NO152072B - PROCEDURE AND PREPARATION FOR AROMATIZATION OF TEA - Google Patents
PROCEDURE AND PREPARATION FOR AROMATIZATION OF TEA Download PDFInfo
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- NO152072B NO152072B NO810530A NO810530A NO152072B NO 152072 B NO152072 B NO 152072B NO 810530 A NO810530 A NO 810530A NO 810530 A NO810530 A NO 810530A NO 152072 B NO152072 B NO 152072B
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- Prior art keywords
- oil
- polybutadiene
- butadiene
- solution
- diene
- Prior art date
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- 238000000034 method Methods 0.000 title claims description 6
- 238000002360 preparation method Methods 0.000 title description 2
- 238000005899 aromatization reaction Methods 0.000 title 1
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 16
- 229920000578 graft copolymer Polymers 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229920002587 poly(1,3-butadiene) polymer Polymers 0.000 claims description 2
- 235000013311 vegetables Nutrition 0.000 claims description 2
- 239000003921 oil Substances 0.000 description 18
- 235000019198 oils Nutrition 0.000 description 18
- 229920002857 polybutadiene Polymers 0.000 description 16
- 239000005062 Polybutadiene Substances 0.000 description 13
- 239000000944 linseed oil Substances 0.000 description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- 235000021388 linseed oil Nutrition 0.000 description 10
- 150000001993 dienes Chemical class 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 5
- 239000002274 desiccant Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical compound C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 description 3
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 2
- RFFLAFLAYFXFSW-UHFFFAOYSA-N 1,2-dichlorobenzene Chemical compound ClC1=CC=CC=C1Cl RFFLAFLAYFXFSW-UHFFFAOYSA-N 0.000 description 2
- FRIBMENBGGCKPD-UHFFFAOYSA-N 3-(2,3-dimethoxyphenyl)prop-2-enal Chemical compound COC1=CC=CC(C=CC=O)=C1OC FRIBMENBGGCKPD-UHFFFAOYSA-N 0.000 description 2
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- 229920003051 synthetic elastomer Polymers 0.000 description 2
- 239000005061 synthetic rubber Substances 0.000 description 2
- 239000002966 varnish Substances 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 235000019482 Palm oil Nutrition 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 235000012716 cod liver oil Nutrition 0.000 description 1
- 239000003026 cod liver oil Substances 0.000 description 1
- 235000005687 corn oil Nutrition 0.000 description 1
- 239000002285 corn oil Substances 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002432 hydroperoxides Chemical class 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000013521 mastic Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000000025 natural resin Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000004006 olive oil Substances 0.000 description 1
- 235000008390 olive oil Nutrition 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002540 palm oil Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- SCUZVMOVTVSBLE-UHFFFAOYSA-N prop-2-enenitrile;styrene Chemical compound C=CC#N.C=CC1=CC=CC=C1 SCUZVMOVTVSBLE-UHFFFAOYSA-N 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 229920000638 styrene acrylonitrile Polymers 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000011269 tar Substances 0.000 description 1
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 1
- 239000002383 tung oil Substances 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- PXXNTAGJWPJAGM-UHFFFAOYSA-N vertaline Natural products C1C2C=3C=C(OC)C(OC)=CC=3OC(C=C3)=CC=C3CCC(=O)OC1CC1N2CCCC1 PXXNTAGJWPJAGM-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- -1 white spirit Chemical compound 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
- A23F3/00—Tea; Tea substitutes; Preparations thereof
- A23F3/40—Tea flavour; Tea oil; Flavouring of tea or tea extract
- A23F3/405—Flavouring with flavours other than natural tea flavour or tea oil
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
- A23F3/00—Tea; Tea substitutes; Preparations thereof
- A23F3/06—Treating tea before extraction; Preparations produced thereby
- A23F3/14—Tea preparations, e.g. using additives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/70—Fixation, conservation, or encapsulation of flavouring agents
- A23L27/75—Fixation, conservation, or encapsulation of flavouring agents the flavouring agents being bound to a host by chemical, electrical or like forces, e.g. use of precursors
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/80—Emulsions
Landscapes
- Polymers & Plastics (AREA)
- Food Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Tea And Coffee (AREA)
- Seasonings (AREA)
- Fats And Perfumes (AREA)
- Cosmetics (AREA)
- Medicines Containing Plant Substances (AREA)
- Non-Alcoholic Beverages (AREA)
- Disinfection, Sterilisation Or Deodorisation Of Air (AREA)
Description
Fremgangsmåte for fremstilling av en pode-sampolymer. Process for the preparation of a graft copolymer.
Foreliggende oppfinnelse angår en The present invention relates to a
fremgangsmåte for fremstilling av en ny type pode-sampolymer med i det vesentlige to bestanddeler, hvorav den ene er butadien. method for producing a new type of graft copolymer with essentially two components, one of which is butadiene.
Oppfinnelsen angår således en fremgangsmåte for fremstilling av en pode-sampolymer av butadien og det særegne ved fremgangsmåten i henhold til oppfinnelsen består i at en butadien-polymer bringes til å reagere med en umettet vege-tabilsk eller marin olje eller et derivat av denne ved oppvarming til en temperatur mellom 50 og 350°C. The invention thus relates to a method for producing a graft copolymer of butadiene and the peculiarity of the method according to the invention is that a butadiene polymer is made to react with an unsaturated vegetable or marine oil or a derivative thereof by heating to a temperature between 50 and 350°C.
Som eksempler på egnede umettede organiske oljer skal nevnes vegetabilske As examples of suitable unsaturated organic oils, mention should be made of vegetable oils
oljer som f. eks. linolje, soyabønneolje, pal-meolje, maisolje, tungolje eller olivenolje, derivater av disse som f. eks. dehydratisert risinusolje og marineoljer som f. eks. tor-skeleverolje eller spermolje. Uttrykket «marine oljer» skal her bety oljer som er fremstillet fra levende organismer i sjøen. oils such as linseed oil, soya bean oil, palm oil, corn oil, tung oil or olive oil, derivatives thereof such as e.g. dehydrated castor oil and marine oils such as cod liver oil or sperm oil. The term "marine oils" shall here mean oils produced from living organisms in the sea.
. Polymeren kan være polybutadien og . The polymer can be polybutadiene and
fortrinnsvis et polybutadien med i det vesentlige ikke forgrenede molekyler og fullstendig gelfritt. Polymeren kan også være en sampolymer av butadien med andre preferably a polybutadiene with substantially unbranched molecules and completely gel-free. The polymer can also be a copolymer of butadiene with others
diener som f. eks. isopren eller med olefin-monoirierer som f. eks. styren akrylnitril osv. hvor butadiendelen overskrider 50 mol-prosent. serves as e.g. isoprene or with olefin monomers such as e.g. styrene acrylonitrile etc. where the butadiene portion exceeds 50 mole percent.
De best egnede polybutadien-gummier er de som er fremstillet i oppløsning under bruk av litium-alkyl-initiatorer, et ty-pisk eksempel på disse er en dientype som The most suitable polybutadiene rubbers are those prepared in solution using lithium alkyl initiators, a typical example of which is a diene type which
er brakt på markedet av Firestone Synthetic Rubber & Latex Co. Limited. Analyse is brought to market by Firestone Synthetic Rubber & Latex Co. Limited. Analysis
'viser at denne polybutadien-type er nesten 'shows that this type of polybutadiene is almost
fullstendig uforgrenet og lineær og om-fatter tilnærmet 6—10 pst. 1,2-struktur, 30—60 pst. cis-l,4-struktur mens resten er trans-1,4-. Disse forhold avhenger helt av de forhold hvorunder polybutadienet er fremstillet, f. eks. av katalysatorkonsentra-sjonen og polymeriseringstemperaturen. completely unbranched and linear and comprises approximately 6-10% 1,2-structure, 30-60% cis-1,4-structure while the remainder is trans-1,4-. These conditions depend entirely on the conditions under which the polybutadiene is produced, e.g. of the catalyst concentration and the polymerization temperature.
Dette i det vesentlige lineære polybutadien oppløses lett i umettede oljer. Andre po-lybutadiener, f. eks. de som er fremstillet ved emulgering, inneholder en annen ste-risk struktur og er i alminnelighet ikke helt fri for gel, slik at de ikke oppløses fullt så lett. Ikke desto mindre kan det fremstilles brukbare pode-sampolymerer fra slike po-lybutadiener. This essentially linear polybutadiene dissolves readily in unsaturated oils. Other polybutadienes, e.g. those produced by emulsification contain a different steric structure and are generally not completely free of gel, so that they do not dissolve quite so easily. Nevertheless, useful graft copolymers can be prepared from such polybutadienes.
Molekylvekten for polybutadien-polymeren ligger fortrinnsvis i området 2000— 200 000, selv om høyere og lavere verdier ikke er utelukket. Mengden av olje og butadien som brukes ved fremstillingen av pode-sampolymeren ligger normalt på 5— 99 pst. olje og 95—1 pst. polybutadien. Når mengden av olje er fra 85—95 pst., er det ikke nødvendig å bruke noe ekstra oppløs-ningsmiddel. Utenfor dette område kan det imidlertid være nødvendig å bruke et opp-løsningsmiddel for å nedsette viskositeten for blandingen. Typiske oppløsningsmidler som kan brukes, er hydrokarboner eller klorerte hydrokarboner, f. eks. xylen, to-luen, white spirit, decalin, tetralin, klor-benzen, o-diklorbenzen etc. The molecular weight of the polybutadiene polymer is preferably in the range 2000-200,000, although higher and lower values are not excluded. The amount of oil and butadiene used in the production of the graft copolymer is normally 5-99 percent oil and 95-1 percent polybutadiene. When the quantity of oil is from 85-95 per cent, it is not necessary to use any additional solvent. Outside this range, however, it may be necessary to use a solvent to lower the viscosity of the mixture. Typical solvents that can be used are hydrocarbons or chlorinated hydrocarbons, e.g. xylene, toluene, white spirit, decalin, tetralin, chlorobenzene, o-dichlorobenzene etc.
For å pode ved lav temperatur, kan det være gunstig å medanvende en katalysator, f. eks. en forbindelse som danner frie ra-dikaler. Egnede katalysatorer er peroksy-der eller hydroperoksyder, f. eks. benzoyl-peroksyd, cumen-hydroperoksyd, dicumyl-peroksyd eller tertiært butyl-hydroperoksyd. In order to graft at a low temperature, it may be beneficial to co-use a catalyst, e.g. a compound that forms free radicals. Suitable catalysts are peroxides or hydroperoxides, e.g. benzoyl peroxide, cumene hydroperoxide, dicumyl peroxide or tertiary butyl hydroperoxide.
Den omstendighet at poding virkelig finner sted kan vises ved å forsøke å ekstrahere den umettede olje, f. eks. linolje, med aceton etter utførelsen av fremgangsmåten i henhold til oppfinnelsen. The fact that grafting really takes place can be shown by attempting to extract the unsaturated oil, e.g. linseed oil, with acetone after carrying out the method according to the invention.
Når det dreier seg om uomsatte blandinger med polybutadien, kan linoljen eller annen umettet olje lett ekstraheres, men etter at fremgangsmåten i henhold til oppfinnelsen er gjennomført, har det vist seg at oljen ikke kan ekstraheres fullstendig. Fra 5—50 pst. av den olje som brukes, blir normalt podet med polybutadien. Selv om noe overskudd av olje kan ekstraheres ved hjelp av aceton, slik som beskrevet, trenger slik ekstrahering normalt ikke å utføres da pode-sampolymeren i alminnelighet kan brukes med hvilket som helst overskudd av olje. When it concerns unreacted mixtures with polybutadiene, the linseed oil or other unsaturated oil can be easily extracted, but after the method according to the invention has been carried out, it has been found that the oil cannot be extracted completely. From 5 to 50 percent of the oil used is normally grafted with polybutadiene. Although some excess of oil may be extracted with acetone, as described, such extraction does not normally need to be carried out as the graft copolymer can generally be used with any excess of oil.
Infrarød analyse som karakteriserer forskjellige grupper som er tilstede i de forbindelser som reagerer, tyder også på kjemisk binding mellom de to bestanddeler. En annen antydning om at kjemisk poding har funnet sted fås ved sammen-ligning mellom filmer fremstilt fra uomsatte polybutadien-linolje-blandinger, og blandinger hvor polybutadien og linolje har reagert med hverandre. De første, med tilsatte tørkere frembringer slørede filmer, men de siste, fremstilt av blandinger som er reagert på den måten som er beskrevet, gir helt klare filmer. Evnen til å frembrin-re klare filmer er av betydning i maling-og lakkindustrien. De pode-sampolymerer som er fremstillet i henhold til oppfinnelsen, kan brukes på følgende viktige om-råder : 1. For fremstilling av fyllmasser (mastiks), kitt og dikkingsmasser. Disse meddeles da forbedret motstandsevne mot vann, ettergivenhet, styrke og klebeevne. 2. I overflatebelegg, f. eks. ved fremstilling av forbedrede alkyd-harpikser, fernisser og stoffer for å impregnere eller behandle tre. 3. Som fremstillings- og behandlings-hjelpestoffer i gummi- og plastindustrien. 4. For å forsterke syntetiske og na-turlige harpikser, f. eks. bitumen, tjære og treharpiks. Infrared analysis which characterizes different groups present in the reacting compounds also indicates chemical bonding between the two constituents. Another indication that chemical grafting has taken place is obtained by comparing films produced from unreacted polybutadiene-linseed oil mixtures, and mixtures where polybutadiene and linseed oil have reacted with each other. The former, with added driers, produce blurred films, but the latter, prepared from mixtures reacted in the manner described, produce perfectly clear films. The ability to produce clear films is important in the paint and varnish industry. The graft copolymers produced according to the invention can be used in the following important areas: 1. For the production of fillers (mastic), putty and sealing compounds. These are then given improved resistance to water, flexibility, strength and adhesiveness. 2. In surface coatings, e.g. in the manufacture of improved alkyd resins, varnishes and substances for impregnating or treating wood. 3. As manufacturing and processing aids in the rubber and plastics industry. 4. To reinforce synthetic and natural resins, e.g. bitumen, tar and wood resin.
Eksempel 1. Example 1.
10 deler «Diene» 35S, som er et polybutadien som forekommer i handelen med tilnærmet 35 ML4 Mooney viskositet ved 100°C, ble oppløst i 90 deler alkali-raffi-nert linolje ved 100°C og ga en oppløsning med viskositet 960 poise ved 20°C. Denne oppløsning ble oppvarmet til 250°C og holdt på denne temperatur i 3y2 time hvoretter viskositeten var 50 poise. Deler av denne blanding ble fortynnet med white spirit og tørkemidlet ble tilsatt (0,5 pst. bly- og 0,05 pst. kobolt-tørkemiddel regnet på ikke flyktige bestanddeler). En film dannet fra denne oppløsning var be-røringstørr etter en natt og var helt klar. En lignende film fremstillet fra blandingen før denne var oppvarmet til 250°C. 10 parts of "Diene" 35S, which is a commercially available polybutadiene of approximately 35 ML4 Mooney viscosity at 100°C, was dissolved in 90 parts of alkali-refined linseed oil at 100°C to give a solution of viscosity 960 poise at 20°C. This solution was heated to 250°C and held at this temperature for 3y2 hours after which the viscosity was 50 poise. Parts of this mixture were diluted with white spirit and the desiccant was added (0.5 per cent lead and 0.05 per cent cobalt desiccant calculated on non-volatile components). A film formed from this solution was dry to the touch after one night and was completely clear. A similar film was prepared from the mixture before it was heated to 250°C.
En del av den opprinnelige oppløsning (fra før oppvarmingen) ble behandlet med et stort overskudd aceton for å ekstrahere linoljen. Etter tre slike ekstraheringer ble den ikke oppløselige fraksjon tørket og viste seg å være i det vesentlige uendret «Diene» 35 S. Dette ble påvist ved infrarød analyse, bestemmelse av jodverdien og må-linger av viskositet. A portion of the original solution (from before heating) was treated with a large excess of acetone to extract the linseed oil. After three such extractions, the insoluble fraction was dried and proved to be essentially unchanged "Diene" 35 S. This was demonstrated by infrared analysis, determination of the iodine value and measurements of viscosity.
Etter at materialet var oppvarmet i 3y2 time ved 250°C ble det behandlet med aceton på samme måte. Etter både 6 og 12 slike ekstraheringer var den uoppløse-lige fraksjon forskjellig fra den opprinnelige polymer. Det var et oljeaktig material og det infrarøde spektrum viste at det var et reaksjonsprodukt mellom linolje og polybutadienet. After the material had been heated for 3y2 hours at 250°C, it was treated with acetone in the same way. After both 6 and 12 such extractions, the insoluble fraction was different from the original polymer. It was an oily material and the infrared spectrum showed that it was a reaction product between linseed oil and the polybutadiene.
Eksempel 2. Example 2.
10 deler «Diene» 35 S ble oppløst i 90 deler rå linolje ved 100°C. Oppløsningen ble så oppvarmet ved 250°C i en time og blandingen oppløst i white spirit. Tøfke-midler, 0,5 pst. bly- og 0,05 pst. kobolt-tørkemidler regnet på ikke flyktige bestanddeler, ble tilsatt og en film ble dannet av oppløsningen. Den var berøringstørr etter en natt og var fullstendig klar. 10 parts of "Diene" 35 S were dissolved in 90 parts of crude linseed oil at 100°C. The solution was then heated at 250°C for one hour and the mixture dissolved in white spirit. Tøfke agents, 0.5 percent lead and 0.05 percent cobalt desiccants based on non-volatile constituents, were added and a film was formed from the solution. It was touch dry after one night and was completely clear.
Eksempel 3. Example 3.
Eksempel 2 ble gjentatt under bruk av soyabønneolje i stedet for linolje. Lignende resultater ble oppnådd. Example 2 was repeated using soybean oil instead of linseed oil. Similar results were obtained.
Eksempel 4. Example 4.
Eksempel 2 ble gjentatt bortsett fra at materialet ble holdt ved 250°C inntil viskositeten'øket til 1200 poise, målt ved 20°C. Dette tok 15 timer. Lignende resultater ble oppnådd. Example 2 was repeated except that the material was held at 250°C until the viscosity increased to 1200 poise, measured at 20°C. This took 15 hours. Similar results were obtained.
Eksempel 5. 10 deler «Diene» 35 S og 90 deler linolje ble oppløst i 100 deler white spirit, en del cumen-hydroperoksyd ble tilsatt og opp-løsningen oppvarmet ved 150°C i 10 timer. Etter kjøling ble det tilsatt tørkemidler, 0,5 pst. bly- og 0,05 pst. kobolt-tørkere regnet på ikke flyktige bestanddeler og opp-løsningen ble helt ut over en glassplate. Den dannede film var berøringstørr etter en natt og var fullstendig klar. Example 5. 10 parts "Diene" 35 S and 90 parts linseed oil were dissolved in 100 parts white spirit, one part cumene hydroperoxide was added and the solution heated at 150°C for 10 hours. After cooling, drying agents were added, 0.5 percent lead and 0.05 percent cobalt driers based on non-volatile components and the solution was poured over a glass plate. The film formed was dry to the touch after one night and was completely clear.
Eksempel 6. Example 6.
Eksempel 2 ble gjentatt bortsett fra at «Diene» 35 NF, et ikke flytende polybutadien med Mooney-viskositet på tilnærmet 35 ML4 ved 100°C, ble brukt i stedet for «Diene» 35 S. Lignende resultater ble oppnådd Example 2 was repeated except that "Diene" 35 NF, a non-liquid polybutadiene having a Mooney viscosity of approximately 35 ML4 at 100°C, was used instead of "Diene" 35 S. Similar results were obtained
Eksempel 7. Example 7.
iksempel 2 ble gjentatt under bruk av en sampolymeroppløsning som inneholdt 86 pst. butadien og 14 pst. styren med grenseviskositet i benzen ved 20°C lik 1,5. Lignende resultater ble oppnådd. Example 2 was repeated using a copolymer solution containing 86% butadiene and 14% styrene with an intrinsic viscosity in benzene at 20°C of 1.5. Similar results were obtained.
Eksempel 8. Example 8.
Eksempel 2 ble gjentatt under bruk av en sampolymeroppløsning som inneholdt 99,95 pst. butadien og 0,05 pst. divinyl-benzen med grenseviskositet målt i benzen ved 20°C på 2,6. Resultater som i det vesentlige var lik de som ble oppnådd i eksempel 6, ble oppnådd. Example 2 was repeated using a copolymer solution containing 99.95% butadiene and 0.05% divinylbenzene with an intrinsic viscosity measured in benzene at 20°C of 2.6. Results substantially similar to those obtained in Example 6 were obtained.
Eksempel 9. Example 9.
Eksempel 2 ble gjentatt bortsett fra at det i stedet for «Diene» 35 S ble brukt en emulsj on-polymerisert styren-butadien-sampolymer med lav molekylvekt som forekommer i handelen under navnet «Flos-brene» LV. Denne type polymer er fremstilt av American Synthetic Rubber Corpora-tion. Lignende resultater ble oppnådd bortsett fra at filmen tørket langsommere. Example 2 was repeated except that instead of "Diene" 35 S, an emulsion-polymerized styrene-butadiene copolymer of low molecular weight was used, which appears in the trade under the name "Flos-brene" LV. This type of polymer is manufactured by the American Synthetic Rubber Corporation. Similar results were obtained except that the film dried more slowly.
Eksempel 10. 10 deler «Diene» 35 S ble oppløst i 90 deler oleinsyre ved 100°C. Denne oppløs-ning ble oppvarmet ved 250°C i 6 timer. Etter kjølingen ble blandingen helt ut i et stort overskudd av aceton. Gummi-pode-sampolymeren skilte seg ut som en uopp-løselig fraksjon. Example 10. 10 parts of "Diene" 35 S were dissolved in 90 parts of oleic acid at 100°C. This solution was heated at 250°C for 6 hours. After cooling, the mixture was poured into a large excess of acetone. The rubber graft copolymer separated as an insoluble fraction.
Claims (1)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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HU8080358A HU180556B (en) | 1980-02-18 | 1980-02-18 | Granules serving for aromatization of teas and method for producing same |
HU35980A HU180557B (en) | 1980-02-18 | 1980-02-18 | Process for improving flavour of theas |
Publications (3)
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NO810530L NO810530L (en) | 1981-08-19 |
NO152072B true NO152072B (en) | 1985-04-22 |
NO152072C NO152072C (en) | 1985-07-31 |
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NO810530A NO152072C (en) | 1980-02-18 | 1981-02-17 | PROCEDURE AND PREPARATION FOR AROMATIZATION OF TEA |
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CH (1) | CH656778A5 (en) |
CS (2) | CS250245B2 (en) |
DD (1) | DD156414A5 (en) |
DE (1) | DE3105666A1 (en) |
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SE (1) | SE450453B (en) |
SU (1) | SU1382392A3 (en) |
YU (1) | YU42716B (en) |
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NL8203963A (en) * | 1982-10-14 | 1984-05-01 | Naarden International Nv | METHOD FOR AROMATIZING DRY VEGETABLE MATERIAL |
DE3778568D1 (en) * | 1986-02-05 | 1992-06-04 | Firmenich & Cie | METHOD FOR THE FLAVORING OF TOBACCO. |
DE3883273T2 (en) * | 1987-03-26 | 1994-01-27 | Firmenich & Cie | Flavored food or spice. |
US5094860A (en) * | 1991-02-20 | 1992-03-10 | Firmenich Sa | Process for the aromatization of dry vegetable matter |
US5144964A (en) * | 1991-03-14 | 1992-09-08 | Philip Morris Incorporated | Smoking compositions containing a flavorant-release additive |
CA2245995A1 (en) * | 1997-10-23 | 1999-04-23 | Societe Des Produits Nestle S.A. | Tea bag for iced tea |
DE69716627T2 (en) * | 1997-12-23 | 2003-07-10 | I.M.A. Industria Macchine Automatiche S.P.A., Ozzano Dell'emilia | Device for granulating and / or coating solids |
GB2350047B (en) * | 1999-05-06 | 2002-07-17 | Unilever Plc | Black tea manufacture |
US6287603B1 (en) * | 1999-09-16 | 2001-09-11 | Nestec S.A. | Cyclodextrin flavor delivery systems |
AU2001265937A1 (en) * | 2000-06-30 | 2002-01-14 | Societe Des Produits Nestle S.A. | Flavouring compositions |
GB0016312D0 (en) * | 2000-07-04 | 2000-08-23 | Zylepsis Ltd | Separation method |
US6761918B2 (en) | 2002-07-18 | 2004-07-13 | Tata Tea Ltd. | Method of processing green tea leaves to produce black tea that can be brewed in cold water |
DE10240698A1 (en) | 2002-09-04 | 2004-03-18 | Symrise Gmbh & Co. Kg | cyclodextrin particles |
DE102004036187A1 (en) * | 2004-07-26 | 2006-03-23 | Symrise Gmbh & Co. Kg | Tea Flavoring |
EA012674B1 (en) | 2005-04-29 | 2009-12-30 | Филип Моррис Продактс С.А. | Tobacco pouch product |
US9044049B2 (en) | 2005-04-29 | 2015-06-02 | Philip Morris Usa Inc. | Tobacco pouch product |
US8685478B2 (en) | 2005-11-21 | 2014-04-01 | Philip Morris Usa Inc. | Flavor pouch |
US20090185985A1 (en) * | 2006-06-13 | 2009-07-23 | Cargill, Incorporated | Large-particle cyclodextrin inclusion complexes and methods of preparing same |
US8616221B2 (en) | 2007-02-28 | 2013-12-31 | Philip Morris Usa Inc. | Oral pouch product with flavored wrapper |
US9888712B2 (en) | 2007-06-08 | 2018-02-13 | Philip Morris Usa Inc. | Oral pouch products including a liner and tobacco beads |
WO2009010876A2 (en) | 2007-07-16 | 2009-01-22 | Philip Morris Products S.A. | Oral pouch product having soft edge and method of making |
US8424541B2 (en) | 2007-07-16 | 2013-04-23 | Philip Morris Usa Inc. | Tobacco-free oral flavor delivery pouch product |
WO2009010881A2 (en) * | 2007-07-16 | 2009-01-22 | Philip Morris Products S.A. | Oral pouch products with immobilized flavorant particles |
US8119173B2 (en) | 2007-07-16 | 2012-02-21 | Philip Morris Usa Inc. | Method of flavor encapsulation through the use of a drum coater |
US8377215B2 (en) | 2008-12-18 | 2013-02-19 | Philip Morris Usa Inc. | Moist botanical pouch processing |
US8863755B2 (en) | 2009-02-27 | 2014-10-21 | Philip Morris Usa Inc. | Controlled flavor release tobacco pouch products and methods of making |
GB2471303A (en) | 2009-06-24 | 2010-12-29 | Bell Flavors & Fragrances Duft Und Aroma Gmbh | Microparticles and method of making microparticles |
US8747562B2 (en) | 2009-10-09 | 2014-06-10 | Philip Morris Usa Inc. | Tobacco-free pouched product containing flavor beads providing immediate and long lasting flavor release |
JP6093693B2 (en) | 2010-04-12 | 2017-03-08 | アルトリア クライアント サービシーズ エルエルシー | Bag product with improved seal and method of manufacturing |
US9428328B2 (en) | 2011-09-01 | 2016-08-30 | 2266170 Ontario Inc. | Beverage capsule |
EP2730523B1 (en) | 2012-11-12 | 2016-04-06 | 2266170 Ontario, Inc. | Beverage capsule and process and system for making same |
EP2981198A4 (en) | 2013-04-03 | 2016-11-16 | 2266170 Ontario Inc | Capsule machine and components |
WO2014186897A1 (en) | 2013-05-23 | 2014-11-27 | 2266170 Ontario Inc. | Capsule housing |
WO2015024125A1 (en) | 2013-08-20 | 2015-02-26 | 2266170 Ontario Inc. | A capsule containing a dosing agent and system and process for making same |
US10314319B2 (en) | 2013-11-20 | 2019-06-11 | 2266170 Ontario Inc. | Method and apparatus for accelerated or controlled degassing of roasted coffee |
CA2943295C (en) | 2014-03-21 | 2022-06-28 | 2266170 Ontario Inc. | Capsule with steeping chamber |
CN114449898A (en) * | 2019-09-30 | 2022-05-06 | 三得利控股株式会社 | Solid composition with floral aroma |
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US3528819A (en) * | 1967-02-16 | 1970-09-15 | Cpc International Inc | Eliminating undesirable taste from coffee and tea extracts and products |
JPS5644905B2 (en) * | 1973-11-26 | 1981-10-22 | ||
GB1564001A (en) * | 1975-10-24 | 1980-04-02 | Unilever Ltd | Beverge compositions |
HU174699B (en) * | 1977-07-01 | 1980-03-28 | Chinoin Gyogyszer Es Vegyeszet | Process for preparing cyclodextrin inclusion complexes of natural and synthetic spices, aromatic and flavoring materials |
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1981
- 1981-02-13 CS CS85269A patent/CS250245B2/en unknown
- 1981-02-13 CS CS811045A patent/CS250209B2/en unknown
- 1981-02-13 YU YU373/81A patent/YU42716B/en unknown
- 1981-02-13 FI FI810466A patent/FI67168C/en not_active IP Right Cessation
- 1981-02-17 FR FR8103077A patent/FR2475858A1/en active Granted
- 1981-02-17 SE SE8101071A patent/SE450453B/en not_active IP Right Cessation
- 1981-02-17 GB GB8104949A patent/GB2074838B/en not_active Expired
- 1981-02-17 NO NO810530A patent/NO152072C/en unknown
- 1981-02-17 DE DE19813105666 patent/DE3105666A1/en not_active Withdrawn
- 1981-02-17 CA CA000371020A patent/CA1168090A/en not_active Expired
- 1981-02-17 PL PL1981229721A patent/PL125711B1/en unknown
- 1981-02-17 DK DK069481A patent/DK158763C/en not_active IP Right Cessation
- 1981-02-17 NL NL8100763A patent/NL8100763A/en not_active Application Discontinuation
- 1981-02-18 SU SU813251307A patent/SU1382392A3/en active
- 1981-02-18 DD DD81227712A patent/DD156414A5/en not_active IP Right Cessation
- 1981-02-18 ES ES500423A patent/ES500423A0/en active Granted
- 1981-02-18 LU LU83149A patent/LU83149A1/en unknown
- 1981-02-18 CH CH1072/81A patent/CH656778A5/en not_active IP Right Cessation
- 1981-06-02 FR FR8110896A patent/FR2484205A1/en active Granted
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PL125711B1 (en) | 1983-06-30 |
DD156414A5 (en) | 1982-08-25 |
SU1382392A3 (en) | 1988-03-15 |
NO810530L (en) | 1981-08-19 |
DK158763B (en) | 1990-07-16 |
FR2475858A1 (en) | 1981-08-21 |
NO152072C (en) | 1985-07-31 |
GB2074838B (en) | 1983-11-09 |
CH656778A5 (en) | 1986-07-31 |
CS250245B2 (en) | 1987-04-16 |
FI810446L (en) | 1981-08-19 |
FR2484205B1 (en) | 1984-04-27 |
FR2484205A1 (en) | 1981-12-18 |
NL8100763A (en) | 1981-09-16 |
CA1168090A (en) | 1984-05-29 |
FI67168B (en) | 1984-10-31 |
ES8201406A1 (en) | 1982-01-16 |
GB2074838A (en) | 1981-11-11 |
PL229721A1 (en) | 1981-10-30 |
FR2475858B1 (en) | 1985-03-29 |
CS250209B2 (en) | 1987-04-16 |
ES500423A0 (en) | 1982-01-16 |
YU37381A (en) | 1984-02-29 |
DK69481A (en) | 1981-08-19 |
FI67168C (en) | 1985-02-11 |
DK158763C (en) | 1990-12-17 |
LU83149A1 (en) | 1981-06-05 |
YU42716B (en) | 1988-12-31 |
DE3105666A1 (en) | 1982-01-07 |
SE8101071L (en) | 1981-08-19 |
SE450453B (en) | 1987-06-29 |
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