TR201807287T4 - Taneli, fonksiyonlu silisik asit, bunun üretimine ve kullanımına yönelik yöntem. - Google Patents

Taneli, fonksiyonlu silisik asit, bunun üretimine ve kullanımına yönelik yöntem. Download PDF

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TR201807287T4
TR201807287T4 TR2018/07287T TR201807287T TR201807287T4 TR 201807287 T4 TR201807287 T4 TR 201807287T4 TR 2018/07287 T TR2018/07287 T TR 2018/07287T TR 201807287 T TR201807287 T TR 201807287T TR 201807287 T4 TR201807287 T4 TR 201807287T4
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ultrasonic
granular
functional
silicic acid
value
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Drexel Claus-Peter
Meyer Jürgen
Heindl Frank
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Evonik Degussa Gmbh
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Abstract

Mevcut buluş taneli, fonksiyonlu silisik asitler ile ilgilidir, burada Hg gözenek hacmi (< 4 µm) 0,80 ml/g üzerinde, dQ3=%10 değeri 400 µm üzerinde dQ3=%90 değeri 3000 µm altında, ultrasonik etki olmadığındaki d50 değerinin 3 dakika ultrasonik etkiden sonraki d50 değerine oranı <4,00 ve C oranı ağırlıkça %1,0-15,0'dır. Buluşa göre, taneli, fonksiyonlu silisik asitler özellikle de enzimlere yönelik taşıyıcı olmak üzere substrat olarak kullanılabilir.

Description

TARIFNAME TANELI, FONKSIYONLU SILISIK ASIT, BUNUN ÜRETIMINE VE KULLANIMINA YÖNELIK YÖNTEM Mevcut bulus taneli, fonksiyonlu silisik asitler, bunlarin üretimi ve kullanimi ile ilgilidir.
Bitki koruma ürünleri, farmasötik aktif bilesenler, hayvan yemi ve hayvan yemi katkilari üretimi veya gida endüstrisi gibi pek çok uygulama alaninda sivi veya reçine biçimindeki aktif bilesenleri akiskan ve stabil olarak depolanabilen bir biçime getirmek edilmektedir.
Substrata yönelik önemli bir gereklilik, mümkün oldugunca az substrat kullanilmasi gerekmesini saglayacak yükseklikte bir emicilik özelligidir. Bu nedenle örnegin DE artirilmasina yönelik yöntemler ile ilgilenmektedir. Ancak bu yöntemlerin yürütülmesi çok masraflidir ve simdiye kadar büyük ölçekli teknik uygulamalarda yayginlasmamistir.
Substrata yönelik bir diger gereklilik, absorbatlarin iyi akiskanlik ve buna bagli olarak iyi islenebilirlik özelliklerine sahip olmasidir. Ayrica silisik asitlerin absorbatlarin tasinmasi, baska kaplara aktarilmasi ve üretimi sirasinda mümkün oldugunca az miktarda toz olusturmasi gerekmektedir. Bu nedenle akiskanligin artirilmasina yönelik substrat biçime ve 150 pm üzerinde ortalama parçacik büyüklügüne sahip mikro taneli silisik asitler kullanilmaktadir. Bu yolla elde edilen absorbatlar gerçekten de daha yüksek akiskanliga sahip olmakta, ancak silisik asitlerin islenebilirlik özellikleri en iyi düzeyde olmamaktadir. yüzeyleri örnegin organosilanlar ile modifiye edilen, taneli silisik asitler bilinmektedir.
Sabit yatakli kataliz konusunda substrata yönelik baska gereklilikler eklenmektedir. Örnegin reaktantlarin üzerine bir katalizör sürülen yüklü substratlar ile dolu bir reaksiyon odasindan geçtigi sabit yatakli reaktörlerde gerçeklesen reaksiyonlarda reaksiyon odasindaki basinç kayiplarinin mümkün oldugunca düsük olmasini saglamak gerekmektedir. Katalizör ile yüklü bir substratin bir reaksiyon ortami içinde süspanse edildigi reaksiyonlarda reaksiyonun sonunda substratin yeniden kolay bir sekilde ayrilabilmesi gerekmektedir. Son olarak akiskan yatakli bir reaktörde gerçeklesen reaksiyonlar, yüklü substratlarin burada iyi bir sekilde akiskanlastirilabilmesini gerektirmektedir. Buna bagli olarak farkli reaktör tiplerinin yüklü tasiyicilara ve böylece substrata yönelik çok farkli gerekliliklere sahip oldugu açiktir. Bu gerekliliklerin yerine altinda, ultrasonik etki olmadigindaki d50 degerinin 3 dakika ultrasonik etkiden sonraki dso degerine orani <4,00 olan, taneli silisik asitler tarif edilmektedir, burada ölçüm 400 ila 500 um'lik bir parçacik fraksiyonunda yapilmaktadir. Ancak bu silisik asitlerin dezavantaji, örnegin enzimler veya biyokatalizörler gibi bazi katalitik etkin bilesenlerin silisik asit yüzeyine yetersiz bir oranda baglanmalari ve hizli bir sekilde yeniden desorbe edilmeleridir. parçacik büyüklügü ortanca degeri 130 ve 500 um arasinda olan silan modifiye oksidik çöktürülmüs silisik asitler, alüminyum oksitten meydana gelen gruptan seçilen hidrofobik anorganik oksitler ve bu gibi anorganik oksitlerin karisimlari bilinmektedir, hidroksil orani 2-15 OH/nmz, karbon orani agirlikça %0,1 ile 6, metanol ile islatilabilirlik Mevcut bulusun amaci, örnegin enzimleri desorpsiyon davranisi daha iyi olan silisik asitler saglamaktadir.
Bulusun konusu, özelligi - Hg gözenek hacminin (< 4 um) 0,80 mI/g üzerinde, tercihen 0,85 mI/g üzerinde, özellikle tercihen 0,90 mI/g üzerinde, son derece tercihen 0,95 mI/g üzerinde, özel olarak tercihen 1,00 mI/g üzerinde olmasi, - dQ3:%10 degerinin 400 pm üzerinde olmasi, - dQ3=o/.,90 degerinin 3000 um altinda olmasi, - ultrasonik etki olmadigindaki d5o degerinin 3 dakika ultrasonik etkiden sonraki dso degerine oraninin 4,00 altinda, tercihen 3,00 altinda, özellikle tercihen 2,60 altinda, son derece tercihen 2,10 altinda ve özel olarak tercihen 1,60 altinda pm ölçüm araligina ve entegre ultrasonik parmak sondasi bulunan Beckman Coulter firmasina ait Small Volume Module Plus 120 ml sivi modülüne, CV 181 ultrasonik konvertörü bulunan ve ultrasonik tepesi 6 mm olan Sonics firmasina ait Vibra Cell VCX 130 ultrasonik islemcisine sahip Beckman Coulter firmasina ait LS 230 lazer kirinim cihazi ile %100 genlikte hacimsel orani 1:1 olan bir etanoI/su karisiminda yapilmasi ve agirlikça %3,0-12,0 olmasi ve bunun Si(CH2)m-R', (R")XSI(CH2)m-R', Si(CH2)m-R' veya (R")xSi(CH2)m-R', burada COO-CHs, -NH-COO-CH2-CH3, -NH-(CH2)3Si(OR)3, -NH-(CH2)3-CH3 veya -NH- CH2-CH2-NH-CH2-CH2-NH2, R" = alkil, sikloalkil, x :1 veya 2, fonksiyonlu gruplarini içermesi ile karakterize edilmesi olan, taneli, fonksiyonlu silisik asittir.
Bulusa göre taneli, fonksiyonlu silisik asitler, 5,0 ila 11,0 arasinda bir pH degerine sahip olabilir.
Porozitenin yeterli yükseklikte 0lmasi,bulusa göre taneli, fonksiyonlu silisik asitlerin mezo ve/veya makro gözeneklerindeki gözenek hacminin yeterli olmasini ve böylece reaktantlarin iyi bir sekilde enzime ulasabilmesini, ayni zamanda da bulusa göre formülasyonlarin üretimine yönelik olarak mümkün oldugunca düsük miktarda substrat gerekmesini saglar.
Ayrica tercih edilen, bulusa göre, taneli, fonksiyonlu silisik asitlerin Hg gözenek hacmi tercihen 0,81 ml/g ila 1,30 ml/g'dir.
Bulusa göre, taneli, fonksiyonlu silisik asitlerin önemli bir diger özelligi sertligidir.
Porozitenin yüksek olmasi halinde mekanik stabilitenin saglanamamasi ve silisik asidin veya bununla üretilen formülasyonlarin mekanik yük altinda kalmasi durumunda olusan küçük taneciklerin oraninin daha yüksek olmasi söz konusu olabilir. Silisik asidin ambalajlanmasi ve tasinmasi sirasindaki, formülasyonlarin üretimi sirasindaki ve yüklü substratlarin kullanimi sirasindaki mekanik yükler, su içinde süspanse edilmis silisik aside 3 dakika boyunca ultrasonik dalga etkisi ile simüle edilir. Ultrasonik etki olmadigindaki dso degerinin 3 dakika ultrasonik etkiden sonraki d50 degerine orani, dso degerinin mekanik yük nedeni ile ne kadar azaldigi hakkinda bilgi verir. Silisik asit ne kadar sert olursa ultrasonik etki sonrasindaki dsou degeri ve ultrasonik etki olmadigindaki dso arasindaki fark 0 kadar düsük olur, baska bir deyisle ideal durumda ultrasonik etki olmadigindaki dso degerinin 3 dakika ultrasonik etkiden sonraki dsou degerine orani 1,00 olur.
Bulusa göre, taneli, fonksiyonlu silisik asitler ortalama parçacik büyüklüklerinin büyük olmasina ragmen çok iyi bir sertlige sahiptir.
Ultrasonik etki olmadigindaki dsou degerinin 3 dakika ultrasonik etkiden sonraki dso parmak sondasi bulunan Beckman Coulter firmasina ait Small Volume Module Plus 120 ml sivi modülüne, CV 181 ultrasonik konvertörü bulunan ve %100 genlikte ultrasonik tepesi 6 mm olan Sonics firmasina ait Vibra Cell VCX 130 ultrasonik islemcisine sahip Beckman Coulter firmasina ait LS 230 lazer kirinim cihazi ile hacimsel orani 1:1 olan bir etanoI/su karisiminda gerçeklestirilir. dQ3:%10 degeri ve d03=%90 degeri ile karakterize edilen parçacik büyüklügü dagilimi, sabit yatakli reaktörlerde akis özelliklerinin iyi ve akiskan yatakli reaktörlerde akiskanlasma özelliklerinin iyi olmasini saglamak açisindan önemlidir. Fazla büyük parçaciklar reaksiyon, çözünme ve difüzyon için yeterli spesifik yüzeye sahip degildir. Fazla küçük parçaciklar ise akis direncini artirir. Bulusa göre, taneli, fonksiyonlu silisik asitler bu Bulusa göre, taneli, fonksiyonlu silisik asitlerin C orani tercihen 1,0-9,0, tercihli olarak 1,0-7,5 özellikle tercihen 2,0-7,5 olabilir.
Fonksiyonlu gruplar Si-O-Si baglari üzerinden silisik asite bagli olabilir: x(R")xSi[(CH2)m-R'].
Taneli, fonksiyonlu silisik asit, pirojenik veya çöktürülmüs bir silisik asit olabilir.
Bulusun bir diger konusu, bulusa göre taneli silisik asidin üretimine yönelik asagidaki adimlari içeren birinci yöntemdir a) Ultrasonik isleme tabi tutulmadan ortalama parçacik büyüklügü dso 0,1 ile 350 olan, çöktürülmüs veya pirojenik bir silisik asit temin etme, b) Kurutma kaybi agirlikça %30-80 olacak sekilde a) adimindan elde edilen silisik asidi nemlendirme, c) Ekstrüzyon, taneleme, sikistirma veya topaklama yolu ile b) adimindan elde edilen silisik asitlere biçim verme, d) Kaliplanmis silisik asidi bir kurutma ünitesinde kurutma, e) 3000 um göz büyüklügü ile elekle taneleme veya granülleri elekten geçirme ve küçük taneli kismi 400 um elek gözü genisligi ile elekten geçirerek ayirma ve f) bir yüzey modifikasyon maddesi ile e) adimindan elde edilen granülleri reakte burada yüzey modifikasyon maddesi olarak asagidaki organosilanlarin en az biri veya bu organosilanlarin karisimlari kullanilir a) formülü (RO)3SI(CH2)m-R' olan organosilanlar, b) formülü (R")X(RO)(3-X)Si(CH2)m-R' olan organosilanlar, c) formülü X38i(CH2)m-R' olan halojen organosilanlar veya d) formülü (R")XX(3-X)SI(CH2)m-R' olan halojen organosilanlar, R = alkil, tercihen metil-, etil- veya propiI-, CH2-CH2-NH2, R" = alkil, sikloalkil, X = Ol veya Br, x :1 veya 2, a) adimindan elde edilen çöktürülmüs veya pirojenik silisik asitler kurutulmus ve gerekiyorsa ögütülmüs olabilir.
Yukarida tarif edilen bulusa göre birinci yöntemin yerine a) adimi için ham madde olarak kurutma kaybi agirlikça %30-80 olan, su içeren birfiltre keki de kullanilabilir.
Bulusun bir diger konusu, bulusa göre taneli silisik asidin üretimine yönelik asagidaki adimlari içeren ikinci yöntemdir i) Kurutma kaybi agirlikça

Claims (1)

  1. ISTEMLER . Taneli, fonksiyonlu silisik asit olup özelligi, - Hg gözenek hacminin (< 4 um) 0,80 mI/g üzerinde olmasi, - d03=%10 degerinin 400 pm üzerinde olmasi, - do3=%90 degerinin 3000 um altinda olmasi, - ultrasonik etki olmadigindaki dso degerinin 3 dakika ultrasonik etkiden sonraki fraksiyonunda 0,04-2000 um ölçüm araligina ve entegre ultrasonik parmak sondasi bulunan Beckman Coulter firmasina ait Small Volume Module Plus 120 ml sivi modülüne, CV 181 ultrasonik konvertörü bulunan ve ultrasonik tepesi 6 mm olan Sonics firmasina ait Vibra Cell VCX 130 ultrasonik islemcisine sahip Beckman Coulter firmasina ait LS 230 lazer kirinim cihazi ile %100 genlikte hacimsel orani 1:1 olan bir etanoI/su karisiminda yapilmasi ve - C oraninin agirlikça %1 ,0-15,0 olmasi ve SI(CH2)m-R', (R")XSI(CH2)m-R', Si(CH2)m-R' veya (R")XSI(CH2)m-R', burada COO-CH3,-NH-COO-CH2-CH3, -NH-(CH2)3SI(OR)3 -NH-(CH2)3-CH3 veya -NH- CH2-CH2-NH-CH2-CH2-NH2, R" = alkil, sikloalkil, x :1 veya 2, fonksiyonlu gruplarini içermesi ile karakterize edilmesidir. . Istem 1'e göre taneli, fonksiyonlu silisik asit olup özelligi, pH degerinin 5,0 ila 11,0 araliginda olmasi ile karakterize edilmesidir. . Istem 1 veya 2'ye göre taneli, fonksiyonlu silisik asit olup özelligi, ultrasonik etki olmadigindaki dso degerinin 3 dakika ultrasonik etkiden sonraki d50 degerine oraninin 1,00 ile 3,00 olmasi ile karakterize edilmesidir, burada ve entegre ultrasonik parmak sondasi bulunan Beckman Coulter firmasina ait Small Volume Module Plus 120 ml sivi modülüne, CV 181 ultrasonik konvertörü bulunan ve ultrasonik tepesi 6 mm olan Sonics firmasina ait Vibra Cell VCX 130 ultrasonik islemcisine sahip Beckman Coulter firmasina ait LS 230 lazer kirinim cihazi ile %100 genlikte hacimsel orani 1:1 olan bir etanol/su karisiminda yapilir. . Istem 1 veya 2'ye göre taneli, fonksiyonlu silisik asit olup özelligi, Hg gözenek hacminin (<4um) 0,90 mI/g üzerinde olmasi ile karakterize edilmesidir. . Istem 1 veya 2'ye göre taneli, fonksiyonlu silisik asit olup özelligi, Hg gözenek hacminin (< 4 um) 0,81 ila 1,50 mI/g olmasi ile karakterize edilmesidir. . istem 1 ila 5'e göre taneli, fonksiyonlu silisik asitleri üretmeye yönelik yöntem olup, özelligi asagidaki adimlari kapsamasidir a) ultrasonik isleme tabi tutulmadanki ortalama parçacik büyüklügü d50 0,1 ila 350 um olan çöktürülmüs veya pirojenik bir silisik asit temin etme, b) kurutma kaybi agirlikça %30-80 olacak sekilde a) adimindan elde edilen silisik asidi nemlendirme, c) ekstrüzyon, taneleme, sikistirma veya topaklama yolu ile b) adimindan elde edilen silisik aside biçim verme, d) kaliplanmis silisik asidi bir kurutma ünitesinde kurutma, e) 3000 um göz büyüklügü ile elekle taneleme veya granülleri elekten geçirme ve küçük taneli kismi 400 um elek gözü genisligi ile elekten geçirerek ayirma ve f) bir yüzey modifikasyon maddesi ile e) adimindan elde edilen granülleri reakte burada yüzey modifikasyon maddesi olarak asagidaki organosilanlarin en az biri veya bu organosilanlarin karisimlari kullanilir a) formülü (RO)3SI(CH2)m-R' olan organosilanlar, b) formülü (R")X(RO)(3-X)SI(CH2)m-R' olan organosilanlar, c) formülü X38i(CH2)m-R' olan halojen organosilanlar veya d) formülü (R")xX(3-x) Si(CH2)m-R' olan halojen organosilanlar, R = alkil, tercihen metiI-, etil- veya propil-, COO-CHs, -NH-COO-CH2-CH3, -NH-(CH2)3SI(OR)3 -NH-(CH2)a-CH3 veya -NH- CH2-CH2-NH-CH2-CH2-NH2, R" = alkil, sikloalkil, X = Ol veya Br, X: 1 veya 2, . Istem 6'ya göre yöntem olup özelligi, a) adimi için ham madde olarak kurutma kaybi agirlikça %30-80 olan, su içeren bir filtre keki kullanilmasi ile karakterize edilmesidir. . Istem 6'ya göre yöntem olup özelligi, silisik asidin c) adiminda hizli hareket eden bir yogun karistiricida yogunlastirilmasi ve tanelenmesi ile karakterize edilmesidir. . Istem 1 ila 5'e göre taneli, fonksiyonlu silisik asitleri üretmeye yönelik yöntem olup, özelligi asagidaki adimlari kapsamasidir i) kurutma kaybi agirlikça
TR2018/07287T 2012-06-28 2013-06-12 Taneli, fonksiyonlu silisik asit, bunun üretimine ve kullanımına yönelik yöntem. TR201807287T4 (tr)

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EP2867310B1 (de) 2018-04-18
CA2878095A1 (en) 2014-01-03
CA2878095C (en) 2020-03-31
AR091614A1 (es) 2015-02-18
JP6218823B2 (ja) 2017-10-25
KR20150032724A (ko) 2015-03-27
BR112014032729B1 (pt) 2021-06-29
US20160082415A1 (en) 2016-03-24
DE102012211121A1 (de) 2014-01-02
ES2671268T3 (es) 2018-06-05
TWI593699B (zh) 2017-08-01
US11458454B2 (en) 2022-10-04
HUE038697T2 (hu) 2018-11-28
CN104508054B (zh) 2016-08-31
WO2014001088A1 (de) 2014-01-03
TW201418269A (zh) 2014-05-16
MY194070A (en) 2022-11-10
MX360032B (es) 2018-10-19
KR102023556B1 (ko) 2019-09-23
MX2015000130A (es) 2015-05-07
BR112014032729A2 (pt) 2017-06-27
CN104508054A (zh) 2015-04-08
PT2867310T (pt) 2018-06-06

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