in which bitumen first is acidified.
  • Sulfuric acid 95 to 98% H 2 S0 4
  • results of dispersion and stability determinations are also shown below in the following Table 3.
  • the results shown in Table 3 indicate that products of formulation containing 0.8 wt% acid and 0 to 30 wt%, preferably 15 to 25 wt% black liquor, based on the amount of asphalt, had good stability.
  • the present invention provides novel procedures for the stable dispersion of lignin components of black liquor in bitumen. Modifications are possible within the scope of the invention.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Civil Engineering (AREA)
  • Structural Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Cette invention se rapporte à une dispersion colloïdale à base de lignine destinée à être incorporée dans une huile lubrifiante ou du bitume, qui est préparée à partir d'un résidu de liqueur noire. Dans un procédé faisant l'objet de cette invention, une première étape consiste à convertir la liqueur noire pour la faire passer de son système colloïdal aqueux à une dispersion colloïdale anhydre dans un milieu à base d'huile lubrifiante ré-affinée, dans lequel un tensioactif, tel que du DDBSA (acide sulfurique dodécylbenzène), est utilisé pour favoriser la dispersion colloïdale. Dans une seconde étape, du bitume est mélangé au produit obtenu dans la première étape. Dans un autre procédé faisant l'objet de cette invention, du bitume est d'abord traité avec un acide inorganique, tel que de l'acide sulfurique, à température élevée. La liqueur noire alcaline est ensuite ajoutée lentement au bitume traité à l'acide, avec agitation, en vue d'obtenir un déshydratation à une vitesse régulée, afin de former une dispersion colloïdale stable sensiblement anhydre dans le bitume.
EP99906000A 1998-02-23 1999-02-22 Compositions colloidales a base de lignine Withdrawn EP1058713A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US7554698P 1998-02-23 1998-02-23
US75546P 1998-02-23
PCT/CA1999/000155 WO1999042526A1 (fr) 1998-02-23 1999-02-22 Compositions colloidales a base de lignine

Publications (1)

Publication Number Publication Date
EP1058713A1 true EP1058713A1 (fr) 2000-12-13

Family

ID=22126470

Family Applications (1)

Application Number Title Priority Date Filing Date
EP99906000A Withdrawn EP1058713A1 (fr) 1998-02-23 1999-02-22 Compositions colloidales a base de lignine

Country Status (4)

Country Link
EP (1) EP1058713A1 (fr)
AU (1) AU2606299A (fr)
CA (1) CA2321735A1 (fr)
WO (1) WO1999042526A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2021502461A (ja) * 2017-11-13 2021-01-28 シュティッヒティング・ヴァーヘニンゲン・リサーチ リグニンベースのバイオアスファルト
EP4008752A1 (fr) * 2020-12-03 2022-06-08 Peab Asfalt AB Procédé de production d'un mélange d'asphalte contenant d'une lignine et une composition d'asphalte produits par ce produit
CN113527778B (zh) * 2021-08-09 2022-12-02 南京工业大学 一种纳米木质素胶乳的制备方法与应用
SE2330210A1 (en) * 2023-05-10 2024-11-11 Stora Enso Oyj Process for producing a binder for a warm mix asphalt composition

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3956002A (en) * 1974-03-18 1976-05-11 Westvaco Corporation Anionic bituminous emulsions
US4293459A (en) * 1979-06-07 1981-10-06 American Can Company Asphalt emulsion-conditioner

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9942526A1 *

Also Published As

Publication number Publication date
CA2321735A1 (fr) 1999-08-26
AU2606299A (en) 1999-09-06
WO1999042526A1 (fr) 1999-08-26

Similar Documents

Publication Publication Date Title
US4293459A (en) Asphalt emulsion-conditioner
AU622136B2 (en) Multigrade asphalt cement product and process
US5911817A (en) Process for paving with asphalt containing mineral lubricating oil base stock
US5476542A (en) Asphalt compositions with improved cross-linking agent
EP3116953B1 (fr) Composition de bitume
CA2355408C (fr) Compose d'asphalte modifie a entreposage stable, et procede de preparation
US5496400A (en) Asphalt compositions with improved cross-linking agent
US6310122B1 (en) Stable bitumen polymer compositions
US5656733A (en) Lignin-containing resinous compositions
EP1740676A2 (fr) Mastic d'asphalte a base de dechets solides de raffinage de petrole
US6737443B1 (en) Lignin based colloidal compositions
de Lima Neto et al. The effects of Kraft lignin on physical, rheological and anti-ageing properties of asphalt binders
EP1058713A1 (fr) Compositions colloidales a base de lignine
JPH0244360B2 (fr)
CN1024421C (zh) 沥青乳液
CN100487057C (zh) 热储存稳定的胶粉-沥青组合物及其制备方法
Gopalakrishnan et al. Lignin recovery and utilization
DE69618648T2 (de) Strassenbelagbindemittel und verfahren zur herstellung
KR19980072997A (ko) 폐아스콘 재생용 첨가제 및 폐아스콘의 재포장방법
CA1306836C (fr) Liant bitumineux pour revetement routier
US4571269A (en) Asphalt compositions
CN1106893C (zh) 一种利用酸渣生产磺化沥青的方法
EP0991723B1 (fr) Revetement
US5401308A (en) Quebracho-modified bitumen compositions, method of manufacture and use
US20250304792A1 (en) Road Bitumen Composition (Variants) And Preparation Method Thereof

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20000913

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE

17Q First examination report despatched

Effective date: 20010525

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN

18D Application deemed to be withdrawn

Effective date: 20030617