NO137125B - PROCEDURES FOR THE MANUFACTURE OF ADHESIVES FOR FIBER PRODUCTS, ESPECIALLY LIGNOCELLULOSIS OR WOOD MATERIALS SUCH AS PINE AND CHIPBOARD. - Google Patents
PROCEDURES FOR THE MANUFACTURE OF ADHESIVES FOR FIBER PRODUCTS, ESPECIALLY LIGNOCELLULOSIS OR WOOD MATERIALS SUCH AS PINE AND CHIPBOARD. Download PDFInfo
- Publication number
- NO137125B NO137125B NO2746/73A NO274673A NO137125B NO 137125 B NO137125 B NO 137125B NO 2746/73 A NO2746/73 A NO 2746/73A NO 274673 A NO274673 A NO 274673A NO 137125 B NO137125 B NO 137125B
- Authority
- NO
- Norway
- Prior art keywords
- glue
- black liquor
- phenol
- formaldehyde
- firmness
- Prior art date
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 239000002023 wood Substances 0.000 title claims description 13
- 239000000463 material Substances 0.000 title claims description 7
- 238000000034 method Methods 0.000 title claims description 6
- 239000011093 chipboard Substances 0.000 title claims description 4
- 239000000853 adhesive Substances 0.000 title description 9
- 239000003292 glue Substances 0.000 claims description 63
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 53
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 39
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 18
- 229920005610 lignin Polymers 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 13
- 239000001913 cellulose Substances 0.000 claims description 7
- 229920002678 cellulose Polymers 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 4
- 229920001568 phenolic resin Polymers 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 15
- 229910021653 sulphate ion Inorganic materials 0.000 description 14
- 235000018185 Betula X alpestris Nutrition 0.000 description 13
- 235000018212 Betula X uliginosa Nutrition 0.000 description 13
- 238000004026 adhesive bonding Methods 0.000 description 12
- 230000001070 adhesive effect Effects 0.000 description 8
- 239000000654 additive Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 108010054218 Factor VIII Proteins 0.000 description 5
- 102000001690 Factor VIII Human genes 0.000 description 5
- 235000013312 flour Nutrition 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 235000017343 Quebracho blanco Nutrition 0.000 description 4
- 241000065615 Schinopsis balansae Species 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- 239000005416 organic matter Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 229930040373 Paraformaldehyde Natural products 0.000 description 3
- 235000011941 Tilia x europaea Nutrition 0.000 description 3
- 241000209140 Triticum Species 0.000 description 3
- 235000021307 Triticum Nutrition 0.000 description 3
- -1 bark boards Substances 0.000 description 3
- 239000004571 lime Substances 0.000 description 3
- 230000020477 pH reduction Effects 0.000 description 3
- 229920002866 paraformaldehyde Polymers 0.000 description 3
- 239000004848 polyfunctional curative Substances 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 239000011122 softwood Substances 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 241000218657 Picea Species 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 238000010411 cooking Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000004310 lactic acid Substances 0.000 description 2
- 235000014655 lactic acid Nutrition 0.000 description 2
- 229940046892 lead acetate Drugs 0.000 description 2
- 239000000123 paper Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000010902 straw Substances 0.000 description 2
- ZMWAXVAETNTVAT-UHFFFAOYSA-N 7-n,8-n,5-triphenylphenazin-5-ium-2,3,7,8-tetramine;chloride Chemical compound [Cl-].C=1C=CC=CC=1NC=1C=C2[N+](C=3C=CC=CC=3)=C3C=C(N)C(N)=CC3=NC2=CC=1NC1=CC=CC=C1 ZMWAXVAETNTVAT-UHFFFAOYSA-N 0.000 description 1
- 241000609240 Ambelania acida Species 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229920001342 Bakelite® Polymers 0.000 description 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- 241000218631 Coniferophyta Species 0.000 description 1
- 108010023321 Factor VII Proteins 0.000 description 1
- 235000008124 Picea excelsa Nutrition 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 235000008582 Pinus sylvestris Nutrition 0.000 description 1
- 241000218626 Pinus sylvestris Species 0.000 description 1
- 239000002535 acidifier Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000012042 active reagent Substances 0.000 description 1
- 125000005910 alkyl carbonate group Chemical group 0.000 description 1
- 150000001350 alkyl halides Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 239000010905 bagasse Substances 0.000 description 1
- 239000004637 bakelite Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 125000000853 cresyl group Chemical class C1(=CC=C(C=C1)C)* 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011121 hardwood Substances 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 239000004849 latent hardener Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 235000010204 pine bark Nutrition 0.000 description 1
- 239000001839 pinus sylvestris Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000000284 resting effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 239000002916 wood waste Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G16/00—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00
- C08G16/02—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes
- C08G16/0293—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes with natural products, oils, bitumens, residues
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F16/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical
- C08F16/02—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an alcohol radical
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/04—Condensation polymers of aldehydes or ketones with phenols only
- C09J161/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2666/00—Composition of polymers characterized by a further compound in the blend, being organic macromolecular compounds, natural resins, waxes or and bituminous materials, non-macromolecular organic substances, inorganic substances or characterized by their function in the composition
- C08L2666/02—Organic macromolecular compounds, natural resins, waxes or and bituminous materials
- C08L2666/26—Natural polymers, natural resins or derivatives thereof according to C08L1/00 - C08L5/00, C08L89/00, C08L93/00, C08L97/00 or C08L99/00
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Phenolic Resins Or Amino Resins (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
- Paper (AREA)
Description
Den foreliggende oppfinnelse angår en fremgangsmåte til fremstilling av lim for fiberprodukter, særlig lignocellulose- The present invention relates to a method for producing glue for fiber products, in particular lignocellulosic
og trematerialer som finér og sponplater, innbefattende å bringe formaldehyd eller formaldehyd-avgivende forbindelser til reaksjon med sulfatligninholdige produkter. and wood materials such as veneer and chipboard, including reacting formaldehyde or formaldehyde-releasing compounds with sulfate lignin-containing products.
Til fabrikasjon av lim for finér, sponplater m.v. anvendes for nærværende først og fremst urea og fenol samt formaldehyd som utgangsmateriale. Disse lim representerer en omkostning som ikke er ubetydelig i forhold til verdien av fibermaterialet, særlig når det gjelder fremstilling av billige produkter som barkplater, halmplater etc., samtidig som urealimets vannfasthet er begrenset og dets sure reaksjon i lengden kan fryktes å være skadelig for cellulosematerialets mekaniske fasthet. For the manufacture of glue for veneer, chipboard, etc. At present, primarily urea and phenol as well as formaldehyde are used as starting materials. These glues represent a cost that is not insignificant in relation to the value of the fiber material, especially when it comes to the production of cheap products such as bark boards, straw boards etc., at the same time that the urea glue's water resistance is limited and its acidic reaction in the long run can be feared to be harmful to the cellulose material's mechanical firmness.
Fra US-PS 3 395 033 er der kjent en fremgangsmåte til fremstilling av lim hvor der blandt annet benyttes ligninbestanddeler som betegnes som nøytralisert ligninsvartlut eller avsukret lignin. Den ligninsvartlut som omtales, er imidlertid sur sulfitt-avlut, idet avluten ved et passende produksjonstrinn nøytraliseres med et alkalisk reagens, nemlig amoniakk. Også når der benyttes avsukret lignin som utgangsmateriale, nøytraliseres dette ifølge det amerikanske patentskrift med ammoniumhydroksyd eller annet alkali, dvs. at der også her er tale om sulfitt-avlut. From US-PS 3 395 033 there is known a method for the production of glue where, among other things, lignin components are used which are referred to as neutralized lignin black liquor or desugared lignin. However, the lignin black liquor referred to is acid sulphite waste liquor, as the waste liquor is neutralized in a suitable production step with an alkaline reagent, namely ammonia. Also when desugared lignin is used as starting material, this is neutralized according to the American patent with ammonium hydroxide or other alkali, i.e. that here too we are talking about sulphite waste liquor.
I et eksempel i det nevnte amerikanske patentskrift er der anført et produkt fra sulfatsvartlut, nærmere bestemt det isolerte sulfatlignin Indulin som utfelles fra sulfatsvartlut ved ansyring og isoleres ved filtrering, dekantering eller sentrifugering. Dette produkt er imidlertid uoppløselig i vann, noe som medfører at man er nødt til å anvende en stor mengde av et oppløsnings-middel for lignin, nemlig dimetylformamid. In an example in the aforementioned US patent, a product from sulphate black liquor is listed, more specifically the isolated sulphate lignin Indulin which is precipitated from sulphate black liquor by acidification and isolated by filtration, decantation or centrifugation. However, this product is insoluble in water, which means that one has to use a large amount of a solvent for lignin, namely dimethylformamide.
Følgelig har det tidligere vært foreslått å benytte isolert sulfatlignin i lim og bakelittplast i kombinasjon med plast, særlig fenolplast. Bruken av isolert sulfatlignin til lim krever imidlertid en kostbar og besværlig isolasjonsprosess som selvsagt vil virke inn både tidsmessig og økonomisk på det ferdige limprodukt. Videre lider en slik kjent fremgangsmåte til fremstilling av lim av den mangel at der må anvendes meget fenol, i regelen fenol og lignin i forholdet 1:1. Consequently, it has previously been proposed to use isolated sulphate lignin in glue and bakelite plastic in combination with plastic, especially phenolic plastic. The use of isolated sulphate lignin for glue, however, requires an expensive and difficult isolation process, which will of course have an impact both in terms of time and financially on the finished glue product. Furthermore, such a known method for producing glue suffers from the shortcoming that a lot of phenol must be used, as a rule phenol and lignin in a ratio of 1:1.
Hensikten med den foreliggende oppfinnelse er å råde bot på de ovennevnte ulemper, idet der ifølge oppfinnelsen gis anvisning på en fremgangsmåte til fremstilling av lim som gir et rimelig limprodukt som åpner nye muligheter for liming av billige treprodukter . The purpose of the present invention is to remedy the above-mentioned disadvantages, as according to the invention, instructions are given for a method for producing glue which gives a reasonable glue product which opens up new possibilities for gluing cheap wood products.
Hensikten er ifølge den foreliggende oppfinnelse oppnådd ved at svartlut fra sulfatcellulosekok ved oppvarmning bringes til å reagere med formaldehyd, at det fremkomne reaksjonsprodukt under oppvarmning, eventuelt under oppvarmning i en og samme operasjon som den nevnte reaksjon, blandes med fenolformaldehydharpiks i så stor mengde at forholdet mellom svartlutens organiske substans og harpiksfenol blir 5:1 -2:1, hvoretter blandingens pH innstilles på en verdi av 7-10,5, og eventuelt at der etter avkjøling tilsettes blandingen 2-15% formaldehyd, regnet på limets organiske substans. According to the present invention, the purpose is achieved by heating black liquor from sulphate cellulose coke to react with formaldehyde, so that the resulting reaction product during heating, possibly during heating in one and the same operation as the aforementioned reaction, is mixed with phenol formaldehyde resin in such a large amount that the ratio between the black liquor's organic substance and resin phenol becomes 5:1 -2:1, after which the mixture's pH is set to a value of 7-10.5, and possibly that after cooling the mixture is added 2-15% formaldehyde, calculated on the glue's organic substance.
Ved systematisk studium av hvilke faktorer det er som vir-ker på limets kvalitet, har man således kommet til det over-raskende resultat at det ved anvendelse av de riktige betingel-ser meget vel lar seg gjøre for slik limfabrikasjon å anvende sulfatsvartlut direkte uten kostbar og besværlig isolering av sulfatligninet. Dessuten kan sulfatsvartlut anvendes i kombinasjon med bare en mindre mengde fenol, f.eks. i forholdet 1 vekt-del fenol til 4 vektdeler organisk substans i svartluten. By systematically studying which factors affect the quality of the glue, the surprising result has thus been reached that, by applying the right conditions, it is very well possible to use sulphate black liquor directly for such glue manufacture without expensive and difficult isolation of the sulfate lignin. Moreover, sulphate black liquor can be used in combination with only a small amount of phenol, e.g. in the ratio of 1 part by weight of phenol to 4 parts by weight of organic substance in the black liquor.
En faktor som har sterk virkning på fremstillingsprosessen, består i å innstille svartlutens pH-verdi etter limkoket på bare svakt alkalisk reaksjon, f.eks. pH 10-8, målt potensiometrisk i lim utspedd med vann i forholdet 1:10. pH-verdien for konsentrert svartlutlim ligger noe høyere. En annen faktor av betydning består i å anvende en ekstra tilsetning av formalin eller paraformaldehyd som en slags herder etter limkoket, men før limingen. A factor that has a strong effect on the manufacturing process consists in setting the pH value of the black liquor after the glue boil to only a weak alkaline reaction, e.g. pH 10-8, measured potentiometrically in glue diluted with water in a ratio of 1:10. The pH value for concentrated black liquor glue is somewhat higher. Another factor of importance consists in using an additional addition of formalin or paraformaldehyde as a kind of hardener after the glue is boiled, but before the gluing.
Arten av det anvendte fenollim spiller også en betydelig rolle. Rikelig anvendelse av formalin ved fremstillingen av limet.er her gunstig. Isteden behøver man ved limkoket på svart-lutandelen bare å tilsette relativt lite formalin. Disse for-holdsregler er enkle og billige. Limkoket kan utføres ved van-lig trykk og ved temperaturer under 100°C og i høyst 3 timer. Den ekstra tilsetning av formaldehyd på slutten har vist seg å om-danne svartlutens organiske sulfider slik at den ubehagelige lukt forsvinner. The nature of the phenolic adhesive used also plays a significant role. Abundant use of formalin in the production of the glue is beneficial here. Instead, you only need to add a relatively small amount of formalin when the glue is boiled on the black-lye part. These precautions are simple and cheap. The glue boil can be carried out at normal pressure and at temperatures below 100°C and for a maximum of 3 hours. The extra addition of formaldehyde at the end has been shown to transform the black liquor's organic sulphides so that the unpleasant smell disappears.
Muligheten av å anvende sulfatsvartlut i opprinnelig form istedenfor isolert lignin medfører store fordeler. Da avluten er alkalisk, behøves det ikke å tilføre svartlutkomponenten ekstra alkali. Operasjoner som ansyring, filtrering og ny til-førsel av alkali blir overflødige. Limkoket blir billigere enn limkok på fenol ved at der kan anvendes lav temperatur (f.eks. 70°C). Det er funnet at også en svartlut som er skånsomt oksydert med luft (jfr. det nedenstående eksempel 9), kan utnyttes for limfabrikasjon. Det er derfor neppe nødvendig å anvende reaksjonstreg beskyttelsesgass ved limfabrikasjonen. Viskositeten av oppløsninger av svartlutlim stiger bare langsomt ved oppbevaring ved værelsetemperatur. The possibility of using sulphate black liquor in its original form instead of isolated lignin entails major advantages. As the waste liquor is alkaline, there is no need to add additional alkali to the black liquor component. Operations such as acidification, filtration and new supply of alkali become redundant. The glue boil is cheaper than glue boil on phenol because a low temperature (e.g. 70°C) can be used. It has been found that a black liquor which is gently oxidized with air (cf. example 9 below) can also be used for adhesive manufacture. It is therefore hardly necessary to use a slow-reacting shielding gas during the adhesive manufacture. The viscosity of solutions of black liquor glue rises only slowly when stored at room temperature.
Da svartluter fra den såkalte sodacellulose-kokeprosess, hvor natriumhydroksyd er det aktive reagens, er alkaliske like-dan som sulfatsvartluter og inneholder alkaliligniner og produkter fra alkalisk nedbrytning av ved av hovedsakelig samme art. som i sulfatsvartluter, sier det seg selv at også svartluter fra sodaprosessen kan anvendes som utgangsmateriale ved den foreliggende oppfinnelse analogt med sulfatsvartluter. Then black liquors from the so-called soda cellulose cooking process, where sodium hydroxide is the active reagent, are alkaline just like sulphate black liquors and contain alkali lignins and products from alkaline decomposition of wood of essentially the same kind. as in sulphate black liquors, it goes without saying that black liquors from the soda process can also be used as starting material in the present invention analogously to sulphate black liquors.
Den lave pris for svartlutlimet ifølge oppfinnelsen åpner nye muligheter for liming av billige treprodukter, som bark, bar og vedavfall av forskjellig art, halm, bagasse etc., som det knapt kan lønne seg å lime med kostbare lim. Én fagmann med kjennskap til fiberprodukter vil lett innse at der foruten de nevnte materialer finnes en lang rekke mer eller mindre sekun-dære fibermaterialer som kan komme i'betraktning for liming med billig svartlutlim, og likeledes at den skisserte innstilling av surhetsgraden til det svakt alkaliske område kan utføres på mange forskjellige måter. Den lykkes godt med svovelsyre, eddiksyre eller melkesyre, men det lar seg selvsagt også gjøre å bruke mange andre sure eller syredannende materialer. Hva man velger, vil vesentlig bero på hva som finnes nærmest og billigst for hånden. Tenkelige materialer er sure kondensater fra inndunstning av sulfittavlut eller andre sure avluter fra kjemiske eller halvkjemiske cellulosekok eller fra tørrdestillasjon av ved, utspedd, rå svovelsyre fremkommet ved katalytisk oksydasjon av svoveldioksyd i røkgasser ved hjelp av luft og aktivt kull som katalysator, samt sluttelig kationbyttere av forskjellig art. Noe som også kan komme på tale, er treflis eller spon som ved oppvarmning, særlig i alkalisk oppløsning, avgir eddiksyre og andre organiske syrer. En spesiell gruppe av ansyringsmidler er de såkalte latente herdere, hvortil hører substanser som estre, inklusive alkylhalogenider, -karbonater og -sulfater, The low price of the black lime glue according to the invention opens up new possibilities for gluing cheap wood products, such as bark, bar and wood waste of various kinds, straw, bagasse etc., which it is hardly profitable to glue with expensive glues. A person skilled in the art with knowledge of fiber products will easily realize that, in addition to the materials mentioned, there are a large number of more or less secondary fiber materials that can be considered for gluing with cheap black liquor glue, and likewise that the outlined setting of the degree of acidity to the slightly alkaline area can be carried out in many different ways. It succeeds well with sulfuric acid, acetic acid or lactic acid, but it is of course also possible to use many other acidic or acid-forming materials. What you choose will largely depend on what is closest and cheapest to hand. Possible materials are acidic condensates from the evaporation of sulphite tailings or other acidic tailings from chemical or semi-chemical cellulose coking or from the dry distillation of wood, dilute, raw sulfuric acid produced by catalytic oxidation of sulfur dioxide in flue gases using air and activated carbon as a catalyst, as well as finally cation exchangers of different species. Something that can also come into question is wood chips or shavings which, when heated, especially in an alkaline solution, give off acetic acid and other organic acids. A special group of acidifying agents are the so-called latent hardeners, which include substances such as esters, including alkyl halides, -carbonates and -sulphates,
samt videre anhydrider og laktoner som ved'oppvarmning i alkalisk oppløsning danner salter av forskjellige syrer. as well as further anhydrides and lactones which, when heated in an alkaline solution, form salts of various acids.
Ved innstillingen av pH-^verdien kan visse deler av limet falle ut som finere eller grovere slam eller danne kolloidale oppløsninger. Også her finnes der variasjonsmuligheter som en fagmann lett vil se, f.eks. anvendelse av emulgatorer eller be-grensende mengder organiske oppløsningsmidler. When setting the pH value, certain parts of the glue may fall out as finer or coarser sludge or form colloidal solutions. Here, too, there are possibilities for variation that a professional will easily see, e.g. use of emulsifiers or limiting amounts of organic solvents.
En annen form for variasjonsmuligheter ligger i valget av separat eller sam-kok av fenollim og svartlutlim, som det fremgår av en sammenligning av det nedenstående eksempel 3 med eksemplene 1, 2 og 4-7. Videre kan man anvende svartluter fra kok av bar- eller løvtre, kokt til forskjellige pH-verdier. Andre variasjonsmuligheter består i kokning av både fenol- og svartlutlim til forskjellige viskositeter og anvendelse av forskjellige tilsetninger eller herdere, særlig ved liming av finér. Eksempler på slike herdere er krittpulver, tremel,.vavanittmel, quebracho og paraformaldehyd. Som det fremgår av eksemplene 7 Another form of variation possibilities lies in the choice of separate or co-cooking of phenol glue and black liquor glue, as can be seen from a comparison of example 3 below with examples 1, 2 and 4-7. You can also use black liquor from the boil of bare or hardwood, boiled to different pH values. Other possibilities for variation consist in boiling both phenolic and black liquor glue to different viscosities and using different additives or hardeners, especially when gluing veneers. Examples of such hardeners are chalk powder, wood flour, vavanite flour, quebracho and paraformaldehyde. As can be seen from the examples 7
og 8, kan det være gunstig å sløyfe en eller annen komponent, and 8, it may be beneficial to loop one or another component,
i dette tilfelle quebracho-ekstrakten. in this case the quebracho extract.
Den fenoliske bestanddel i fenolplastlimet behøver ikke nødvendigvis å være fenol, men kan også være en annen fenolisk substans med reaksjonsevne overfor formaldehyd, f.eks. kresoler, andre alkylfenoler eller blandinger av dem. The phenolic component in the phenolic plastic adhesive does not necessarily have to be phenol, but can also be another phenolic substance with reactivity towards formaldehyde, e.g. cresols, other alkylphenols or mixtures thereof.
Oppfinnelsen vil i det følgende bli belyst mer i detalj ved eksempler: In the following, the invention will be explained in more detail by means of examples:
Eksempel 1 Example 1
Svartlutlim: Black lute glue:
250,4 g svartlut fra cellulosekok på bartre med ca. 2/3 furu (Pinus sylvestris L) og 1/3 gran (Picea abies) med tørr-stoffinnhold 51,2% og innhold av organisk substans bestemt ifølge den av Centrallaboratoriet i Helsingfors foreskrevne analyse-metode 58:64 (CCA 23:48) 38,2% samt spesifikk vekt d=l,33 fikk 39,4 ml 35%'s formalin tilsatt og ble oppvarmet med stigerør i 3 timer ved 70°C samt deretter utspedd med 101,8 ml vann. Etter inndunstning av produktet i vakuum ved ca. 80°C til et tørrstoff innhold av 39,4% fås 1068 Asv.Spec. vekt d 1,21, viskositet (Ford cup nr. 2) 19,0 cP ved 20°C - etter 4 døgn ved værelsetemperatur stadig 19,0 cP. 250.4 g of black liquor from cellulose boiling on conifers with approx. 2/3 pine (Pinus sylvestris L) and 1/3 spruce (Picea abies) with a dry matter content of 51.2% and a content of organic matter determined according to the analysis method prescribed by the Central Laboratory in Helsinki 58:64 (CCA 23:48 ) 38.2% and specific weight d=1.33 had 39.4 ml of 35% formalin added and was heated with a riser for 3 hours at 70°C and then diluted with 101.8 ml of water. After evaporation of the product in vacuum at approx. 80°C to a dry matter content of 39.4% is obtained 1068 Asv.Spec. weight d 1.21, viscosity (Ford cup no. 2) 19.0 cP at 20°C - after 4 days at room temperature still 19.0 cP.
Fenollim: Phenolic glue:
30 g fenol, 28,5 ml natriumhydroksydoppløsning og 48,8 ml 35%'s formalin ble blandet og oppvarmet med stigerør i 3 timer ved 90°C, hvoretter der ble tilsatt 32,1 ml vann. Man fikk 1068 B fen. Beregnet tørrstoffinnhold 36,0%, mengde anvendt fenol 20,3% av limets vekt. Spesifikk vekt d = 1,10, viskositet for fersk prøve 27,0 cP - etter 4 døgn ved værelsetemperatur stadig 27,0 cP. 30 g of phenol, 28.5 ml of sodium hydroxide solution and 48.8 ml of 35% formalin were mixed and heated with a riser for 3 hours at 90°C, after which 32.1 ml of water was added. One got 1068 B fen. Calculated dry matter content 36.0%, amount of phenol used 20.3% of the glue's weight. Specific weight d = 1.10, viscosity for fresh sample 27.0 cP - after 4 days at room temperature still 27.0 cP.
177,9 g av svartlutlimet 1068 Asv og 54,6 g fenollim 1068 B fen ble blandet. Mengden av anvendt fenol var 19,1% av summen av mengdene av fenol og organisk substans i svartluten. Til denne blanding satte man 5,3 ml 35,5%'s formalin. Man fikk et blandingslim 1068 AB form, tørrstoffinnhold 38,5%, d = 1,18, viskositet for ferskt lim 24,9 cP - etter 1 døgn ved værelsetemperatur 27,0 cP. 177.9 g of the black liquor glue 1068 Asv and 54.6 g of phenolic glue 1068 B fen were mixed. The amount of phenol used was 19.1% of the sum of the amounts of phenol and organic matter in the black liquor. To this mixture was added 5.3 ml of 35.5% formalin. A mixed glue 1068 AB form was obtained, dry matter content 38.5%, d = 1.18, viscosity for fresh glue 24.9 cP - after 1 day at room temperature 27.0 cP.
Til 5 g av blandingslimet 1068 AB form satte man 6 dråper (= 0,22 ml) 12 n svovelsyre bg 1,2 g av en tilsatskombinasjon K bestående av 42% vavanitt, 21% quebracho-ekstrakt, 10,5% hvetemel og 26,3% kritt, alt i findelt form. pH-verdien var deretter 9,4, målt potensiometrisk på prøver utspedd med vann i forholdet 1:10. Blandingslimet gir ingen reaksjon på hydrogensulfid med blyacetatpapir etter ansyring med saltsyre 1:3 og skånsom opp-oppvarmning, noe som viser fravær av sulfidioner (S og SH ). Liming 6 min ved 150°C: Mekanisk fasthet på lufttørr bjerkefinér ^ IJ^^ , 2 kp/cm2. To 5 g of the mixed adhesive 1068 AB form, 6 drops (= 0.22 ml) of 12 n sulfuric acid were added together with 1.2 g of an additive combination K consisting of 42% vavanite, 21% quebracho extract, 10.5% wheat flour and 26 .3% chalk, all in finely divided form. The pH value was then 9.4, measured potentiometrically on samples diluted with water in the ratio 1:10. The mixture adhesive does not react to hydrogen sulphide with lead acetate paper after acidification with hydrochloric acid 1:3 and gentle heating, which shows the absence of sulphide ions (S and SH ). Bonding 6 min at 150°C: Mechanical strength on air-dry birch veneer ^ IJ^^ , 2 kp/cm2.
Etter henstand natten over i kar med vann på bunnen: After resting overnight in a vessel with water at the bottom:
v V V Fuktighetsøkning i finéren 4,3, resp. 4,7 fasthet 27^3 23x6 kp/cm . Kryssene her betyr at den ene eller begge limfuger i prøvestykket holdt godt mot bending for hånd. Bendingsforsøket med opprinnelig lufttørr finér ble foretatt etterat prøvestykket hadde fått stå i vann i 18-20 timer ved værelsetemperatur. Understrekede tall betyr: Fullt opptrukken linje: treet helt brukket før limetj prikket linje: treet rispet opp. Fasthetsfaktor (antall kryss) 7 av 8 mulige. v V V Moisture increase in the veneer 4.3, resp. 4.7 firmness 27^3 23x6 kp/cm . The crosses here mean that one or both glue joints in the test piece held well against bending by hand. The bending test with the original air-dry veneer was carried out after the test piece had been allowed to stand in water for 18-20 hours at room temperature. Underlined numbers mean: Full solid line: the wood completely broken before the gluej dotted line: the wood scratched up. Firmness factor (number of crosses) 7 out of 8 possible.
Eksempel 2 Example 2
Svartlutlim 1070 Csv ble fremstilt analogt med 1068 Asv (Eksempel 1) av 243,3 g svartlut og 38,7 ml 35%'s formalin ved oppvarmning i 3 timer ved 70°C og tilsetning av 64,1 ml vann. Tørrstoffinnholdet var deretter 39,9%, d = 1,23. Black liquor glue 1070 Csv was prepared analogously to 1068 Asv (Example 1) from 243.3 g of black liquor and 38.7 ml of 35% formalin by heating for 3 hours at 70°C and adding 64.1 ml of water. The dry matter content was then 39.9%, d = 1.23.
Fenollim 1070 B fen ble fremstilt analogt med 1068 B fen Phenolic glue 1070 B fen was produced analogously to 1068 B fen
i eksempel 1. in example 1.
212,5 g 1070 Csv ble blandet med 69,6 g 1070 B fen og 36,4 g 35%'s formalin og man fikk 1070 BC form. Tørrstoffinnhold 38,5%, spesifikk vekt d = 1,18, viskositet ved værelsetemperatur for fersk prøve (Ford cup nr. 2) 37,7 cP, viskositet etter 11 døgn ved værelsetemperatur 273 cP. Prøve på hydrogensulfid med blyacetatpapir (se eksempel 1) negativ. Til 5 g av denne blanding ble der satt 10 dråper (= 0,20 ml) 9,5-molar melkesyre og 1,2 g av samme tilsetning K som i eksempel 1. pH var deretter 8,95. Liming i 6 min ved 150°C: Fasthet for lufttørr bjerkefinér ^ ll^, <XX>17X4 kp/cm<2>. Fuktighetsøkning 4,2; 4,2%, fasthet <XX>2ii2, <X>26j,5 kp/cm<2>. Fasthetsfaktor 7 av 8 mulige. 212.5 g of 1070 Csv was mixed with 69.6 g of 1070 B fen and 36.4 g of 35% formalin and 1070 BC form was obtained. Dry matter content 38.5%, specific weight d = 1.18, viscosity at room temperature for fresh sample (Ford cup no. 2) 37.7 cP, viscosity after 11 days at room temperature 273 cP. Test for hydrogen sulphide with lead acetate paper (see example 1) negative. To 5 g of this mixture were added 10 drops (= 0.20 ml) of 9.5-molar lactic acid and 1.2 g of the same addition K as in example 1. The pH was then 8.95. Gluing for 6 min at 150°C: Firmness for air-dry birch veneer ^ ll^, <XX>17X4 kp/cm<2>. Humidity increase 4.2; 4.2%, firmness <XX>2ii2, <X>26j,5 kp/cm<2>. Firmness factor 7 out of 8 possible.
Eksempel 3 Example 3
5,8 g fenol, 6,15 ml 4 n natriumhydroksydoppløsning, 8,45 ml 35%'s formalin og 6,1 ml vann ble oppvarmet i 3 timer ved 90°C og forsynt med en tilsetning av 58,3 g svartlut med tørr-stoff innhold 55,2% samt et innhold av organisk substans på 38,6% fra sulfatcellulosekok på bjerkeved, hvoretter der ble tilsatt 9,3 ml 35%'s formalin og oppvarmet i 3 timer ved 70°C. Man til- 5.8 g of phenol, 6.15 ml of 4 N sodium hydroxide solution, 8.45 ml of 35% formalin and 6.1 ml of water were heated for 3 hours at 90°C and provided with the addition of 58.3 g of black liquor with dry matter content 55.2% and an organic substance content of 38.6% from sulphate cellulose boiling on birch wood, after which 9.3 ml of 35% formalin was added and heated for 3 hours at 70°C. Man to-
førte 21 ml vann og fikk samkokt bjerkelim L 3319 b. Tørr-stoff innholdet var 38,9% og mengden av anvendt fenol 20,5% av summen av mengdene av fenol og organisk substans i svartluten. Viskositet for ferskt lim ca. 30 cP, etter 1 døgn ved værelsetemperatur ca. 35 og etter ialt 4 3/4 døgn ca. 40 cP. Til 5 g av blandingen ble der satt 0,22 ml 16,6-molar eddiksyre og 1,2 g av tilsetning K (se eksempel 1). pH-verdien bestemt som i eksempel 1, var deretter 8,6. Liming i 6 min ved 150°C: Fasthet for lufttørr bjerkefinér <XX>13,0<XX>14 kp/cm<2>. Fuktighetsøkning 4,7; 5,5%, fasthet X X14, 7X X21, 9 kp/cm<2>. Fasthetsfaktor 8 av 8 added 21 ml of water and obtained co-boiled birch glue L 3319 b. The dry matter content was 38.9% and the amount of phenol used 20.5% of the sum of the amounts of phenol and organic substance in the black liquor. Viscosity for fresh glue approx. 30 cP, after 1 day at room temperature approx. 35 and after a total of 4 3/4 days approx. 40 cP. 0.22 ml of 16.6-molar acetic acid and 1.2 g of additive K were added to 5 g of the mixture (see example 1). The pH value, determined as in Example 1, was then 8.6. Gluing for 6 min at 150°C: Firmness for air-dry birch veneer <XX>13.0<XX>14 kp/cm<2>. Humidity increase 4.7; 5.5%, firmness X X14, 7X X21, 9 kp/cm<2>. Firmness factor 8 out of 8
mulige. possible.
Eksempel 4 Example 4
Dette eksempel ble utført på samme måte som eksempel 3, This example was carried out in the same way as example 3,
når unntas at der istedenfor 0,22 ml 16,6-molar eddiksyre ble anvendt 0,22 ml 12 n svovelsyre. pH deretter 7,5. Liming i 6 min ved 150°C: Fasthet for lufttørr bjerkefinér X12x6xx12j. 4 kp. Fuktighetsøkning 5,3; 5,3%, fasthet ^^^ S^ IS^ kp/cm<2>. Fasthetsfaktor 8 av 8 mulige. except that instead of 0.22 ml of 16.6-molar acetic acid, 0.22 ml of 12 N sulfuric acid was used. pH then 7.5. Gluing for 6 min at 150°C: Strength for air-dry birch veneer X12x6xx12j. 4 cp. Humidity increase 5.3; 5.3%, firmness ^^^ S^ IS^ kp/cm<2>. Firmness factor 8 out of 8 possible.
Eksempel 5 Example 5
(L 3301, 23 o. 24) (L 3301, 23 o. 24)
Svartlutlim: Black lute glue:
78,0 g av samme bartresvartlut som i eksempel 1 ble for- 78.0 g of the same softwood black liquor as in example 1 was prepared
synt med 12,5 ml 35%'s formalin og varmet opp i 4,5 timer ved 70°C. Der ble tilsatt 32,5 ml vann, hvoretter tørrstoffinnholdet var 36% og viskositeten på ferskt lim 30,7 cP, etter 5 døgn ved værelsetemperatur 36,6 cP, etter ytterligere 3 døgn 40,7 cP og etter 12 døgn 77,9 cP. synthesized with 12.5 ml of 35% formalin and heated for 4.5 hours at 70°C. 32.5 ml of water was added, after which the dry matter content was 36% and the viscosity of fresh glue 30.7 cP, after 5 days at room temperature 36.6 cP, after a further 3 days 40.7 cP and after 12 days 77.9 cP .
Fenollim: Phenolic glue:
57 g fenol, 53,5 ml 4 n natriumhydroksydoppløsning og 78 57 g phenol, 53.5 ml 4 N sodium hydroxide solution and 78
ml 35%'s formalin ble varmet opp i 4 timer ved 90°C. Der ble tilsatt 60 ml vann. Tørrstoffinnhold deretter.ca. 36%, viskosi- ml of 35% formalin was heated for 4 hours at 90°C. 60 ml of water was added. Dry matter content then.ca. 36%, viscosity
tet 23 døgn etter fremstillingen 146 cP. r tet 23 days after production 146 cP. r
Man blandet 4 g av svartlutlimet og 1 g av fenollimet og tilsatte deretter 0,22 ml 16,6-molar eddiksyre, 1,4 g vavanitt-kombinasjon K (se eksempel 1) og 0,2 g paraformaldehyd. pH be- 4 g of the black liquor glue and 1 g of the phenol glue were mixed and then 0.22 ml of 16.6-molar acetic acid, 1.4 g of vavanite combination K (see example 1) and 0.2 g of paraformaldehyde were added. pH be-
stemt som i eksempel 1 var deretter 7,4. Liming i 7 min ved 150°C: Fasthet for lufttørr bjerkefinér <XX>15,5<XX>20,8 kp/cm<2>. voted as in example 1 was then 7.4. Gluing for 7 min at 150°C: Firmness for air-dry birch veneer <XX>15.5<XX>20.8 kp/cm<2>.
Fuktighet 5,1; 5,3%. Fasthet deretter <XX>23,7<XX>29,9 kp/cm<2>. Fasthetsfaktor 8 av 8 mulige. Humidity 5.1; 5.3%. Firmness then <XX>23.7<XX>29.9 kp/cm<2>. Firmness factor 8 out of 8 possible.
Eksempel 6 Example 6
Dette eksempel ble utført som eksempel 5, når unntas at svartlutlimet bare ble varmet opp i 3 timer ved 70°C. Viskositet for svartlutlimet ferskt 21,8 cP, etter 5 døgn ved værelsetemperatur 24,0 cP, etter ytterligere 8 døgn 28,0 cP, 7 døgn senere 36,6 cP. Blandingslimets pH-verdi bestemt som i eksempel 1 var 7,4. Liming i 7 min ved 150°C: Fasthet for lufttørr bjerkefinér ^ll^^lj.^ kp, fuktøkning 4,8; 5,3%, fasthet deretter vy yv This example was carried out as example 5, except that the black lute glue was only heated for 3 hours at 70°C. Viscosity of the black lutic glue fresh 21.8 cP, after 5 days at room temperature 24.0 cP, after a further 8 days 28.0 cP, 7 days later 36.6 cP. The mixing adhesive's pH value determined as in example 1 was 7.4. Gluing for 7 min at 150°C: Firmness of air-dry birch veneer ^ll^^lj.^ kp, moisture increase 4.8; 5.3%, firmness then vy yv
18,8 25 kp. Fasthetsfaktor 8 av 8 mulige. 18.8 25 kp. Firmness factor 8 out of 8 possible.
Eksempel 7 Example 7
120 g fenol, 112,4 ml 4-molar natriumhydroksydoppløsning 120 g phenol, 112.4 ml 4-molar sodium hydroxide solution
og 165,6 ml 35%'s formalin ble varmet opp i 2 timer og 55 minutter ved 87°C under anvendelse av tilbakeløpskjøler. Viskositeten av det fremkomne fenollim Bj 796 var deretter 180 cP. and 165.6 ml of 35% formalin was heated for 2 hours and 55 minutes at 87°C using a reflux condenser. The viscosity of the resulting phenol glue Bj 796 was then 180 cP.
Det hadde et tørrstoffinnhold av 46,9%, og mengden av anvendt fenol var 28,1% av limets vekt. It had a solids content of 46.9%, and the amount of phenol used was 28.1% of the glue's weight.
125,7 g av fenollimet Bj 796, 208 g av sulfatsvartlut fra kok på bartre samt den svartlut som ble nevnt i eksempel 1, men med tørrstoffinnhold 53,0% og et innhold av organisk substans på 39,7%, samt 35,6 ml 35%'s formalin ble varmet opp i 1 time og 35 minutter ved 70°C under anvendelse av tilbakeløpskjøler. Viskositeten av det fremkomne lim Bj 798 var deretter 162 cP. Dette lim hadde et tørrstoffinnhold av 49,1%, og mengden av anvendt fenol var 30% av summen av mengdene av fenol og svartlutens organiske substans. 125.7 g of the phenol lime Bj 796, 208 g of sulphated black liquor from boiling on softwood as well as the black liquor that was mentioned in example 1, but with a dry matter content of 53.0% and an organic substance content of 39.7%, as well as 35.6 ml of 35% formalin was heated for 1 hour 35 minutes at 70°C using a reflux condenser. The viscosity of the resulting glue Bj 798 was then 162 cP. This glue had a solids content of 49.1%, and the amount of phenol used was 30% of the sum of the amounts of phenol and the black liquor's organic substance.
Til 5 g av limet Bj 798 ble der satt 1,2 g av en blanding av tilsetninger som inneholdt 0,64 g vavanitt, 0,40 g kritt og 0,16 g hvetemel - altså uten quebracho-ekstrakt - samt enn videre 1,2 ml 1,95-molar svovelsyre. Det beregnede tørrstoffinnhold, fråsett tilsetningsblandingen og bare medregnet vannet i den tilsatte utspedde svovelsyre, utgjorde 40,0%. pH bestemt som i eksempel 1 var 10,3. Liming i 6 min ved 150°C og et trykk av 17 kp/cm : Fasthet på tre prøver av lufttørr bjerkefinér: <xx>23,9, <xx>24,2, <xx>24,2 kp/cm<2>. Fuktøkning 5,0; 5,2%, fasthet for fuktet, limet og deretter vannbehandlet bjerkefinér <xx>28, <xx>30,2, <xx>25,8 kp/cm<2>. Fasthetsfaktor: 12 av 12 mulige. To 5 g of the glue Bj 798 was added 1.2 g of a mixture of additives containing 0.64 g of vavanite, 0.40 g of chalk and 0.16 g of wheat flour - i.e. without quebracho extract - as well as further 1, 2 ml of 1.95-molar sulfuric acid. The calculated solids content, apart from the additive mixture and only including the water in the added diluted sulfuric acid, amounted to 40.0%. pH determined as in example 1 was 10.3. Bonding for 6 min at 150°C and a pressure of 17 kp/cm : Firmness on three samples of air-dry birch veneer: <xx>23.9, <xx>24.2, <xx>24.2 kp/cm<2 >. Moisture Increase 5.0; 5.2%, firmness for moistened, glued and then water-treated birch veneer <xx>28, <xx>30.2, <xx>25.8 kp/cm<2>. Firmness factor: 12 out of 12 possible.
Eksempel 8 Example 8
Dette eksempel var maken til eksempel 7, når unntas at tilføyet 1,2 ml svovelsyre var 2,25-molar, og at tilføyet 1,2 g tilsatsmiddel inneholdt 0,3 g furubarkpulver og 0,9 g av en blanding av vavanitt, kritt og hvetemel maken til den som ble brukt i eksempel 7. pH målt som i eksempel 1 etter tilsetning av tilsatsmidlene var 9,9. Liming i 6 min ved 150°C og et trykk av 17 kp/cm 2: Fasthet for tre prøver av limet, lufttørr bjerkefinér: <xx>23,6, <xx>22,8, * x21, l kp/cm<2>. Fuktøkning 5,7%, fasthet etter behandling med vann ved værelsetemperatur <yv>25,6, xx25,9, xx23, 9 kp/cm<2>. Fas the ts f aktor 12 av 12 mulige. This example was similar to example 7, except that the added 1.2 ml of sulfuric acid was 2.25 molar, and that the added 1.2 g of additive contained 0.3 g of pine bark powder and 0.9 g of a mixture of vavanite, chalk and wheat flour the same as that used in example 7. pH measured as in example 1 after addition of the additives was 9.9. Gluing for 6 min at 150°C and a pressure of 17 kp/cm 2: Firmness for three samples of the glue, air-dry birch veneer: <xx>23.6, <xx>22.8, * x21, l kp/cm< 2>. Moisture gain 5.7%, firmness after treatment with water at room temperature <yv>25.6, xx25.9, xx23, 9 kp/cm<2>. Fas the ts f prosecutor 12 out of 12 possible.
Eksempel 9 Example 9
28,2 g fenol, 26,1 ml 4-molar natriumhydroksydoppløsning og 38,9 ml 35%'s formalin ble innført i en kolbe i et vannbad ved værelsetemperatur. Vannbadet ble varmet opp til 90°C, og limblandingen ble holdt på denne temperatur i 4 timer under anvendelse av tilbakeløpskjøler. Viskositeten for det fremkomne fenollim 3387 f var 1064 cP. Det hadde et tørrstoffinnhold av 37,0%, og mengden av anvendt fenol var 28,2% av limets vekt. 28.2 g of phenol, 26.1 ml of 4 molar sodium hydroxide solution and 38.9 ml of 35% formalin were introduced into a flask in a water bath at room temperature. The water bath was heated to 90°C and the adhesive mixture was held at this temperature for 4 hours using a reflux condenser. The viscosity of the resulting phenolic glue 3387 f was 1064 cP. It had a solids content of 37.0%, and the amount of phenol used was 28.2% of the glue's weight.
26,5 g av fenollimet 3387 f og 58,3 g sulfatsvartlut fremkommet ved kok på en blanding av ca. 65% bjerkeved og 35% bartre, lett oksydert med luft og med tørrstoffinnhold 51,8% samt et innhold av 39,0% organisk substans, ble varmet opp sammen med 10,2 ml 35%'s formalin og 14,2 ml vann i 1 time og 30 minutter ved 70°C. Det fremkomne lim 3391 b hadde en viskositet av 37 cP ved værelsetemperatur og et tørrstoffinnhold av 42,3%. Mengden av anvendt fenol var 20,3% av summen av mengdene av fenol og organisk substans i svartluten. 26.5 g of the phenol lime 3387 f and 58.3 g of sulphate black liquor obtained by boiling a mixture of approx. 65% birch wood and 35% softwood, slightly oxidized with air and with a dry matter content of 51.8% and a content of 39.0% organic matter, was heated together with 10.2 ml of 35% formalin and 14.2 ml of water for 1 hour and 30 minutes at 70°C. The resulting glue 3391 b had a viscosity of 37 cP at room temperature and a solids content of 42.3%. The amount of phenol used was 20.3% of the sum of the amounts of phenol and organic matter in the black liquor.
Til 5 g av limet 3391 b ble der føyet 1,2 g av blandingen "K" av vavanitt m.v. som i eksempel 1, og 0,38 ml 6-molar svovelsyre. pH målt som i eksempel 1 var 9,15'. Liming i 6 min ved 145°C og et trykk av 17 kp/cm2: Fasthet for to prøver på limt lufttørr bjerkefinér <xx>18,0, xx2 3j9 kp/cm<2>. Fuktøkning 9,6; 8,5%, fasthet etter behandling med vann ved værelsetempera-xx xx 2 To 5 g of the glue 3391 b was added 1.2 g of the mixture "K" of vavanite etc. as in Example 1, and 0.38 ml of 6-molar sulfuric acid. The pH measured as in example 1 was 9.15'. Gluing for 6 min at 145°C and a pressure of 17 kp/cm2: Firmness for two samples on glued air-dry birch veneer <xx>18.0, xx2 3j9 kp/cm<2>. Moisture increase 9.6; 8.5%, firmness after treatment with water at room temperature-xx xx 2
tur 30, 31,0 kp/cm . Fasthetsfaktor 8 av 8 mulige. turn 30, 31.0 kp/cm . Firmness factor 8 out of 8 possible.
Claims (1)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FI721965A FI52226C (en) | 1972-07-10 | 1972-07-10 | Process for the production of glue intended for the manufacture of veneer and particle board. |
Publications (1)
Publication Number | Publication Date |
---|---|
NO137125B true NO137125B (en) | 1977-09-26 |
Family
ID=8506478
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
NO2746/73A NO137125B (en) | 1972-07-10 | 1973-07-04 | PROCEDURES FOR THE MANUFACTURE OF ADHESIVES FOR FIBER PRODUCTS, ESPECIALLY LIGNOCELLULOSIS OR WOOD MATERIALS SUCH AS PINE AND CHIPBOARD. |
Country Status (4)
Country | Link |
---|---|
DE (1) | DE2334540A1 (en) |
FI (1) | FI52226C (en) |
GB (1) | GB1382964A (en) |
NO (1) | NO137125B (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2010127422A1 (en) * | 2009-05-08 | 2010-11-11 | Flavio Maluf | Binder extender for producing chipboards and wood fiberboards |
SE539543C2 (en) | 2015-07-03 | 2017-10-10 | Stora Enso Oyj | A method for increasing the reactivity of lignin by storage |
CN111944464B (en) * | 2020-07-02 | 2023-01-24 | 上海昶法新材料有限公司 | Modified phenolic resin adhesive and preparation method and application thereof |
-
1972
- 1972-07-10 FI FI721965A patent/FI52226C/en active
-
1973
- 1973-07-04 NO NO2746/73A patent/NO137125B/en unknown
- 1973-07-06 DE DE19732334540 patent/DE2334540A1/en active Pending
- 1973-07-10 GB GB3284373A patent/GB1382964A/en not_active Expired
Also Published As
Publication number | Publication date |
---|---|
DE2334540A1 (en) | 1974-01-24 |
FI52226B (en) | 1977-03-31 |
GB1382964A (en) | 1975-02-05 |
FI52226C (en) | 1977-07-11 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US3864291A (en) | Kraft or soda black liquor adhesive and procedure for making the same | |
Ghaffar et al. | Lignin in straw and its applications as an adhesive | |
EP3052549B1 (en) | A method for increasing the reactivity of lignin | |
US10858554B2 (en) | High residual content (HRC) kraft/soda lignin as an ingredient in wood adhesives | |
Dunky | Wood adhesives based on natural resources: a critical review: Part III. Tannin‐and lignin‐based adhesives | |
EP2922885B1 (en) | Method for producing phenol formaldehyde resin-based polymers | |
US20150210904A1 (en) | Lignin adhesive | |
US3025250A (en) | Resin composition containing alkalibark product and phenol-formaldehyde resin, and method of preparation | |
US3886101A (en) | Phenolic adhesives | |
NO137125B (en) | PROCEDURES FOR THE MANUFACTURE OF ADHESIVES FOR FIBER PRODUCTS, ESPECIALLY LIGNOCELLULOSIS OR WOOD MATERIALS SUCH AS PINE AND CHIPBOARD. | |
CN107236500A (en) | The preparation method of lignin sulfonate modified urea-phenolic resin | |
FI129275B (en) | Phenol-free impregnation resin | |
DK3219756T3 (en) | Formaldehyde-free wood binder. | |
JP7209648B2 (en) | Liquid lignin composition comprising lignin, water, alkali and urea | |
Thébault et al. | Naturally occurring phenolic sources for industrial applications | |
US4127544A (en) | Process for the partial substitution of ammonium lignosulfonate for phenol in phenolic-aldehyde resin adhesives | |
McElroy et al. | Fractionation-purification, IR, 1H 13C NMR spectral and property studies of an industrial based sludge lignin | |
NO790684L (en) | PROCEDURE FOR THE MANUFACTURE OF ARTIC RESIN FROM WASTE PRODUCTS | |
NO760226L (en) | ||
AU2018335246B2 (en) | Binder for cellulose-containing materials | |
Jenkin | Adhesives from Pinus radiata bark extractives | |
FI129050B (en) | Phenol-free tannin-formaldehyde impregnation resin | |
RU2802891C2 (en) | Aqueous adhesive composition for lignocellulose materials such as wood and method for its production | |
Abu-Ayyash et al. | Lignin Isolation from Wood by Organosolv Method | |
Campbell et al. | The chemical changes induced in wood by saturated steam under pressure |