公开(公告)号：US2964387A

公开(公告)日：1960-12-13

申请号：US78307058

申请日：1958-12-29

Applicant: ETHYL CORP

Inventor： PODALL HAROLD E ,  HYMIN SHAPIRO

IPC: C01G1/04

CPC classification number: C01G1/04

公开(公告)号：US2952518A

公开(公告)日：1960-09-13

申请号：US2425660

申请日：1960-04-25

Applicant: ETHYL CORP

Inventor： PODALL HAROLD E ,  HYMIN SHAPIRO

IPC: C01G1/04

CPC classification number: C01G1/04

公开(公告)号：US3053628A

公开(公告)日：1962-09-11

申请号：US4608760

申请日：1960-07-29

Applicant: ETHYL CORP

Inventor： PODALL HAROLD E ,  HYMIN SHAPIRO

IPC: C01G1/04

CPC classification number: C01G1/04

公开(公告)号：US2952523A

公开(公告)日：1960-09-13

申请号：US78321258

申请日：1958-12-29

Applicant: ETHYL CORP

Inventor： PODALL HAROLD E

IPC: C01G1/04

CPC classification number: C01G1/04

公开(公告)号：US3214452A

公开(公告)日：1965-10-26

申请号：US18929262

申请日：1962-04-23

Applicant: ETHYL CORP

Inventor： WERNER ROBERT P M ,  PODALL HAROLD E

IPC: C07F9/00

CPC classification number: C07F9/005

公开(公告)号：US2952524A

公开(公告)日：1960-09-13

申请号：US83543659

申请日：1959-08-24

Applicant: ETHYL CORP

Inventor： PODALL HAROLD E

IPC: C01G1/04

CPC classification number: C01G1/04

公开(公告)号：US3046290A

公开(公告)日：1962-07-24

申请号：US5082360

申请日：1960-08-22

Applicant: ETHYL CORP

Inventor： PODALL HAROLD E

IPC: C07F5/06

CPC classification number: C07F5/065

公开(公告)号：US3028220A

公开(公告)日：1962-04-03

申请号：US92960

申请日：1960-01-07

Applicant: ETHYL CORP

Inventor： GIRAITIS ALBERT P ,  PODALL HAROLD E

IPC: C01G45/04

CPC classification number: C01G45/04

公开(公告)号：US2952517A

公开(公告)日：1960-09-13

申请号：US2425560

申请日：1960-04-25

Applicant: ETHYL CORP

Inventor： PODALL HAROLD E ,  HYMIN SHAPIRO

IPC: C01G1/04

CPC classification number: C01G1/04

公开(公告)号：US3161469A

公开(公告)日：1964-12-15

申请号：US74881358

申请日：1958-07-16

Applicant: ETHYL CORP

Inventor： ASHBY EUGENE C ,  PODALL HAROLD E

IPC: C07F5/00

CPC classification number: C01B6/00 ,  C01B35/026 ,  C07F5/006

Abstract: Hydrides of boron, particularly diborane, are prepared by reacting an organic ester of boric acid with aluminium metal and hydrogen at elevated temperatures. Suitable esters are listed, examples being triphenyl borate, trimethyl borate, tri-(t-butyl) borate, tricyclohexyl borate, tribenzyl borate and tri-(p-chlorophenyl) borate. Tertiary amines which form complexes with the boron hydrides may be present as diluents, examples of which are triethylamine, trimethylamine, and triphenylamine; diborane is obtained from these complexes by acidification with hydrochloric acid or boron trichloride at room temperature. Other diluents are specified, including alkyl, cycloalkyl and aromatic hydrocarbons and ethers. The aluminium is preferably in finely divided form and may have been activated by treatment with triethyl-aluminium and hydrogen at 140 DEG C. and 1000 lbs. per sq. inch pressure or by recycling excess aluminium from a previous run. Reaction temperature may be 120-300 DEG C., 140-180 DEG C. being preferred in the absence of a tertiary amine and 200-250 DEG C. when a tertiary amine is present. Hydrogen pressures of 500 to 5000 lbs. per sq. inch may be employed. The reaction may be catalyzed by trialkyl aluminium or boron compounds or by aluminium halides, especially aluminium chloride. The boron hydride or its complex with the tertiary amine is removed from the product by distillation; by-product aluminium alcoholate may be recovered and hydrolysed to form the alcohol which is reacted with boric oxide to produce boron alcoholate for re-use in the process.