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    Production of butanediolformal
    2.
    发明授权
    Production of butanediolformal 失效
    生产丁二醛

    公开(公告)号：US3849444A

    公开(公告)日：1974-11-19

    申请号：US13992271

    申请日：1971-05-03

    Applicant: BASF AG

    Inventor： FUCHS H ,  RICKER E ,  SCHMIDT F ,  SCHWARTZ E ,  SPERBER H

    IPC: C07D17/00

    Abstract: 1. IN A PROCESS FOR THE PRODUCTION OF 1,4-BUTANEDIOLFORMAL WHEREIN A MIXTURE OF BUTANEDIOL-1,4M AN AQUEOUS SOLUTION OF FORMALDEHYDE OT A SUBSTANCE YIELDING FORALDEHYDE, AND AN ACID OR ACID SALT IS HEATED IN A REACTION VESSEL, THE IMPROVEMENT WHICH COMPRISES CONTINUOUSLY (A) HEATING AT THE BOIL A CONSTANT AMOUNT OF SAID REACTION MIXTURE WHICH CONTAINS LESS THAN 1% BY WEIGHT OF A STRONG ACID OR LESS THAN 10% BY WEIGHT OF AN ACID SALT OR A WEAK ACID, (B) EVAPORATING THE PRODUCT OF THE SYNTHESIS FROM THE REACTION MIXTURE AT SUCH A VELOCITY THAT A MEAN RESIDUE TIME IN THE REACTION VESSEL OF LESS THAN 240 MINUTES IS SET UP FOR A REACTION MIXTURE, (C) CONDENSING THE VAPORS OF THE PRODUCT OF THE SYNTHESIS, (D) SEPARATING THE TWO LAYERS WHICH FORM IN A LIQUID CONDENSATE, (E) SUBJECTING THE UPPER LAYER TO TREATMENT WITH ALKALI, PASSING SAID LAYER THROUGH AN EVAPORATOR AND THEREAFTER FRACTIONALLY DISTILLING SAID TREATED LAYER, AND (F) SUBJECTING THE LOWER LAYER TO AZEOTROPIC DISTILLATION AND RECYCLING THE THE DISTILLATE TO THE UNCONDENSED PRODUCT STREAM WHICH LEAVES THE REACTION VESSEL.

    4.
    发明专利
    未知

    公开(公告)号：SE373861B

    公开(公告)日：1975-02-17

    申请号：SE517371

    申请日：1968-04-17

    Applicant: BASF AG

    Inventor： RICKER E ,  SANDER B ,  SCHMIDT F ,  SCHWARTZ E ,  SPERBER H ,  WILHELM H

    IPC: C08G12/04 ,  C08G12/34 ,  C08L59/02 ,  C08L61/20 ,  C08G37/02 ,  C08G51/60

    Abstract: 1,216,275. Modified urea-formaldehyde condensates for stabilizing polyacetates. BADISCHE ANILIN- & SODA-FABRIK A.G. 19 April, 1968 [21 April, 1967 (2)], No. 18622/68. Headings C3P and C3R. Polycondensates useful as stabilizers of polyacetals against heat are prepared by heating (A) a diamide of a dicarboxylic acid having 4-18 C atoms and (B) an N : N 1 -alkyleneurea having 3-10 C atoms and/or an N : N 1 - distributed urea having alkyl, aryl or aralkyl groups of up to 8 C atoms as substituents with (C) formaldehyde in aqueous acid medium at 50‹-100‹ C., the molar ratio of (C) to (A) plus (B) being 1 to 2 : 1. Suitable starting materials are (A): azelaic, sebacic, decanedicarboxylic diamides, N : N 1 -dimethylsuberamide, adipamide and isophthalamide; (B): N : N 1 -ethylene - and - propylene - ureas, and N : N 1 - dimethyl-, -diethyl-, -dibutyl-, -diphenyl-, -ditolyl- and -methyl-tolyl-ureas. The preferred molar ratio of (A) to (B) is 0À7-1À3 : 1. The formaldehyde (C) may be supplied as paraformaldehyde, trioxane or polyoxymethylene, or in the form of previously made N-methylol derivatives of (A) or (B). H 2 SO 4 , H 3 PO 4 or strongly acid ion exchangers are suitable polycondensation catalysts. The product is preferably neutralized and washed; the viscous aqueous solution may be diluted with e.g. 1 : 3-dioxolane, methanol or methoxyethanol for use in solution, or spray dried. They are suitable for stabilizing mouldable polyacetals, especially those containing at least 80 mol. per cent oxymethylene units, the remaining units being residues of e.g. ethylene oxides, propylene oxide, 1 : 3-dioxolane, 1:3- dioxane, 1:3-dioxacycloheptone or diglycol formal. Conventional phenolic or hydrazone antioxidants may also be added, or secondary aromatic amines, and also pigments and fillers. In Examples stabilizers are prepared from (Example 1-3) isophthalamide, N : N 1 - ethyleneurea and 30% formalin; in Examples 4 and 6 adipamide is used as (A); in Example 8 4-methoxy-5 : 5 dimethyl-N : N 1 -propyleneurea is used as (B). In Example 5 a trioxane (97%) dioxolane (3%) copolymer is stabilized with 0À2% of products of the invention, 0À25% of 2 : 2 1 - methylene - bis (4 - methyl - 6 - t - butylphenol) and 0À02% NaF.

    6.
    发明专利
    未知

    公开(公告)号：NL6805505A

    公开(公告)日：1968-10-22

    申请号：NL6805505

    申请日：1968-04-18

    Applicant: BASF AG

    Inventor： RICKER E ,  SANDER B ,  SCHMIDT F ,  SCHWARTZ E ,  SPERBER H ,  WILHELM H

    IPC: C08G12/04 ,  C08G12/34 ,  C08L59/02 ,  C08L61/20

    Abstract: 1,216,275. Modified urea-formaldehyde condensates for stabilizing polyacetates. BADISCHE ANILIN- & SODA-FABRIK A.G. 19 April, 1968 [21 April, 1967 (2)], No. 18622/68. Headings C3P and C3R. Polycondensates useful as stabilizers of polyacetals against heat are prepared by heating (A) a diamide of a dicarboxylic acid having 4-18 C atoms and (B) an N : N 1 -alkyleneurea having 3-10 C atoms and/or an N : N 1 - distributed urea having alkyl, aryl or aralkyl groups of up to 8 C atoms as substituents with (C) formaldehyde in aqueous acid medium at 50‹-100‹ C., the molar ratio of (C) to (A) plus (B) being 1 to 2 : 1. Suitable starting materials are (A): azelaic, sebacic, decanedicarboxylic diamides, N : N 1 -dimethylsuberamide, adipamide and isophthalamide; (B): N : N 1 -ethylene - and - propylene - ureas, and N : N 1 - dimethyl-, -diethyl-, -dibutyl-, -diphenyl-, -ditolyl- and -methyl-tolyl-ureas. The preferred molar ratio of (A) to (B) is 0À7-1À3 : 1. The formaldehyde (C) may be supplied as paraformaldehyde, trioxane or polyoxymethylene, or in the form of previously made N-methylol derivatives of (A) or (B). H 2 SO 4 , H 3 PO 4 or strongly acid ion exchangers are suitable polycondensation catalysts. The product is preferably neutralized and washed; the viscous aqueous solution may be diluted with e.g. 1 : 3-dioxolane, methanol or methoxyethanol for use in solution, or spray dried. They are suitable for stabilizing mouldable polyacetals, especially those containing at least 80 mol. per cent oxymethylene units, the remaining units being residues of e.g. ethylene oxides, propylene oxide, 1 : 3-dioxolane, 1:3- dioxane, 1:3-dioxacycloheptone or diglycol formal. Conventional phenolic or hydrazone antioxidants may also be added, or secondary aromatic amines, and also pigments and fillers. In Examples stabilizers are prepared from (Example 1-3) isophthalamide, N : N 1 - ethyleneurea and 30% formalin; in Examples 4 and 6 adipamide is used as (A); in Example 8 4-methoxy-5 : 5 dimethyl-N : N 1 -propyleneurea is used as (B). In Example 5 a trioxane (97%) dioxolane (3%) copolymer is stabilized with 0À2% of products of the invention, 0À25% of 2 : 2 1 - methylene - bis (4 - methyl - 6 - t - butylphenol) and 0À02% NaF.

    10.
    发明专利
    未知

    公开(公告)号：FR1569910A

    公开(公告)日：1969-06-06

    申请号：FR1569910D

    申请日：1968-04-16

    Applicant: BASF AG

    Inventor： RICKER E ,  SANDER B ,  SCHMIDT F ,  SCHWARTZ E ,  SPERBER H ,  WILHELM H

    IPC: C08G12/04 ,  C08G12/34 ,  C08L59/02 ,  C08L61/20

    Abstract: 1,216,275. Modified urea-formaldehyde condensates for stabilizing polyacetates. BADISCHE ANILIN- & SODA-FABRIK A.G. 19 April, 1968 [21 April, 1967 (2)], No. 18622/68. Headings C3P and C3R. Polycondensates useful as stabilizers of polyacetals against heat are prepared by heating (A) a diamide of a dicarboxylic acid having 4-18 C atoms and (B) an N : N 1 -alkyleneurea having 3-10 C atoms and/or an N : N 1 - distributed urea having alkyl, aryl or aralkyl groups of up to 8 C atoms as substituents with (C) formaldehyde in aqueous acid medium at 50‹-100‹ C., the molar ratio of (C) to (A) plus (B) being 1 to 2 : 1. Suitable starting materials are (A): azelaic, sebacic, decanedicarboxylic diamides, N : N 1 -dimethylsuberamide, adipamide and isophthalamide; (B): N : N 1 -ethylene - and - propylene - ureas, and N : N 1 - dimethyl-, -diethyl-, -dibutyl-, -diphenyl-, -ditolyl- and -methyl-tolyl-ureas. The preferred molar ratio of (A) to (B) is 0À7-1À3 : 1. The formaldehyde (C) may be supplied as paraformaldehyde, trioxane or polyoxymethylene, or in the form of previously made N-methylol derivatives of (A) or (B). H 2 SO 4 , H 3 PO 4 or strongly acid ion exchangers are suitable polycondensation catalysts. The product is preferably neutralized and washed; the viscous aqueous solution may be diluted with e.g. 1 : 3-dioxolane, methanol or methoxyethanol for use in solution, or spray dried. They are suitable for stabilizing mouldable polyacetals, especially those containing at least 80 mol. per cent oxymethylene units, the remaining units being residues of e.g. ethylene oxides, propylene oxide, 1 : 3-dioxolane, 1:3- dioxane, 1:3-dioxacycloheptone or diglycol formal. Conventional phenolic or hydrazone antioxidants may also be added, or secondary aromatic amines, and also pigments and fillers. In Examples stabilizers are prepared from (Example 1-3) isophthalamide, N : N 1 - ethyleneurea and 30% formalin; in Examples 4 and 6 adipamide is used as (A); in Example 8 4-methoxy-5 : 5 dimethyl-N : N 1 -propyleneurea is used as (B). In Example 5 a trioxane (97%) dioxolane (3%) copolymer is stabilized with 0À2% of products of the invention, 0À25% of 2 : 2 1 - methylene - bis (4 - methyl - 6 - t - butylphenol) and 0À02% NaF.

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