PL104515B1 - METHOD OF PRODUCING A STABLE SUSPENSION OF MOLYBDENE AND GRAPHITE SULFACE - Google Patents

METHOD OF PRODUCING A STABLE SUSPENSION OF MOLYBDENE AND GRAPHITE SULFACE Download PDF

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Publication number
PL104515B1
PL104515B1 PL1976193695A PL19369576A PL104515B1 PL 104515 B1 PL104515 B1 PL 104515B1 PL 1976193695 A PL1976193695 A PL 1976193695A PL 19369576 A PL19369576 A PL 19369576A PL 104515 B1 PL104515 B1 PL 104515B1
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Poland
Prior art keywords
graphite
suspension
molybdenum disulfide
grinding
producing
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PL1976193695A
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Polish (pl)
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PL193695A1 (en
Inventor
Franciszek Steinmec
Stefan Patzan
Wlodzimierz Montewski
Anna Zajezierska
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Inst Technologii Nafty
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Priority to PL1976193695A priority Critical patent/PL104515B1/en
Publication of PL193695A1 publication Critical patent/PL193695A1/en
Publication of PL104515B1 publication Critical patent/PL104515B1/en

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Description

Przedmiotem wynalazku jest sposób wytwatrzania stabilnej suspensji dwusiarczku molibdemu i grafitu w cieklym oleofilnym osrodku. Wedlug znanych metod suspensje dwusiarczku molibdenu i grafitu wytwarzane sa w procesie dwuetapowym.W pierwszym etapie proszek dwusiarczku molibdenu i grafitu poddaje sie procesowi wstepnego mielenia.Mielenie prowadzi sie do uzyskania proszku o srednicy ziaren ponizej 100 m, w niektórych metodach rzedu 2/im, stosujac technike separacji dla wydzielenia frakcji o zadanej srednicy ziaren.W drugim etapie tak wytworzony proszek, poddaje sie procesowi mielenia w zawiesinie w cieklym osrodku.Ze wzgledu na wystepowanie zjawiska aglomeracji ziaren dwusiarczku molibdenu i grafitu, konieczne jest stoso¬ wanie w trakcie mielenia dodatku stabilizatorów suspensji. Mielenie w zawiesinie w osrodku cieklym w obecnosci stabilizatorów prowadzi sie do uzyskania ziaren o srednicy zapewniajacej wytworzenie sie równowagi sedymenta¬ cyjnej, zazwyczaj ponizej 1 /im.W charakterze'stabilizatorów suspensji stosowane sa substancje wykazujace zdolnosc selektywnego adsorbo- wania sie na powierzchni ziaren dwusiarczku molibdenu i grafitu oraz blokowanie procesu aglomeracji.Jako stabilizatory suspensji dwusiarczku molibdenu i grafitu w cieklym oleofilnym osrodku, stosowane sa rozpuszczalne w tym osrodku: aminy tluszczowe, nafteny, oraz naftosulfoniany metali alkalicznych i ziem alka¬ licznych oraz alkilosalicylany glównie magnezu, wapnia i baru.W charakterze osrodka cieklego stosowane sa: oleje mineralne, syntetyczne, lotne, ciekle weglowodory alkohole, ketony, estry, etery itp.Stwierdzono, ze stabilna suspensje dwusiarczku molibdenu i grafitu wytworzyc mozna stosujac w procesie mielenia w charakterze stabilizatora suspensji amidoimid alkenobursztynowy.Sposób wg wynalazku polega na mieleniu dwusiarczku molibdenu i(lub) grafitu w zawiesinie w cieklym oleofilnym osrodku w temp. do 160°C, glównie 20-70°C, zawierajacym rozpuszczony aminoimid alkeno¬ bursztynowy w ilosci do 20% wag glównie do 10% wag. Mielenie prowadzi sie korzystnie w obecnosci amidoimi- du alkenobursztynowego zawierajacego do 8, glównie do 5 grup aminowych oraz rodnik alkenowy o ciezarze czasteczkowym 200-2000 glównie 800-1400.2 104515 Przyklad I. Do mlyna kulowego pojemnosci roboczej 100 kg wprowadza sie 84 kg deju weglowodo* rowcgo o lepkosci 21,5 cSt w temperaturze 50°C, 6 kg. 50% roztworu olejowego aminoimidu alkenoburszty- nowego, wytworzonego w reakcji bezwodnika alkenobursztynowego o ciezarze czasteczkowym 1130 z czteroety- lenopiecioamina przy stosunku molowym reagentów 1:1 oraz 10 kg dwusiarczku molibdenu o srednicy ziaren do 2/Ltm. Mielenie prowadzi sie przez okres okolo 100 godzin w temperaturze 40-50°C do uzyskania srednicy ziaren dwusiarczku molibdenu w suspensji okreslonej metoda mikroskopowa ponizej 1 /im. Uzyskuje sie 100 kg. % suspensji dwusiarczku molibdenu o lepkosci 780 cP w temperaturze 20°C nie wykazujacej sedymentacji w czasie pólrocznego przechowywania.Przyklad II. Do mlyna perelkowego pojemnosci roboczej 200 dm3 wprowadza sie 69 kg cieklego polizobutylenu o srednim ciezarze czasteczkowym 460 i lepkosci 2177 cSt w temperaturze 50°C, 50 kg benzenu 16 kg 50% roztworu olejowego aminoimidu alkenobursztynowego wytworzonego w reakcji bezwodnika alkeno¬ bursztynowego o ciezarze czasteczkowym 950 z dwuetylenotrójamina przy rtosunku molowym reagentów 1:1 oraz 15 kg. proszku grafitu naturalnego o srednicy ziaren do 15/im oraz pozostalosci po spopieleniu 0,21%.Mielenie prowadzi sie przez ok. 30 godzin w temperaturze 30—40°C do uzyskania srednicy ziaren grafitu w su¬ spensji okreslanej metoda mikroskopowa ponizej 2 /im. Nastepnie suspensje kieruje sie do wyparki, której kub wyposazony jest w mieszadlo, oddestylowuje benzen oraz przedmuchuje pozostalosc azotem, celem odpedzenia sladów benzenu. Uzyskuje sie 100 kg 15% suspensji grafitu, o lepkosci 5300 cP w temperaturze 20°C nie wykazu¬ jacej sedymentacji w czasie pólrocznego przechowywania.Przyklad III. Do mlyna kulowego pojemnosci roboczej 100 kg wprowadza sie 76 kg deju weglowo¬ dorowego o lepkosci 91 cSt w temperaturze 50°C, 12 kg 60% roztworu olejowego aminoimidu alkenobursztyno¬ wego wytworzonego w reakcji bezwodnika alkenobursztynowego o ciezarze czasteczkowym 1050 z piperazyna przy stosunku molowym reagentów 1:1 oraz 6 kg. dwusiarczku molibdenu o srednicy ziaren do 10 jum i 6 kpn grafitu syntetycznego o srednicy ziaren do 15 jum. Mielenie prowadzi sie w temperaturze 60—70°C do uzyskania srednicy ziaren grafitu i dwusiarczku molibdenu suspensji okreslonej metoda mikroskopowa ponizej 1 /im, w cia¬ gu 130 godz. Uzyskuje sie 100 kg 12% suspensji dwusiarczku molibdenu i grafitu o lepkosci 1700 cP w tempera¬ turze 20°C nie wykazujacej sedymentacji w czasie pólrocznego przechowywania. PLThe subject of the invention is a method of preparing a stable suspension of molybdenum disulfide and graphite in a liquid oleophilic medium. According to known methods, suspensions of molybdenum disulphide and graphite are produced in a two-stage process. In the first stage, the powder of molybdenum disulphide and graphite is subjected to a preliminary grinding process. separation technique to separate fractions with a given grain diameter. In the second stage, the powder thus produced is subjected to a suspension milling process in a liquid medium. Due to the phenomenon of agglomeration of the grains of molybdenum disulfide and graphite, it is necessary to use the addition of suspension stabilizers during grinding . Grinding in suspension in a liquid medium in the presence of stabilizers leads to obtaining grains with a diameter ensuring the creation of a sedimentation equilibrium, usually below 1 µm. As suspension stabilizers, substances showing the ability to selectively adsorb on the surface of molybdenum disulfide grains are used. and graphite and blocking the agglomeration process. As stabilizers for the suspension of molybdenum disulphide and graphite in a liquid oleophilic medium, the following soluble in this medium are used: fatty amines, naphthenes, and alkali metal and alkaline earth kerosulfonates and alkylsalicylates, mainly magnesium, calcium and barium. as a liquid medium are used: mineral oils, synthetic, volatile, liquid hydrocarbons, alcohols, ketones, esters, ethers, etc. It has been found that stable suspensions of molybdenum disulfide and graphite can be produced by using alkenesuccinic amideimide as a stabilizer in the grinding process. The invention consists in grinding molybdenum disulfide and / or graphite in suspension in a liquid oleophilic medium at temperatures up to 160 ° C, mainly 20-70 ° C, containing dissolved alkenesuccinaminoimide in an amount up to 20% by weight, mainly up to 10% by weight. Grinding is preferably carried out in the presence of an alkenesuccinic amideimide with up to 8, mainly up to 5 amine groups and an alkene radical with a molecular weight of 200-2000, mainly 800-1400.2 104515 also with a viscosity of 21.5 cSt at 50 ° C, 6 kg. 50% of an oily solution of an alkenesuccinic aminoimide, prepared by the reaction of an alkenesuccinic anhydride with a molecular weight of 1130 with tetraethylene esteramine at a molar ratio of the reagents of 1: 1 and 10 kg of molybdenum disulfide with a grain diameter of up to 2 / Ltm. The grinding is carried out for a period of about 100 hours at 40-50 ° C until the grain diameter of the molybdenum disulfide in the suspension is below 1 µm by microscopy. You get 100 kg. % suspension of molybdenum disulfide with a viscosity of 780 cP at 20 ° C showing no sedimentation during six-month storage. Example II. 69 kg of liquid polyisobutylene with an average molecular weight of 460 and a viscosity of 2177 cSt at 50 ° C, 50 kg of benzene 16 kg of a 50% oil solution of alkenesuccinic aminoimide produced by the reaction of alkenesuccinic anhydride with a molecular weight of 950 are introduced into the bead mill with a working capacity of 200 dm3. with diethylene triamine at the molar ratio of the reagents 1: 1 and 15 kg. natural graphite powder with a grain diameter of up to 15 µm and an ashing residue of 0.21%. The grinding is carried out for about 30 hours at a temperature of 30-40 ° C until the diameter of the graphite grains in the suspension determined by the microscopic method is below 2 µm . Then the suspensions are directed to the evaporator, the cup of which is equipped with a stirrer, distills the benzene and blows the residue with nitrogen in order to drive off the traces of benzene. One obtains 100 kg of a 15% graphite suspension with a viscosity of 5300 cP at 20 ° C, showing no evidence of sedimentation during six-month storage. Example III. 76 kg of hydrocarbon dehydration with a viscosity of 91 cSt at 50 ° C, 12 kg of a 60% oily solution of alkenesuccinic aminoimide prepared by reaction of alkenesuccinic anhydride with a molecular weight of 1050 with piperazine at the molar ratio of the reactants are introduced into the ball mill with a working capacity of 100 kg. 1: 1 and 6 kg. molybdenum disulfide with a grain diameter of up to 10 µm and 6 kpn of synthetic graphite with a grain diameter of up to 15 µm. The grinding is carried out at a temperature of 60-70 ° C. until the grain diameter of the graphite and molybdenum disulfide of the suspension is obtained by microscopy below 1 µm for 130 hours. The result is 100 kg of a 12% suspension of molybdenum disulfide and graphite with a viscosity of 1700 cps at 20 ° C. showing no sedimentation during 6 months of storage. PL

Claims (2)

Zastrzezenia patentowe 1. Sposób wytwarzania stabilnej suspensji dwusiarczku molibdenu i(lub) grafitu w procesie mielenia zawiesi¬ ny dwusiarczku molibdenu i(lub) grafitu w cieklym oleofilnym osrodku w temperaturze do 160° w obecnosci stabilizatora suspensji, znamienny tym, ze mielenie prowadzi sie w obecnosci do 20% wagowych glównie do 10% wagowych aminoimidu alkenobursztynowego rozpuszczonego w oleofilnym osrodku.Claims 1. A method of producing a stable suspension of molybdenum disulfide and / or graphite by grinding a suspension of molybdenum disulfide and / or graphite in a liquid oleophilic medium at a temperature of up to 160 ° in the presence of a suspension stabilizer, characterized in that the grinding is carried out in the presence of up to 20 wt.% of primarily up to 10 wt.% of an alkenesuccinic aminoimide dissolved in an oleophilic medium. 2. Sposób wedlug zastrz. 1,znamienny tym, ze stosuje sie aminoimid alkenobursztynowy zawiera¬ jacy do 8, glównie do 5 grup aminowych oraz rodnik alkenowy o ciezarze czasteczkowym 200-2000 glównie, 800-1400. Prac. Poligraf. UP PRL naklad 120+18 Cena 45 zl PL2. The method according to p. A method as claimed in claim 1, characterized in that the alkenesuccinimide containing up to 8, mainly up to 5, amino groups and an alkene radical with a molecular weight of 200-2000, mainly 800-1400, are used. Wash. Typographer. UP PRL, circulation 120 + 18 Price PLN 45 PL
PL1976193695A 1976-11-12 1976-11-12 METHOD OF PRODUCING A STABLE SUSPENSION OF MOLYBDENE AND GRAPHITE SULFACE PL104515B1 (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7537724B2 (en) 2002-08-20 2009-05-26 Siemens Vai Metals Technologies Gmbh & Co. Cooling plate for metallurgic furnaces

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7537724B2 (en) 2002-08-20 2009-05-26 Siemens Vai Metals Technologies Gmbh & Co. Cooling plate for metallurgic furnaces
AU2003250046B2 (en) * 2002-08-20 2010-03-04 Voest-Alpine Industrieanlagenbau Gmbh & Co Cooling plate for metallurgic furnaces

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