DEP0053993MA - Process for the production of guanidine salts - Google Patents

Description

wrllegmde SrXindimg liet ^ ifft the BeveteHnag

f © rfator © n aar ürektea Heretellaag tob

Dinsaisen from s ©% ^ i4ii & ®te ^ CjariaEiiden are desciirem _e Sn iron ¥ © rfahre » « ä, rÄ Xalksiiekstoff with € da © m saiedrig sehaelseaäem AjofflQBtiiünsalz swecks Gewtnnimg -dee correspond to aeo. © ^ ajiidiiisalses Trerseisiolsea * bei elaigea Atssfäfcrsagen nlrd ! Assex sar BÄÖhmig. The bulging closed - QbgX @ ieli Ü @ Officials at Sea ^ experience with Ämmoaxossalgeii was good @ a _s has this general description for G-uaaidinsalsje d © a! compartment relative iioliex E®stea. 4 © r ijsssBiiaffis & lg © im fe ^ gl ^ ieli with the materials of the · "porliegeiiieia, Srfindimg. Ätteh wsrte dea _s da0 b © i der

Terfatores attentiveness that you see »with dsm in Xalfe»

Entlialt © B®ii & rapM.t explosioaeartig m. react «^. · ^ e ^ extetand the inventor toesteiit in it, Simnidiasalse cheaper than it was previously possible wsr ₉ isad oime & e £ abx for the worker heart-share *

Avl £ @raad äex Srfiadmag would © in proceedings. elaborated * the aas Erkits-en τοη ammonia., KoJaXeadioxyd land CaleiiiEacyaaaaiaid with a f seaperatsr of about 65 ⁰ Ma 250 ° C in a Gesehloe-

d aa.B der dee # asaidiiä £ & l £ es aas der & eaktionssi @ se © consists.

The UfflsetsjtiBg makes it unnecessary because the la Wüxm. eis © s Salses TörhaMea is » s © £ k is an iiSs

1289/53 ,

W t / S di / 5

© äer a Söamelss for the Äeaktiöm erfoxderlicii., © imd at the? © rf ahran der -? © rllegeadea Srfinäimgkeime ^ g @ faba

Aiamoniuiasaise like ftitrat.necessary trad the setaung is sieker füfeb

fcami in des Se & tetioasraam outer itself; contains "Praelc be performed · Me f $ is ^ erature IIad the brackish Hegen best voa within a range about 65 ° C and 3 ^ 2" at up to 250 ° C ώσι & 148 at. The Be & ktism wXrü best wäiLjpenä, a 2eitramies durehgsfilii -t äer about 4 aielat Überselirel ^ e ^ »Is ist -rorteilliafts di © Beatetioa © o

Ammoaiaic * £ oM. © »i.iösyä" saa iron wa £ ®f®3ar & n Eol-TerMlteiB iron 20-30? J-? 5 1

The caleitiaejaiiamid required for the implementation came in fora vp "XaUfcstickatQf t isfendet" During the s w chfulinuig der önse ^ fesusag der Briiadss ^ g

as AvBQs & g & gwutfs wm weaigstess © iae ©

des Amm @ KLlal £ © nnä.

Uia die Briiüduag m © oii wrsi & ndÜQher 2 »jaaoheix * she becomes άητφ. the followeadeai, illustrative examples beselirie'bim ι

"Example, 1" _ι

15 © g Ealkstic & ßtssoff wearsrin

Λ _{) M | [|} "M

the dasia ftuf 15O Ö © rhitst ward® «burnt and gas and egg» lil @ adi © xyÄ in the mol ratio Amwimiak t y as 2iT ϊ 3 im des Aatokla-r xmtvr 46 at Brack? 5 Sisaalaag © isleit ^

wichrt zn n »d BB ward © ei» Äeafctx @ as | jroaiikt erlialtea?

is

held * Me llmnidij & b © trigs was not alh @ r bsstiamt, @s is srnsimehmeBi that they mostly aas b@BtaE.dea «Bis-? ros®ataiisiieut © berafet aaf the Meage as dimearii®aat * which was obtained from this value ©» To a ©

for the iProsestaasbeutes. feßtsi, leg © B _s the overview Mwnshms sacked * dafi öieJb 1 mol Caleismeyaa- aiald in eis Mol ßuanidiii or monoßauree SuanidiaBals mswaa - »- delt or 2 be for a di & aares (Smsaiidiesoffä like that |! arbaii - Bateltoffaii -

^ mamiiüsiiarboaat was aas der EeaJctiosejaasse, in which it is dieaeia me in the following example. eaMialte-n was minded, darefc leaching with iaeißeai water «The aut Maßliek irorliaii- 4mm fmaaMineariiaaat parde saf this $ ice © sra hydrolyzes * the laeaer ISati das

the aqueous solution by dirui & mpfen or terc & with ethane © 3. ¹ ^ filter can be obtained. Other ©

aiareli alis can leach the reaction mass from the precipitating, aqueous acid w © rdea *

did © in usual outputEprodi & t for

slefc and Eoiileji & isxyä «Bs do not brew with the au * isi« la dfes. following »examples

One as. Both. Ends of open CJlasst? Linder vm about 35 sm- Biir Dhmgsser imd 200 in the length a was in the middle with Saseeiaeilit wy®®li®aeJsi 4er eisea. HS3 £ te der Eöii ^ e 30 g Aimaeniiisiearfeamaii mxd in dsr antierea SHfte 12 g KaUc * sti # tet © f £ Tmtersefeyaokti ^ as Bqät with eeiaem so treantem warde in © ia ^^^ O ocmpStokla ^ slngefeiaeiit in öeuI m B ^ tKTEir ^ idraok 1 * B © a? Office © ^ 1Le, T wart © g

aaf IfO ⁰ G © xiaitzt "S®r eatwicfcslte Bruote was 70.3 9% was" a gmasiftinlialtige E®aktiQ "in etmmr • as 4 ^ example 1 explained". -s ^ ii Z $$ cool down *.

The said aimoniiamcarbaisat canoe in the same way

iit © the in it (with © the © 2me direct Bertis with the calcium cyanamide) dtsreii üms®tsimg -ron ammonia with

w © a # «wun these ß-as« are drawn up ^ © the team as a result "feei & er stiffs" h.anö.0'11 his

To obtain a greater reaction area for Aiamoniak; w & l

is it torteiliiafts a feing © mah.l © Bes -GaX- ®a related © n _f as in dea ^ © iden © pi @ lea g @ seigt *

Example 3.

50 g ßaleiiacji ^^ iid C91i3f * reis) * 67 * 0 g 72 # 3 S Amiaraii ^ k wardeji in

of the 2 stands aaf 150 ⁰ O erMtst «earth. under the eic & ent ^ iokeltea pressure resulted in eise Ma & se _r sub d ^ r diirojb. with laeißeia lasser - as in example 1 * -

"Di® yield" was 1i $> which resulted in fb.e®ris * Di © Bi © "b-» analys® 4es beweatet © m CalaimoyanaaulAe on ei®. @ m 20 ÄaßclaaiEisieto * 14 · 1 ^ on buckets 40 amf iron 100 Äaschieasieb imd der Elicicstand gimg ämrch eia

■ '

The first and last example was repeated with the intimate undertaking * that the ösleimsicjasafflid was ground in such a way that it was went through a 200 cup strainer. The "output was $ 53"

M © methanol etc * _s are Toll Absorbed _e ^ edocli is not a solvent ertorderlioh it mad 1st also besBer _s it wegssulasBesii w © sm tee. Guanidine as £ gxtees, at which is to be obtained »

Since TATlialteismassig yejbnes OalclTistejasiasiid t®o. © x, QB is wirtee & aftlicher ,, teeimiscshee öalei ^ eyaaaait © der

asu ^ erwendeni because this b ^ sö © r "began to eat" This substance is commercially available in feiii gemaliX @ ii © r imd for dl © £ @ a te tion geeigaeform sur TeriHgang iasiä contains 6 © «öfj $ Galet ^ aeja ^ afflld ι isr

bsöte & t sum gross th feil wsm EaIk tmd ß-rapiiit ^ ^ @ r in this Irfindimg geiaraciate Kal & stlafcBtofi contained about 43 $ © e »eamt calcium _e

The following example if the fulfillment further? is the Calciuiaeyaa.sjBid Isaaer as Ka3JtesiiidfcBtoff ¥ orliaa waä. where calcium is meant i & tt scialiess the oalsima in the

"and in dea Termreinigtärigezi eia *

Example, $, «

^ nitrogen will ^ with 76 _t S g Aiaaöisiafc «next 73 # 3 g

2 StoMesi long in elttSa5jOOöoy <uioiuü5l ^ ei

The ejal ^ ioctlte Draok was 95%. Sey Autelclair isnrde then öffaet and the Bea & tiomsmaBse laersusgeaojoimen * Die booty »als jW" bo: rjat gewoisieiii tetru ^ -65 ^ of the theory * Bsi weeeatHö & effi iron deviating from the one stipulated in the B © iBpi © l

feaperatmr TerriÄgert slela, di © lasbeiute an d © r Tafeelle I iintea is inclined *

d @ r Ssmperatar at the OmöstzTang -vcaa, 73 # 3 g 76.8 g VS. and 50 g of limestone (makes one mol ÖÖg s Oa yob 3 ί 1) In a 300 ecm ÄmtoklaT during 2

T © ag »© τ®, door belt developed Yield of fiiassic lin- » © G, sals In $ der ϊ & βι »Ri« 1 65 35 11th D. 125 84 57 150 95 65 175 119.5 43 25Ö 148 6th 1) Bas «Le synthesized above © iruanidimsals irfard © not nüi®r

read & nd ©! key probably the largest website from daxfeanat · Dte ifMstg © yields were based on aaf (taaBlaixusarfee & Bt * Aae were obtained from this salary «.

If the sole diexytf ι calcium ratio is reduced to 1 * 5 ι 1 instead of 3 l 1 as in the previous examples, the yield aa ß-uanidiss as toei the same Seffiperatnr * as in Satoelle II gsseigt - noticeable Jades weä a little 0iiazddi33.ss .l2! obe careful consideration of the nature of the

äer R ^ action material aagöweadtt werä © a _s imä dl «Is not limited to any special feritalimiss® *

XI »

Si «Äussirtomi der Seioper & tw to © id © ^ WiasetsOag rom 73 ^ 3 g 76 ^ 8 g IH mkü 100 g Ksl & sticxfcstoff (gives a ratio SOg s Ca * 1i5 · 1} in ^^ eiae ^ Seitraum es voa 2 Stomäm *

f © mperatßx Same teat «ickelter Anebfe-ot © an © G.., JDraGk- ^ #>t> SaIa ₁₁ in ^ _{1 i} d _i

50 - 0

75 31 * ß 4

125 90 25

ITS tit * 5 25

200 12S ₈ 5 16

1} see definition in fatelle Ϊ *

In table JU witeja, the ice cream is further approved *

soft dee carbon dioxide 1 Oalciiam V ^ hCLtnis vom © tea value 3 1 1 a ^ ejcmintening the Ai ^ toemten sur Follow® has «

der ¥ erB © hie & © iLheite! 3. des 00 «ι δ &

häliseee bei der UssetzuBg öO _2f IHj, and Ealti © fcet0ff la O SSS ^ eines ^ eitrsiaaes v © a

OOrjtOa a © i ratio yield en i-iasnidiiäsals

(ifi every game is given here © fi © l · f> der

Ratio öOgglH, about 1i2 _s 5)

1.5 t 1 28

2.4 s 1 54

3.0 s 1 m

£ * 3 § 1 5t

β 1 s 1 5 ©

1) see definition in table I «

S «act4 (ms» ei * ϋϋβφ about 4 stands for the

s geseigt the itisbeute aer & lä.eJbi au eriiQ & esi * ia as f & Töll © Xf "

forked IT »

äer Ke & fctiönsseit at the turnover point 73 * 3, 7 € # S g SH ^ tmd 100 g KallEötleksstofS: (gives eia V

selbB-fc

From booty on

4 6

23 25 28

33 31

1} see® infinities, in

Jn Ϊa & © 13 »? It will be AiasfiirtoHig increased Eeaktionsseit with the optiaa, lea üohlgixdiozyd s Galciiam relation J- ι 1 Ss feaian b-eiaerfetl · will be »that a T-ErlSagsiuag the toi & au something. 2 hours "at 150 0 or about ^5/4 Stroxit ©! Be di @ Äuebeutea eicJa aclmell ^ rhöhexi ^ daaacli but a longer one

fiex Aiißb @ iit © b © iii_? iite

73 * 1

76s ©

) SaO

5Ö g Ealketickstoi ^ («r ^ Lbt ei» 1) is eiis, ÄV3 © Ö a © ^ AutöÄ: Xai

self & ntyj & te «lt @ ai Dracte:

1/12 1/4 t / 3

4 16

trnmtm

2> © £ iiiiti © 2i in fabeile 2 *

Ammonia § Calcium M ©! Ratio won etira S s 1 to 12 * 1 wixä Terzugswsise ia der Seclmik loud temp Sruefe rarsresa & © t _? as in

Sabell »

the differences in the IB, ι Ca Xo ^ -Vexhftlt ale

"at a constant GO« β Ca Mol-ferliEltsils imii 3 s 1 -äaroh. Heating ύόώ. j & amo »± a & t Kahlendioxyd m & Calcium cyanamide in ela © m« eaa / AutQfclain & ei 15ö ^Q ö during a period wist 2

Mol- Verh & ltais ^ elbetentwicltelter Bruok Amsbetxts aa

KH- s Ga et. disisalz 1)

3 t 1 7 © 40

6.1 s'1 - 6g

8.4 si 95 66

IUS t 1 119 »5 ^ 9

21.7 ι 1 123 & 9

1} see Uoflniifion is Säbel} «X«

J »all * dea voret®nea <äen example remained the lutoklaT ilex Heaktioa g © B <äkl © Been. Ss were Jesiodi eogsr

who ö, sr Aixt © k: 3ÄT fortlasafafid «4er mit

wüironä which aired EeaktiOBrätaNMNP woriä © _s when the Äiamonlak "Calciiam ffiol-TerfeältmiB © xJaetelieh Waer ferliältEia wait increased * AEAS lsi unventilated Beaktisse" was suitable as # geseilt in AEEN "following JBeispielea

6 _ifii

g la.Ästäc & stQj: f8 424 S Sblileadiexsrd ^ nd 826 g

"heated at 150 C ^@ In Sto ^ rt ^ apexatur amount of 4 Bniefe 11 ec

but Jjaaexkalb 10 minutes. saf eats 112 etlsg at ^ wemn E "a3ctioai.ßteaj ^ eratar IISO ⁰ C reached · lit OCE Mftspag wurfie b ^ goBneB uaä this" dam in ^ ÄaSe fortgeeetatr DAJ 55 minutes tos Begiaa from d 'r ami 2raek S? at fell. l @ it © r @ e tea braalite de »Druei: isjaerhalb ψρη 1 St ^ mde and 25 Eiaat ^ n Begiaii an on 53 * 4 & t and iimerhalto of 1 hour Tand 55 was the - ^ rack ^ is bm £ 30 at gefalloa «Laughing process iron Z Stimdea uad 10 Kdmiten the l ^ rack fell to 24« 6 at uaÄ au wait ö @ r Aatökla-v opened and that

the ^ eafctioiismasee obtained as in Example 1. The yield was $ 81 based on the theory φ

in the degree of ventilation are possible xmä -kSim & m. With

in the fer & eldiiiBsea fier BeaktioÄSstoffej as in d®m Beispi «! is sighed »combined

200 g Salketiokstoff, 282 g Koülendi & xyä and 718 g Immoaiafe

Claims (1)

LA.2U744 play heated »S ^ r autoclave was τα & 126 · 5 at is, a period τοε. 2 strandings on 33 * 7 et aired and the S-ua & idlnc & rbQnat the ^ eakticmeiaasee wi © in example 1 in elser. Ausbeut «Pn a t CnS1Ii1S, Ji1111S11P1J1 U11-O h eif 1.) Terfabren ssur Merstellermg ron S-uanidSjasalsea "nnsieiciiaetf daB AmmniBk" I ^ lilendlo ^ d wsaä a S "mperatux swiecben about 65 uoad 250 ° 0 in ßende & eakti & nsrs £ iia imter Ül> erais ^ iia imter Ül> erais. the & uanidinß as the name of & ea "fctioa.eiaas £ se g © w © smen" the turnover in d © m gesoü-oseenen ^ saktionsraiB among themselves 3 *) ^ experience ^ n nacii den Ansprtteäea 1 o-d @ r 2 * s that ^ Qjiporatiir wad Srucfc in the range, from irngsföss ¹ 65 S and 31-6 at to 250 ⁰ C and 148 at li @ g «2U 4) Method according to the Ans-iüek "ia 1 Me 3, Saäusfeh g @ kesa" "that the Oalciniscjaaaiaid ale Kalfcietlckstofi Torkanden Sb t 5 «) ^ © s'fahrem make the AaspsrSelieii 1 to 4 * through it * that AmmnUaks Xob.lüB.4iozjd and Salei-Estcjaiiaiait 1 «Sol-? ariisl, t2ii & 20 - 30 s 3 - 7« 1 applied 6 ») Verfabreji naisii den. Aaej ^ rtiela ^ a 1 to $ 5 tastor t »dafi the Umsetema ^ - during a 2 © itra & a © $ titoer about 4 S aacii deta Aasyrüciieii 1 'to 6, in that AzoaioniQffie & rbeM "al" liasgeagegrodiAt tqei a © m rope dee AmmoB | .aks and