NO156227B - PROCEDURE FOR TRANSFERING DATA IN LARGE WATER DEPTHS. - Google Patents
PROCEDURE FOR TRANSFERING DATA IN LARGE WATER DEPTHS. Download PDFInfo
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- NO156227B NO156227B NO810415A NO810415A NO156227B NO 156227 B NO156227 B NO 156227B NO 810415 A NO810415 A NO 810415A NO 810415 A NO810415 A NO 810415A NO 156227 B NO156227 B NO 156227B
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- 238000000034 method Methods 0.000 title claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title description 7
- 239000000203 mixture Substances 0.000 claims description 10
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 8
- 238000009833 condensation Methods 0.000 claims description 8
- 230000005494 condensation Effects 0.000 claims description 8
- GUOSQNAUYHMCRU-UHFFFAOYSA-N 11-Aminoundecanoic acid Chemical compound NCCCCCCCCCCC(O)=O GUOSQNAUYHMCRU-UHFFFAOYSA-N 0.000 claims description 7
- SLXKOJJOQWFEFD-UHFFFAOYSA-N 6-aminohexanoic acid Chemical compound NCCCCCC(O)=O SLXKOJJOQWFEFD-UHFFFAOYSA-N 0.000 claims description 5
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 claims description 4
- 150000001413 amino acids Chemical class 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 150000003951 lactams Chemical class 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- -1 aliphatic diamine Chemical class 0.000 description 9
- 150000004985 diamines Chemical class 0.000 description 9
- 230000008018 melting Effects 0.000 description 8
- 238000002844 melting Methods 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- 229920002292 Nylon 6 Polymers 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 235000011037 adipic acid Nutrition 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 229960002684 aminocaproic acid Drugs 0.000 description 3
- 150000001735 carboxylic acids Chemical class 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000006068 polycondensation reaction Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- KXDAEFPNCMNJSK-UHFFFAOYSA-N Benzamide Chemical compound NC(=O)C1=CC=CC=C1 KXDAEFPNCMNJSK-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 239000001361 adipic acid Substances 0.000 description 2
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001991 dicarboxylic acids Chemical class 0.000 description 2
- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- UFFRSDWQMJYQNE-UHFFFAOYSA-N 6-azaniumylhexylazanium;hexanedioate Chemical compound [NH3+]CCCCCC[NH3+].[O-]C(=O)CCCCC([O-])=O UFFRSDWQMJYQNE-UHFFFAOYSA-N 0.000 description 1
- ITIONVBQFUNVJV-UHFFFAOYSA-N Etomidoline Chemical compound C12=CC=CC=C2C(=O)N(CC)C1NC(C=C1)=CC=C1OCCN1CCCCC1 ITIONVBQFUNVJV-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical class Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 229920000571 Nylon 11 Polymers 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 125000005521 carbonamide group Chemical class 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229940006198 sodium phenylacetate Drugs 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04L—TRANSMISSION OF DIGITAL INFORMATION, e.g. TELEGRAPHIC COMMUNICATION
- H04L5/00—Arrangements affording multiple use of the transmission path
- H04L5/22—Arrangements affording multiple use of the transmission path using time-division multiplexing
- H04L5/26—Arrangements affording multiple use of the transmission path using time-division multiplexing combined with the use of different frequencies
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- Engineering & Computer Science (AREA)
- Signal Processing (AREA)
- Computer Networks & Wireless Communication (AREA)
- Selective Calling Equipment (AREA)
- Cable Transmission Systems, Equalization Of Radio And Reduction Of Echo (AREA)
- Lubricants (AREA)
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- Magnetic Resonance Imaging Apparatus (AREA)
Description
Fremgangsmåte til fremstilling av transparente polykondensater. Process for the production of transparent polycondensates.
Ifølge en tidligere foreslått fremgangsmåte som er omtalt i patent nr. 104 601 kan man polykondensere 3-(aminometyl)-3,5,5-trimetyl-cykloheksylamin i det følgende for korthets skyld «ringdiamin» med dikarbon-syrer, fortrinnsvis adipinsyre. De herved dannede produkter viser ved siden av meget gode egenskaper, som f. eks. overflatehårdhet en rekke av egenskaper som for-styrrer for de vanlige anvendelsesformål. Spesielt må her det høye mykningsintervall nevnes som vanskeliggjør sterkt en forar-beidelse av polykondensatet under de vanlige arbeidsbetingelser. According to a previously proposed method which is mentioned in patent no. 104 601, 3-(aminomethyl)-3,5,5-trimethyl-cyclohexylamine, hereinafter referred to as "ring diamine" for brevity, can be polycondensed with dicarboxylic acids, preferably adipic acid. The products formed in this way also show very good properties, such as e.g. surface hardness a number of properties which interfere with the usual application purposes. In particular, the high softening interval must be mentioned here, which greatly complicates the processing of the polycondensate under normal working conditions.
De ovenfor nevnte polykondensaters høye mykningsintervall kan imidlertid However, the high softening interval of the above-mentioned polycondensates can
sterkt senkes ved at man under de samme reaksjonsbetingelser gjennomfører en blan-dingskondensasjon, hvori ringdiaminet del-vis erstattes med et rettlinjet alifatisk dia-min med to til 10 karbonatomer, fortrinnsvis heksametylendiamin. Det fremkommer polykondensater med praktisk talt samme overflatehårdhet og transparens som ved de i innledningen nevnte produkter. is greatly lowered by carrying out a mixture condensation under the same reaction conditions, in which the ring diamine is partially replaced by a linear aliphatic diamine with two to 10 carbon atoms, preferably hexamethylenediamine. Polycondensates are produced with practically the same surface hardness and transparency as with the products mentioned in the introduction.
Det er nu blitt funnet at man betrak-telig kan forbedre egenskapene av polykondensatet av ringdiaminet og dikarbon-syren når man gjennomfører blandingskondensas j onen med aminosyrer som e-aminokapronsyre eller 11-aminoundekan-syre. Begrepet dikarbonsyre omfatter såvel alifatiske som adipinsyre eller sebasinsyre, deres en- eller flere ganger metylerte deri-vater, som også aromatiske dikartoonsyrer, såvel som blandinger av de ovenfor nevnte. Disse blandingskondensas joners produkter har ennu meget større overflatehårdheter enn blandingskondensatene av ringdiamin-adipinsyrer med heksametylendiamin-adipinsyre. Blandingskondensasj onen med z-amino-kapronsyre gjennomfører man hen-siktsmessig med s-kaprolaktam under hjelp av de vanlige kondensasjonsmidler, som f. eks. alkalimetaller-, -hydroksyder, -alkoholater, -karbonater, -hydrider, alka-likaprolaktam eller også alkalisaltene av ustabile karbonsyrer (f. eks. natriumfenyl-acetat) og metallorganiske forbindelser med eller uten tilsetning av kokatalysatorer, som f. eks. amider, imider, isocyanater, an-hydrider osv. (se Houben-Weyl, Methoden der organischen Chemie, 4.A., Bind 14/2, side 115; Stuttgart 1963). It has now been found that the properties of the polycondensate of the ring diamine and the dicarboxylic acid can be considerably improved when the mixed condensation is carried out with amino acids such as ε-aminocaproic acid or 11-aminoundecanoic acid. The term dicarboxylic acid includes aliphatic as well as adipic or sebacic acid, their single or multiple methylated derivatives, as well as aromatic dicartoic acids, as well as mixtures of the aforementioned. The products of these mixed condensates have even much greater surface hardness than the mixed condensates of ring diamine adipic acids with hexamethylenediamine adipic acid. The mixture condensation with z-amino-caproic acid is conveniently carried out with s-caprolactam using the usual condensation agents, such as e.g. alkali metals, hydroxides, alcoholates, carbonates, hydrides, alka-lycaprolactam or also the alkali salts of unstable carboxylic acids (e.g. sodium phenylacetate) and organometallic compounds with or without the addition of cocatalysts, such as e.g. amides, imides, isocyanates, anhydrides, etc. (see Houben-Weyl, Methoden der organischen Chemie, 4.A., Volume 14/2, page 115; Stuttgart 1963).
Man kan arbeide med eller uten opp-løsningsmidler (aromatiske eller alifatiske hydrokarboner eller også vann), eventuelt under tilsetning av de vanlige stabilisato-rer eller kj edeavforytere som f. eks. mono-funksjonelle karbonsyrer eller aminer. Ved reaksjoner i vannfritt medium er det mulig som katalysatorer f. eks. å tilsette aminer, karbonsyrer, ammoniumsalter (f. eks. ammoniumklorid) eller saltsure salter av karbonamider (f. eks. av urinstoff, kaprolaktam eller benzamid) under tilsetning av et dikarbonsurt ringdiamin. Eventuelt kan man blandingskondensere allerede ferdig polykaprolaktam, i handelen kjent som Ny-lon 6, med et dikarbonsurt ringdiamin og en dikarbonsyre ved at man oppvarmer denne blanding i en time til slutt i vakuum inntil ca. IO-<2> torr i smeltestrøm. Selvsagt kan man ved blandingskondensasj onen og-så gå ut fra den frie e-aminokapronsyre. Ved blandingskondensas j onen med 11-amino-undekansyre kan man gå frem så-ledes at man eventuelt omsetter ferdig po-lyamid 11 med dikarbonsyre — ringdiamin. Også i fast fase (under ca. 200° C) lar blandingspolymerisasjonen seg gjennomfø-re. Likeledes i oppløsnlngsmidler som f. eks. i aromatiske eller alifatiske hydrokarboner under blandingspolyamidets smeltepunkt, idet disse utskiller seg pulverformet. You can work with or without solvents (aromatic or aliphatic hydrocarbons or also water), possibly with the addition of the usual stabilizers or chain de-furriers such as e.g. mono-functional carboxylic acids or amines. For reactions in an anhydrous medium, it is possible as catalysts, e.g. adding amines, carboxylic acids, ammonium salts (eg ammonium chloride) or hydrochloric acid salts of carbonamides (eg urea, caprolactam or benzamide) while adding a dicarboxylic ring diamine. Alternatively, ready-made polycaprolactam, known in the trade as Nylon 6, can be mixed-condensed with a dicarboxylic acid ring diamine and a dicarboxylic acid by heating this mixture for an hour, finally in a vacuum until approx. IO-<2> dry in melt flow. Of course, in the case of mixed condensation, you can also proceed from the free ε-aminocaproic acid. In the case of the mixed condensation with 11-amino-undecanoic acid, one can proceed in such a way that one optionally reacts finished polyamide 11 with dicarboxylic acid — ring diamine. The mixture polymerization can also be carried out in the solid phase (below approx. 200° C). Likewise in solvents such as e.g. in aromatic or aliphatic hydrocarbons below the melting point of the mixed polyamide, as these separate in powder form.
Til dikarbonsure ringdiaminer kan man sette e-aminokapronsyre og/eller 11-amino-undekansyre i polymer eller mono-molekylær form — for e-aminokapronsyre også kaprolaktam — i mengder inntil ca. To dicarboxylic acid ring diamines, e-aminocaproic acid and/or 11-amino-undecanoic acid can be added in polymer or mono-molecular form — for e-aminocaproic acid also caprolactam — in amounts up to approx.
60 pst. uten at polykondensatets glassaktige karakter går tapt. Selv ved overskridelse av disse mengder, eksempelvis til 80 pst., får man alltid ennu tydeligere effekter; som nedre grense skal den tilsatte mengde van-ligvis ikke underskride 2 pst. Selvsagt kan det i steden for dikarbonsure rene diami-ner også anvendes dikarbonsyre og ringdiamin uten tidligere isolering av saltet som danner seg av begge komponenter. Det er likeledes mulig i steden for de frie di-karbonsyrer å anvende estere eller halv-estere, eller også syrehalogenider eller 60 percent without the polycondensate's glassy character being lost. Even if these quantities are exceeded, for example to 80 per cent, you always get even clearer effects; as a lower limit, the added quantity should usually not fall below 2 percent. Of course, instead of pure dicarboxylic acid diamines, dicarboxylic acid and ring diamine can also be used without prior isolation of the salt formed from both components. It is also possible to use esters or half-esters instead of the free dicarboxylic acids, or also acid halides or
-amider. -amides.
Polykondensas j onens g j ennomf øring foregår under de vanlige betingelser om-trent på følgende måte: Man oppvarmer eksempelvis kaprolaktam med et kondensasjonsmiddel (f. eks. etznatron) til temperaturer fra 170 til 300° C, fortrinnvis 240 til 280° C, og tilset-ter etterat det øyensynlig er inntrådt en viskositetsøkning av smeiten det dikarbonsure 3- (aminometyl) -3,5,5-trimetyl-cyklo-heksylamin og viderekondenserer til slutt i vakuum. Selvsagt kan også dikarbonsyre og ringdiamin tilsettes etter hverandre. På kjent måte kan aminer eller syrer anvendes for dannelse av endegrupperinger. The polycondensation is carried out under the usual conditions in approximately the following way: For example, caprolactam is heated with a condensing agent (e.g. caustic soda) to temperatures from 170 to 300° C, preferably 240 to 280° C, and added - after an apparent increase in the viscosity of the melt has occurred, the dicarboxylic acid 3-(aminomethyl)-3,5,5-trimethyl-cyclohexylamine and finally condenses further in vacuum. Of course, dicarboxylic acid and ring diamine can also be added one after the other. On known way, amines or acids can be used to form end groups.
For nærmere forklaring av fremgangs-måten ifølge oppfinnelsen skal det angis noen eksempler hvori resultatene av de en-kelte polykondensasjoner er sammenfattet tabellarisk. Som grad for molvekten angis den reduserte spesifike viskositet ( r\ red) som måles som 1 pst.-ig oppløsning i ren maursyre ved 20° C. For a more detailed explanation of the method according to the invention, some examples shall be given in which the results of the individual polycondensations are summarized in tabular form. As a measure of the molecular weight, the reduced specific viscosity (r\red) is given, which is measured as a 1% solution in pure formic acid at 20°C.
Kuletrykkhårdheten bestemmes ifølge DIN 57302 (kulediameter 5 mm, prøvelast 50 kg). Det angis den første verdi som inn-stiller seg («0 sek.») som kuletrykkhårdhet i eksemplene. The ball compressive hardness is determined according to DIN 57302 (ball diameter 5 mm, test load 50 kg). The first value that sets ("0 sec.") is indicated as ball pressure hardness in the examples.
Til bestemmelse av mykningsinterval-let blir en ca. knappenålshodestor prøve av det material som skal undersøkes bragt mellom et varmemikroskops to dekkglass med 100 ganger forstørrelse. Prøven opp-varmes til ca. 20° C under den antatte myk-ningsibegynnelse, og nu foretas under sta-dig iakttagelse gjennom okulare på varme-bordet en temperaturøkning på ca. 1—2° C/min. Som begynnelse for mykningsinter-vallet gjelder den første synlige smeltning og som øvre grense prøvens. fullstendige fly tendegj øring. To determine the softening interval, an approx. pinhead-sized sample of the material to be examined placed between two coverslips of a heating microscope with 100 times magnification. The sample is heated to approx. 20° C below the assumed beginning of softening, and now, under constant observation through eyepieces on the heating table, a temperature increase of approx. 1-2° C/min. The first visible melting applies as the beginning of the softening interval and as the upper limit of the sample. complete aircraft tending.
Eksempel 1. Example 1.
50 g kaprolaktam ble i en rundkolbe med tilbakeløpsrør og rørverk oppvarmet under nitrogen til 270° C og blandet med 0,2 pst. fast etznatron. Smeltens viskositet økte nu hurtig. Etter ca. 5 minutter fore-gikk tilsteningen av et salt av adipinsyre og 3- (aminometyl)-3,5,5-trlmetyl-cyklo-heksylamin (i tabellen kort kalt A-R-salt). Det dannet seg en gjennomsiktig smelte. Under omrøring ble det nu oppvarmet i 4 timer under nitrogen ved 230—240° C og deretter i 7 timer ved 250—260° C og 12 mm Hg ble det dannede reaksjonsvann fjernet. 50 g of caprolactam were heated under nitrogen to 270° C. in a round flask with a reflux tube and piping and mixed with 0.2 percent solid caustic soda. The viscosity of the melt now increased rapidly. After approx. After 5 minutes, the solidification of a salt of adipic acid and 3-(aminomethyl)-3,5,5-trimethylcyclohexylamine (abbreviated as A-R salt in the table) took place. A transparent melt formed. With stirring, it was now heated for 4 hours under nitrogen at 230-240° C and then for 7 hours at 250-260° C and 12 mm Hg, the formed water of reaction was removed.
Noen fysikalske verdier av de dannede kondensater fremgår av følgende tabell. Some physical values of the condensates formed appear in the following table.
Eksempel 2. Example 2.
50 g polykaprolaktam (rj-red-verdi 1,25, smeltepunkt 222—224° C) oppvarmet man med A-R-salt under omrøring og under nitrogen i 5 timer ved 230—240° C i en 50 g of polycaprolactam (rj-red value 1.25, melting point 222-224° C) was heated with A-R salt while stirring and under nitrogen for 5 hours at 230-240° C in a
rundkolbe. Reaksjonsvannet ble deretter fjernet ved 12 mm Hg og 250—260° C bad-temperatur i løpet av 8 timer. round flask. The reaction water was then removed at 12 mm Hg and 250-260° C bath temperature during 8 hours.
De dannede kondensater har følgende verdier: The condensates formed have the following values:
Eksempel 3a. 20 g e-kaprolaktam og 0,02 g pulverisert etznatron ble oppvarmet under nitrogen ved ca. 220° C og etter noen minutter tilsatt 10 g salt av tereftalsyre og ringdiamin (smeltepunkt 226° C). Etter 9 timers reaksjonstid anla man i løpet av ytterligere 9 timer et vakuum på 14 mm g og øket tem-peraturen til 240° C. Nu var det dannet et polykondensat som hadde et mykningsin-terval på 63—172° C, en kuletrykkhårdhet på 1608 og en ^-red på 0,56. Example 3a. 20 g of ε-caprolactam and 0.02 g of powdered caustic soda were heated under nitrogen at approx. 220° C and after a few minutes added 10 g salt of terephthalic acid and ring diamine (melting point 226° C). After a reaction time of 9 hours, a vacuum of 14 mm g was applied during a further 9 hours and the temperature was increased to 240° C. Now a polycondensate had formed which had a softening interval of 63-172° C, a bullet pressure hardness of 1608 and a ^-red of 0.56.
Eksempel 3b. Example 3b.
Ved anvendelse av 28,5 g e-kaprolaktam, 0,02 g pulverisert etznatron og 1,5 g tereftalsurt ringdiamin, kondensert under forøvrig samme betingelser som angitt under eksempel 3a, oppstod et polykondensat med mykningsintervall på 185—215° C, kuletrykkhårdhet på 1248 og t| red-verdi på 0,84. By using 28.5 g of ε-caprolactam, 0.02 g of powdered caustic soda and 1.5 g of terephthalic acid ring diamine, condensed under otherwise the same conditions as stated under example 3a, a polycondensate with a softening interval of 185-215° C, bullet pressure hardness of 1248 and t| red value of 0.84.
Eksempel 4. Example 4.
En blanding av salter av 10 g 2-metyl-adipinsurt ringdiamin (smeltepunkt 195°C) og 10 g sebacinsurt ringdiamin (smeltepunkt 152° C) ble forkondensert med 10 g e-kaprolaktam under tilsetning av 30 cm3 vann i 9 timer ved 200° C under nitrogen og deretter oppvarmet ytterligere 9 timer ved 220° C ved et vakuum på 20 mm Hg. Deretter var det dannet et kondensat som hadde et mykningsintervall på 87—167° C. en kuletrykkhårdhet på 1447 og en t) red-verdi på 0,86. Eksempel 5. 10 g 11-amino-undekansyre, 20 g A-R-salt og 10 cm<3> vann oppvarmet man i 10 timer under nitrogen under tilbakeløp ved 200° C og deretter i 8 timer ved 220° C under anlegg av et vakuum på 16 mm Hg. Det var dannet et kunststoff som hadde et smelteområde på 121—185° C, en kuletrykkhårdhet på 1253 og en t| red-verdi på 1,27. A mixture of salts of 10 g of 2-methyl-adipic acid ring diamine (melting point 195°C) and 10 g sebacic acid ring diamine (melting point 152° C) was precondensed with 10 g of ε-caprolactam while adding 30 cm3 of water for 9 hours at 200° C under nitrogen and then heated for an additional 9 hours at 220° C. under a vacuum of 20 mm Hg. Subsequently, a condensate had formed which had a softening range of 87-167° C., a bullet pressure hardness of 1447 and a t) red value of 0.86. Example 5. 10 g of 11-amino-undecanoic acid, 20 g of A-R salt and 10 cm<3> of water were heated for 10 hours under nitrogen under reflux at 200° C and then for 8 hours at 220° C under a vacuum of 16 mm Hg. A plastic had been formed which had a melting range of 121-185° C, a bullet pressure hardness of 1253 and a t| red value of 1.27.
Eksempel 6. Example 6.
En blanding av 10 g poly-ll-amino-undekansyre, 10 g A-R-salt, 5,3 g tereftal-syredimetylester og 4,7 g ringdiamin ble . oppvarmet under tilsetning av 10 cm<3> vann i 9 timer under nitrogen og tilbakeløpt ved 200° C. Deretter førte man polykondensa-sjonen videre ved anlegg av et vakuum på 20 mm Hg ved 220° C i løpet av 8 timer. Nu var det dannet et kondensat, som hadde en kuletrykkhårdhet på 1632, et smelteområde på 103—214° C og en ti red-verdi på 0,87. A mixture of 10 g of poly-11-amino-undecanoic acid, 10 g of A-R salt, 5.3 g of terephthalic acid dimethyl ester and 4.7 g of ring diamine was . heated with the addition of 10 cm<3> of water for 9 hours under nitrogen and refluxed at 200° C. The polycondensation was then carried on by applying a vacuum of 20 mm Hg at 220° C for 8 hours. Now a condensate had formed, which had a bullet pressure hardness of 1632, a melting range of 103-214° C and a ti red value of 0.87.
Claims (2)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE3004981A DE3004981C2 (en) | 1980-02-11 | 1980-02-11 | Method for data transmission in great water depths |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| NO810415L NO810415L (en) | 1981-08-12 |
| NO156227B true NO156227B (en) | 1987-05-04 |
| NO156227C NO156227C (en) | 1987-08-19 |
Family
ID=6094285
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| NO810415A NO156227C (en) | 1980-02-11 | 1981-02-06 | PROCEDURE FOR TRANSFERING DATA IN LARGE WATER DEPTHS. |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP0033844B1 (en) |
| DE (1) | DE3004981C2 (en) |
| NO (1) | NO156227C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2377131B (en) * | 2001-04-23 | 2006-01-25 | Schlumberger Holdings | Subsea communication systems and techniques |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AT197904B (en) * | 1955-11-22 | 1958-05-27 | Landis & Gyr Ag | Device for superimposing audio-frequency control pulses on power distribution networks |
| AR205086A1 (en) * | 1972-08-28 | 1976-04-05 | Ibm | COMMUNICATION DEVICE WITH A CENTRAL STATION AND A PLURALITY OF REMOTE STATIONS |
| CA1053343A (en) * | 1976-03-19 | 1979-04-24 | Canadian Rgl Electronics | Electrical data collecting device |
| US4069392A (en) * | 1976-11-01 | 1978-01-17 | Incorporated Bell Telephone Laboratories | Dual speed full duplex data transmission |
| JPS6028424B2 (en) * | 1977-04-25 | 1985-07-04 | ケイディディ株式会社 | Transmission speed switching method |
-
1980
- 1980-02-11 DE DE3004981A patent/DE3004981C2/en not_active Expired
-
1981
- 1981-01-12 EP EP81100156A patent/EP0033844B1/en not_active Expired
- 1981-02-06 NO NO810415A patent/NO156227C/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| DE3004981A1 (en) | 1981-08-20 |
| NO156227C (en) | 1987-08-19 |
| DE3004981C2 (en) | 1981-10-29 |
| EP0033844B1 (en) | 1985-07-31 |
| NO810415L (en) | 1981-08-12 |
| EP0033844A1 (en) | 1981-08-19 |
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