JPH0359035A - Production of concentrated lignocellulosic substance solution - Google Patents
Production of concentrated lignocellulosic substance solutionInfo
- Publication number
- JPH0359035A JPH0359035A JP19271889A JP19271889A JPH0359035A JP H0359035 A JPH0359035 A JP H0359035A JP 19271889 A JP19271889 A JP 19271889A JP 19271889 A JP19271889 A JP 19271889A JP H0359035 A JPH0359035 A JP H0359035A
- Authority
- JP
- Japan
- Prior art keywords
- solution
- concentration
- weight
- lignocellulosic
- lignocellulosic material
- 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.)
- Pending
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000000126 substance Substances 0.000 title abstract 4
- 238000004090 dissolution Methods 0.000 claims abstract description 19
- 239000003960 organic solvent Substances 0.000 claims abstract description 11
- 239000012978 lignocellulosic material Substances 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 12
- 239000002023 wood Substances 0.000 abstract description 20
- 235000013312 flour Nutrition 0.000 abstract description 12
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 abstract description 10
- 239000000203 mixture Substances 0.000 abstract description 6
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 15
- -1 bisphenol compound Chemical class 0.000 description 10
- 239000003054 catalyst Substances 0.000 description 7
- 239000002253 acid Substances 0.000 description 5
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229930185605 Bisphenol Natural products 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 150000002989 phenols Chemical class 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- NXXYKOUNUYWIHA-UHFFFAOYSA-N 2,6-Dimethylphenol Chemical compound CC1=CC=CC(C)=C1O NXXYKOUNUYWIHA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- IWDCLRJOBJJRNH-UHFFFAOYSA-N p-cresol Chemical compound CC1=CC=C(O)C=C1 IWDCLRJOBJJRNH-UHFFFAOYSA-N 0.000 description 2
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000010902 straw Substances 0.000 description 2
- 150000005846 sugar alcohols Polymers 0.000 description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- WHOZNOZYMBRCBL-OUKQBFOZSA-N (2E)-2-Tetradecenal Chemical compound CCCCCCCCCCC\C=C\C=O WHOZNOZYMBRCBL-OUKQBFOZSA-N 0.000 description 1
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 description 1
- YKCPTPSKQFNDHL-UHFFFAOYSA-N 2-(chloroamino)acetic acid Chemical compound OC(=O)CNCl YKCPTPSKQFNDHL-UHFFFAOYSA-N 0.000 description 1
- ABMULKFGWTYIIK-UHFFFAOYSA-N 2-hexylphenol Chemical compound CCCCCCC1=CC=CC=C1O ABMULKFGWTYIIK-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- KLSLBUSXWBJMEC-UHFFFAOYSA-N 4-Propylphenol Chemical compound CCCC1=CC=C(O)C=C1 KLSLBUSXWBJMEC-UHFFFAOYSA-N 0.000 description 1
- CYYZDBDROVLTJU-UHFFFAOYSA-N 4-n-Butylphenol Chemical compound CCCCC1=CC=C(O)C=C1 CYYZDBDROVLTJU-UHFFFAOYSA-N 0.000 description 1
- QHPQWRBYOIRBIT-UHFFFAOYSA-N 4-tert-butylphenol Chemical compound CC(C)(C)C1=CC=C(O)C=C1 QHPQWRBYOIRBIT-UHFFFAOYSA-N 0.000 description 1
- 241000609240 Ambelania acida Species 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- HTVITOHKHWFJKO-UHFFFAOYSA-N Bisphenol B Chemical compound C=1C=C(O)C=CC=1C(C)(CC)C1=CC=C(O)C=C1 HTVITOHKHWFJKO-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 description 1
- TVWHNULVHGKJHS-UHFFFAOYSA-N Uric acid Natural products N1C(=O)NC(=O)C2NC(=O)NC21 TVWHNULVHGKJHS-UHFFFAOYSA-N 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000010905 bagasse Substances 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- LLEMOWNGBBNAJR-UHFFFAOYSA-N biphenyl-2-ol Chemical compound OC1=CC=CC=C1C1=CC=CC=C1 LLEMOWNGBBNAJR-UHFFFAOYSA-N 0.000 description 1
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 229910000042 hydrogen bromide Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000010893 paper waste Substances 0.000 description 1
- 229940044654 phenolsulfonic acid Drugs 0.000 description 1
- 239000011120 plywood Substances 0.000 description 1
- 229940079877 pyrogallol Drugs 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 229940116269 uric acid Drugs 0.000 description 1
- 239000002916 wood waste Substances 0.000 description 1
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、リグノセルロース物質の濃厚溶液製造方法に
関するものである。更に詳しく述べるならば、本発明は
、リグノセルロース物質を均一に、効率よく溶解してそ
の濃厚溶液を製造する方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing concentrated solutions of lignocellulosic materials. More specifically, the present invention relates to a method for uniformly and efficiently dissolving lignocellulosic materials to produce a concentrated solution thereof.
森林から生産される諸賢源は、再生可能なものであって
、その有効な循環利用が現在強く望まれている。例えば
、バルブ工業や木材工業のような木材を原料とする工業
においては、それから発生する木質系廃棄物の有効な利
用方法の確立が急がれており、また、稲わらやもみがら
のようなリグノセルロース物質を含有する農業廃棄物の
有効利用方法についても、早急の開発が待ち望まれてい
る。The various sources produced from forests are renewable, and their effective cyclical use is currently strongly desired. For example, in industries that use wood as raw material, such as the valve industry and the lumber industry, there is an urgent need to establish ways to effectively utilize the wood waste generated. There is also a need for urgent development of methods for effectively utilizing agricultural waste containing lignocellulosic materials.
木材などを含有するリグノセルロース材料の有効利用法
としては、例えば、特開昭５７−２３６０号、および特
公昭６３−１９９２号などにリグノセルロース分子中の
水酸基の一部分に、少なくとも１種の置換基を導入して
得られる化学修飾リグノセルロース材料を有機溶媒に溶
解し、この溶液を種々の樹脂材料用原料として利用する
方法が開示されている。As an effective use of lignocellulose materials containing wood, for example, Japanese Patent Application Laid-open No. 57-2360 and Japanese Patent Publication No. 63-1992 disclose that at least one substituent is added to a portion of the hydroxyl group in the lignocellulose molecule. A method is disclosed in which a chemically modified lignocellulose material obtained by introducing a lignocellulose material is dissolved in an organic solvent, and this solution is used as a raw material for various resin materials.
また、特開昭６０−２０６８８３号および６０−１０４
５１３号公報には、リグノセルロース材料をフェノール
化合物−ホルムアルデヒド樹脂系接着剤として利用する
方法、およびこれを繊維化する方法が開示されている。Also, JP-A Nos. 60-206883 and 60-104
Publication No. 513 discloses a method of utilizing a lignocellulose material as a phenolic compound-formaldehyde resin adhesive and a method of making it into fibers.
更に、特開昭６１−２１５６７６号、および６１−２１
５６７５号公報には、リグノセルロース材料を多価アル
コール、又はビスフェノール化合物からなる溶剤に溶解
し、この溶液とボリウレクン系、エポキシ系、或はその
他の樹脂材料とともに用いて成形物、発砲体、或は接着
剤を製造する方法などが開示されている。Furthermore, JP-A-61-215676 and JP-A-61-21
No. 5675 discloses that a lignocellulose material is dissolved in a solvent consisting of a polyhydric alcohol or a bisphenol compound, and this solution is used together with polyurecne, epoxy, or other resin materials to form molded articles, foams, or Disclosed are methods for producing adhesives and the like.
更に、特開昭６１−２６１３５８号公報には、前処理な
しの木材を、触媒を用いることなしでフェノール化合物
、又はビスフェノール化合物からなる溶剤に直接溶解す
る方法が開示されており、特開昭６２−７９２３０号公
報には、前処理なしの木材を、アルコール化合物、多価
アルコール化合物、オキシエーテル化合物、環状エーテ
ル化合物、またはケトン化合物からなる溶剤に触媒を用
いることな（直接溶解する方法が開示されている。Furthermore, JP-A No. 61-261358 discloses a method of directly dissolving wood without pretreatment in a solvent consisting of a phenol compound or a bisphenol compound without using a catalyst. Publication No. 79230 discloses a method in which wood without pretreatment is directly dissolved in a solvent consisting of an alcohol compound, a polyhydric alcohol compound, an oxyether compound, a cyclic ether compound, or a ketone compound without using a catalyst. ing.
上記のようなリグノセルロース物質の利用に関する従来
技術における問題点は、木材などのリグノセルロース物
質の均一な濃厚溶液の調製が困難であるという点にあっ
た。例えば５０％以上の高濃度のリグノセルロース物質
溶液を得るために、有機溶媒中に当該高濃度に相当する
量のリグノセルロース物質を混合し、この混合物を溶解
反応容器中に充填し、加圧下、又は常圧下で、これに加
熱溶解処理を施す場合、リグノセルロース物質が多量の
空気を含んでいるため熱の伝達効率が低く、このため空
気等の除去および溶解に長時間を要し、エネルギーコス
トが高く、生産性が低いという問題点があった。A problem with the prior art regarding the use of lignocellulosic materials as described above is that it is difficult to prepare a homogeneous concentrated solution of lignocellulosic materials such as wood. For example, in order to obtain a lignocellulosic material solution with a high concentration of 50% or more, an amount of lignocellulosic material corresponding to the high concentration is mixed in an organic solvent, this mixture is filled into a dissolution reaction vessel, and under pressure, Alternatively, when heating and dissolving it under normal pressure, the lignocellulose material contains a large amount of air, so the heat transfer efficiency is low, so it takes a long time to remove and dissolve the air, resulting in energy costs. The problem was that productivity was high and productivity was low.
本発明は従来技術の上記問題点を解消し、リグノセルロ
ース物質の濃度溶液を、簡単な操作で効率よく製造する
方法を提供しようとするものである。The present invention aims to solve the above-mentioned problems of the prior art and provide a method for efficiently producing a concentrated solution of lignocellulosic material with simple operations.
本発明のリグノセルロース物質濃厚溶液の製造方法は、
リグノセルロース物質の濃厚溶液を調製するに際し、先
ず、有機溶媒にセルロース物質を３０重量％以下の濃度
に溶解し、その後、先行溶解工程により得られた溶液に
、リグノセルロース物質を追加し、その濃度を２〜１５
重量％の範囲内で漸次増加させる溶解操作を１回以上施
すことを特徴とするものである。The method for producing a concentrated lignocellulosic material solution of the present invention includes:
In preparing a concentrated solution of lignocellulosic material, first, the cellulosic material is dissolved in an organic solvent to a concentration of 30% by weight or less, and then the lignocellulosic material is added to the solution obtained by the preceding dissolution step to adjust the concentration. 2 to 15
It is characterized by performing a dissolution operation in which the weight percentage is gradually increased within a range of one or more times.
本発明方法に用いられるリグノセルロース物質は、木材
片、木粉、木材ａｍ、木材チップ、単板くず、合板くず
、古紙、パルプ、稲わら、モミガラ、コーリャン、バガ
ス、竹、麦わらなどを包含する植物！ａｍ材料から選択
することができる。Lignocellulosic materials used in the method of the present invention include wood chips, wood flour, wood ammo, wood chips, veneer waste, plywood waste, waste paper, pulp, rice straw, rice husk, kolyang, bagasse, bamboo, wheat straw, etc. plant! AM materials can be selected.
本発明方法に用いられる有機溶媒は、下記のようなフェ
ノール類から選択された少なくとも１種を主成分として
含むものである。The organic solvent used in the method of the present invention contains as a main component at least one kind selected from the following phenols.
（１）−価フエノール化合物：例えば、フェノール、０
−・ｍ−１およびｐ−クレゾール、３５− ２．３−１
および２．６−キシレノール、ｏ−１ｍ−１およびｐ−
プロピルフェノール、０−１ｍ−１およびｐ−ブチルフ
ェノール、〇−ｍ−１およびｐ−５ｅｃ−ブチルフェノ
ール、０−ｌｍ−およびｐ−ｔｅｒｔ−ブチルフェノー
ル、ヘキシルフェノール、フェニルフェノール、オクチ
ルフェノール、およびナフトールなど
（２〉二価フェノール化合物：例えばカテコール、レゾ
ルシノール、キノール、ビスフェノールＡ１ビスフエノ
ールＢおよびビスフェノールＦなど
（３）三価フェノール化合物：例えばピロガロール、ク
ロログリシン、トリヒドロベンゼン、および浸食子酸。(1) -valent phenol compound: for example, phenol, 0
-・m-1 and p-cresol, 35- 2.3-1
and 2,6-xylenol, o-1m-1 and p-
Propylphenol, 0-1m-1 and p-butylphenol, 0-m-1 and p-5ec-butylphenol, 0-lm- and p-tert-butylphenol, hexylphenol, phenylphenol, octylphenol, and naphthol, etc. (2) Dihydric phenolic compounds: such as catechol, resorcinol, quinol, bisphenol A1 bisphenol B and bisphenol F. (3) Trihydric phenolic compounds: such as pyrogallol, chloroglycine, trihydrobenzene, and erosic acids.
有機溶媒は、溶解触媒を含んでいてもよく、含んでいな
くてもよい。The organic solvent may or may not contain a dissolved catalyst.
溶解触媒は下記の酸類から選ばれた少なくとも１員を含
むものである。The dissolved catalyst contains at least one member selected from the following acids.
（１）無機（鉱）酸：例えば塩酸、硫酸、リン酸および
臭化水素など
（２）有機酸
（イ）カルボン酸；ギ酸、酢酸、シュウ酸、酒石酸、お
よび安息香酸など
（０）’［１スルホン酸：例エバフェノールスルホン酸
およびｐ−トルエンスルホン酸など（ハ〉有機スルフィ
ンＩ：例えばフェノールスルフィン酸
（ニ）その他；例えば尿酸
溶解触媒を用いる場合、溶液中に含まれるリグノセルロ
ース物質の最終合計量１００重量部に対し、０．１〜２
０重量部の溶解触媒を用いることが好ましい。(1) Inorganic (mineral) acids: such as hydrochloric acid, sulfuric acid, phosphoric acid, and hydrogen bromide (2) Organic acids (a) Carboxylic acids: such as formic acid, acetic acid, oxalic acid, tartaric acid, and benzoic acid (0)'[ 1 Sulfonic acid: Examples include evaphenolsulfonic acid and p-toluenesulfonic acid (iii) Organic sulfin I: For example, phenolsulfinic acid (d) Others; For example, when using a uric acid dissolving catalyst, the final concentration of lignocellulosic material contained in the solution 0.1 to 2 per 100 parts by weight of total amount
Preferably, 0 parts by weight of dissolved catalyst are used.
本発明方法において、得られるリグノセルロース物質濃
厚溶液の最終濃度については格別の限定はなく、リグノ
セルロース物質の種類、有機溶剤の種類および溶液の用
途、溶解操作における加圧の有無などを勘案して適宜設
定することができるが一般に、４０重量％以上であるこ
とが好ましい。In the method of the present invention, there is no particular limitation on the final concentration of the concentrated solution of lignocellulosic material obtained, and the final concentration of the lignocellulosic material concentrated solution is determined by taking into consideration the type of lignocellulosic material, the type of organic solvent, the use of the solution, the presence or absence of pressure during the dissolution operation, etc. Although it can be set as appropriate, it is generally preferably 40% by weight or more.
加圧溶解の場合、得られる濃厚溶液に、リグノセルロー
ス物質の濃度に格別の限界はない。加圧の程度も格別の
限定はないが、一般に、２〜６０ｋｇ／ｃｄ程度である
ことが好ましい。In the case of pressure dissolution, there is no particular limit to the concentration of lignocellulosic material in the resulting concentrated solution. The degree of pressurization is also not particularly limited, but is generally preferably about 2 to 60 kg/cd.
常圧溶解および加圧溶解のいづれにおいても、有機溶媒
１００重量部に対して、最終合計量５０〜１０００重量
部のリグノセルロース物質を溶解することが可能である
。In both normal pressure dissolution and pressurized dissolution, it is possible to dissolve a final total amount of 50 to 1000 parts by weight of lignocellulosic material per 100 parts by weight of the organic solvent.
本発明方法の各溶解操作における溶解温度に格別の限定
はないが、リグノセルロース物質の種類、有機溶剤の種
類、圧力および濃度などを勘案して、加圧溶解の場合に
は２００℃〜３００℃、常圧溶解の場合には１００℃〜
２００℃の範囲に設定することが好ましい。There is no particular limitation on the melting temperature in each melting operation of the method of the present invention, but in the case of pressurized melting, the temperature is 200°C to 300°C, taking into account the type of lignocellulose material, the type of organic solvent, the pressure and concentration, etc. , in the case of normal pressure melting, 100℃ ~
It is preferable to set the temperature within the range of 200°C.
本発明方法においてその第１溶解操作においてリグノセ
ルロース物質は３０重量％以下の濃度、好ましくは１０
〜２５重量％の濃度で溶解される。この濃度が３０重量
％より高くなると均一溶解が困難になり、場合によって
は殆んど溶解しないこともある。In the method of the invention, in the first dissolution operation, the lignocellulosic material is present at a concentration of less than 30% by weight, preferably 10% by weight.
It is dissolved at a concentration of ~25% by weight. When this concentration is higher than 30% by weight, uniform dissolution becomes difficult, and in some cases, almost no dissolution may occur.
また、第２溶解操作以降の各溶解操作においては、リグ
ノセルロース物質の濃度の増加を２〜１５重量％である
。このとき、各溶解操作におけるリグノセルロース物質
濃度の増加が２重量％未渦の場合、所望濃厚濃度に到達
するに要する溶解操作の回数が過多になって、経済性お
よび生産性が不十分になり、また、それが１５重量％よ
り高くなると、リグノセルロース物質の均一な溶解が困
難になり、溶解に長時間を要したり、或は均一溶液が得
られないことがある。Further, in each dissolution operation after the second dissolution operation, the concentration of the lignocellulosic material is increased by 2 to 15% by weight. At this time, if the lignocellulosic material concentration increases by 2% by weight in each dissolution operation, the number of dissolution operations required to reach the desired concentrated concentration will be excessive, resulting in insufficient economic efficiency and productivity. Moreover, if it is higher than 15% by weight, it becomes difficult to uniformly dissolve the lignocellulosic material, and it may take a long time to dissolve or a homogeneous solution may not be obtained.
本発明方法を下記実施例により更に説明する。 The method of the invention is further illustrated by the following examples.
実施例１
６０ｇ木粉を、第１表記載の溶解操作により、フェノー
ル５０ｇと３．７５ｍ１．のフェノールスルフォン酸（
溶解触媒、フェノール重量に対し、７．５％に相当）と
の混合物（５３，７５ｇ ）に溶解した。Example 1 60 g of wood flour was dissolved with 50 g of phenol and 3.75 ml of phenol. of phenolsulfonic acid (
The catalyst was dissolved in a mixture (53.75 g) of phenol (corresponding to 7.5% by weight, based on the weight of phenol).
第
表
但し、上記溶解操作は加熱、および冷却装置および撹拌
機つきフラスコ中において行われた。However, the above dissolution operation was carried out in a flask equipped with a heating and cooling device and a stirrer.
得られた木粉溶液は、良好な流動性を示した。The obtained wood flour solution showed good fluidity.
比較例１
実施例１と同様の操作を行った。但し、木粉の全１（６
０ｇ）を−度に溶媒に混合した。常圧、１５０℃の溶解
操作が６０分間経過したとき、混合物は全体として黒色
を呈するのみで、固体状であった。この加熱溶解操作を
約１０時間続けたが、フラスコの底部にある木粉部分が
部分的に溶解したが全体としては懸濁混合物の状態であ
った。Comparative Example 1 The same operation as in Example 1 was performed. However, all 1 (6
0g) was mixed into the solvent at a time. After 60 minutes of dissolution operation at normal pressure and 150° C., the mixture had a black color as a whole and was in a solid state. This heating and dissolving operation was continued for about 10 hours, and although the wood flour portion at the bottom of the flask was partially dissolved, the entire mixture remained in a suspended mixture state.
実施例２
１、 ＯＩ！オートクレーブにフェノール４００ｇを仕
込み、第２表記載の溶解操作により、木粉を溶解した。Example 2 1. OI! 400 g of phenol was placed in an autoclave, and the wood flour was dissolved by the dissolving operation described in Table 2.
最終の未溶解木粉の重量は全仕込み木粉重量に対して１
％以下であり、得られた木粉ａ厚溶液は、良好な流動性
を示した。The weight of the final undissolved wood flour is 1 for the total weight of the wood flour used.
% or less, and the obtained wood flour a thick solution showed good fluidity.
第２表
比較例２
実施例２と同一のオートクレーブに、木粉６００ｇおよ
びフェノール４００ｇを同時に仕込み、２５０°Ｃで６
時間加温した。その後、溶解物を観察したところ、不均
一で流動性が無く、未溶解木粉重量は、全仕込み木粉重
量に対し１９％であった。Table 2 Comparative Example 2 Into the same autoclave as in Example 2, 600 g of wood flour and 400 g of phenol were charged at the same time.
Warmed for hours. Thereafter, when the melt was observed, it was found to be non-uniform and had no fluidity, and the weight of undissolved wood flour was 19% of the weight of the total wood flour.
本発明方法によりリグノセルロース物質の均一な濃厚溶
液を短時間内に効率よく、かつ高い生産性で製造するこ
とが可能になった。The method of the present invention makes it possible to produce a uniform, concentrated solution of lignocellulosic material within a short period of time, efficiently, and with high productivity.
Claims (1)
、先ず、有機溶媒に、リグノセルロース物質を、３０重
量％以下の濃度に溶解し、その後、先行溶解工程により
得られた溶液に、リグノセルロース物質を追加し、その
濃度を２〜１５重量％の範囲内で漸次増加させる溶解操
作を１回以上施すことを特徴とする、リグノセルロース
物質濃厚溶液の製造方法。1. When preparing a concentrated solution of lignocellulosic material, first dissolve the lignocellulosic material in an organic solvent to a concentration of 30% by weight or less, and then add the lignocellulosic material to the solution obtained in the preceding dissolution step. 1. A method for producing a concentrated solution of lignocellulosic material, comprising performing a dissolution operation at least once in which the concentration of the lignocellulose material is gradually increased within the range of 2 to 15% by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19271889A JPH0359035A (en) | 1989-07-27 | 1989-07-27 | Production of concentrated lignocellulosic substance solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19271889A JPH0359035A (en) | 1989-07-27 | 1989-07-27 | Production of concentrated lignocellulosic substance solution |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0359035A true JPH0359035A (en) | 1991-03-14 |
Family
ID=16295910
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19271889A Pending JPH0359035A (en) | 1989-07-27 | 1989-07-27 | Production of concentrated lignocellulosic substance solution |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0359035A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005206468A (en) * | 2004-01-20 | 2005-08-04 | Forestry & Forest Products Research Institute | Method for producing saccharides and solid fuel using biomass as raw material |
| JP2005205252A (en) * | 2004-01-20 | 2005-08-04 | Kobe Steel Ltd | High-concentration slurry containing biomass, method for preparing high-concentration slurry and method for manufacturing biomass fuel |
| US7276591B2 (en) | 2003-05-06 | 2007-10-02 | Fuji Carbon Co., Ltd. | Biomass resin composition, process for preparing the same and molding material using the biomass composition |
-
1989
- 1989-07-27 JP JP19271889A patent/JPH0359035A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7276591B2 (en) | 2003-05-06 | 2007-10-02 | Fuji Carbon Co., Ltd. | Biomass resin composition, process for preparing the same and molding material using the biomass composition |
| JP2005206468A (en) * | 2004-01-20 | 2005-08-04 | Forestry & Forest Products Research Institute | Method for producing saccharides and solid fuel using biomass as raw material |
| JP2005205252A (en) * | 2004-01-20 | 2005-08-04 | Kobe Steel Ltd | High-concentration slurry containing biomass, method for preparing high-concentration slurry and method for manufacturing biomass fuel |
| JP4726035B2 (en) * | 2004-01-20 | 2011-07-20 | 独立行政法人森林総合研究所 | Production method of sugar and solid fuel using biomass as raw material |
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