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    31.
    发明专利
    未知

    公开(公告)号：DE1040018B

    公开(公告)日：1958-10-02

    申请号：DEB0040267

    申请日：1956-05-17

    Applicant: BASF AG

    Inventor： BILLE HEINZ ,  SPOHN HANS ,  TRIESCHMANN HANS-GEORG

    IPC: B01D5/00 ,  C07C69/82

    Abstract: Dimethyl terephthalate is purified by continuously distilling the crude ester under reduced pressure, condensing the vapour in a condenser and cooling it down to a temperature which lies above the melting point of the ester, withdrawing the ester in the liquid phase and solidifying it, and precipitating the dimethyl terephthalate entrained by the gases or vaporized liquid from the waste gases before they are allowed to escape through the suction apparatus onto the free atmosphere, by injecting water, withdrawing the resultant suspension and separating the ester. In a preferred embodiment, crude dimethyl terephthalate is heated in a vessel 1 by internal or external steam heating coils 2. The vaporous dimethyl terephthalate passes through a column 4 and a dephlegmator 5 and into a condenser 7 in which the ester is condensed to a temperature such as 145-155 DEG C. which is above the melting-point of the ester. The liquid ester without further cooling passes into a separating vessel 8 and a down pipe 9. The ester is crystallized on rollers 10 and passes through a pipe 11 to storage. The waste gas leaves the condenser 7 at a temperature above the melting-point of the ester and passes through a heated tube 12 into an injection condenser 13 and then through a suction apparatus attached to the pipe 14. By injecting water at a temperature of 0 DEG to 25 DEG C. through pipe 15 into the condenser 13 the dimethyl terephthalate entrained by the waste gases is precipitated in solid form and flows down through pipe 16 as a milky aqueous suspension. After contrifuging and drying this fraction is extremely pure.ALSO:Dimethyl terephthalate is purified by continuously distilling the crude ester under reduced pressure, condensing the vapour in a condenser and cooling it down to a temperature which lies above the melting point of the ester, withdrawing the ester in the liquid phase and solidifying it, and precipitating the dimethyl terephthalate entrained by the gases or vaporized liquid from the waste gases before they are allowed to escape through the suction apparatus into the free atmosphere, by injecting water, withdrawing the resultant suspension and separating the ester. After centrifuging and drying this fraction is extremely pure.

    Finishing cellulosic fibrous materials
    35.
    发明专利
    Finishing cellulosic fibrous materials 未知

    公开(公告)号：GB1116927A

    公开(公告)日：1968-06-12

    申请号：GB1192166

    申请日：1966-03-18

    Applicant: BASF AG

    Inventor： BILLE HEINZ ,  PETERSEN HARRO ,  RUEMENS WILHELM

    IPC: D06M15/423

    Abstract: Cellulosic fibrous materials are finished by impregnating them with an aqueous solution or dispersion containing as crosslinking agent at least one monomeric compound containing at least two groups having the formula -CH2OR, in which R is a hydrogen atom or an alkyl radical containing 1-4 carbon atoms, attached to the nitrogen atom of a carbamide group and a water soluble catalyst comprising a mixture of (a) at least one acid having a dissociation constant of at least 10-4 which is not volatile at temperatures up to 130 DEG C and (b) at least one potentially acid salt, the ratio by weight of (a) to (b) being from 1:10 to 5:1, drying them to a moisture content of 10-35% by weight with reference to the weight of the amorphous regions contained in the cellulose and reacting the crosslinking agent with the cellulose at a temperature of up to 50 DEG C. The crosslinking agent may have the formula: or in which Z is zero or 1, R1, R2, R10 and R\yF are hydrogen atoms or low molecular weight alkyl groups, R3 and R4 are radicals having the formula which are connected with each other directly or via radicals , or when R1 and R2 are low molecular weight alkyl radicals, may be hydrogen atoms, low molecular weight alkyl groups or low molecular weight alkoxymethyl groups, R5 and R7 are hydrogen atoms, R6 and R8 are hydrogen atoms, hydroxyl groups, low molecular weight alkyl groups or low molecular weight alkoxy groups, R9 is a hydrogen atom or a low molecular weight alkyl or hydroxyalkyl group, R12 and R13 are hydrogen atoms, hydroxymethyl groups or low molecular weight alkoxymethyl groups and A is a divalent aliphatic hydrocarbon radical having 2-8 carbon atoms, the low molecular weight alkyl, hydroxyalkyl, alkoxyl and alkoxymethyl groups containing 1-4 carbon atoms. The acid (a) may be sulphuric, phosphoric, oxalic, glycolic, maleic, monochloroacetic, trichloroacetic, tartaric or citric acid and the potentially acid salt (b) may be ammonium chloride, sulphate, phosphate or nitrate, dimonoethanolamine hydrogen phosphate, ethanolamine hydrochloride, 2-methyl-2-amino-propanol hydrochloride, magnesium chloride, aluminium chloride, zinc chloride or zinc nitrate. The treating composition may also contain optical brighteners, wetting agents, e.g. salts of alkyl naphthalenesulphonic acids, alkali metal salts of sulphonated dioctyl succinate and adducts of alkylene oxides and fatty-alcohols, alkylphenols or fatty amines, water repellents, e.g. paraffin wax emulsions containing aluminium or zirconium, silicones and perfluorinated aliphatic compounds, plasticizers, e.g. ethenoxylation products of high molecular weight fatty acids, fatty-alcohols or fatty-acid amides, high molecular weight polyglycol ethers and their esters, high molecular weight fatty-acids, fatty-alcohol sulphonates, stearyl-N, N-ethylene-urea and stearylamido-methylpyridinium chloride and compounds which improve the abrasion resistance of the materials treated, e.g. cellulose ethers and esters, alginates, polyethylene, polyamides, ethenoxylated polyamides, polyvinyl-ethers, polyvinyl alcohol, polyacrylic acid or polymethacrylic acid and the esters and amides thereof, polyvinyl propionate, polyvinyl-pyrrolidone and copolymers of vinyl chloride and acrylic esters, butadiene and styrene or acrylonitrile, a -dichloroethylene, b -chloro alkylacrylic esters or vinyl ethyl ether and acrylamide, or the amides of crotonic acid or maleic acid or from N-methylol acrylamide or methacrylamide and other polymerizable compounds. After drying the treated material may be covered with a moisture-impermeable sheet e.g. polyethylene or stored in a chamber whose atmosphere has an appropriate moisture content and left until the reaction is complete, and then washed and dried. Fibres, flock, slivers and woven, non-woven, knitted or net fabrics comprising cotton, linen or viscose rayon fibres alone or in admixture with wool, silk, cellulose ester, polyester, polyamide, polyolefin, polyacrylonitrile or vinyl chloride polymer fibres, may be treated.

    36.
    发明专利
    未知

    公开(公告)号：FR1504864A

    公开(公告)日：1967-12-08

    申请号：FR84850

    申请日：1966-11-24

    Applicant: BASF AG

    Inventor： BILLE HEINZ ,  RUETTIGER WILHELM

    IPC: D06M15/423

    Abstract: 1,141,515. Mixed aminoplast textile treating compositions. BADISCHE ANILIN- & SODAFABRIK A.G. 25 Nov., 1966 [27 Nov., 1965; 8 June, 1966], No. 52871/66. Heading C3R. [Also in Division D1] A composition suitable for use in the treatment of cellulosic fabrics comprises (a) at least one poly-N-methylol compound which condenses at a temperature less than 140‹ C., (b) at least one poly-N-methylol compound which condenses at a temperature of at least 140‹ C. and (c) at least one acid curing catalyst which forms an acid under the conditions of condensation. The poly-N-methylol compounds contain two or more hydroxymethyl or alkoxymethyl groups having 1-5 carbon atoms in the alkoxy group which are attached to nitrogen. The compounds (a) may have the formula in which each R 1 is a hydrogen atom or when taken together the two substituents R 1 denote and the substituents R 2 which may be the same or different are hydrogen atoms or alkyl groups having 1-4 carbon atoms and the compounds (b) may have the formula or in which R 3 is a hydrogen atom or alkyl group having 1-4 carbon atoms, R 4 is R 5 is a hydrogen atom, an alkyl group having 1-4 carbon atoms or a group of the formula R 3 O-CH 2 -, R 6 is an alkylene group having 2-4 carbon atoms, R 7 is methyl or ethyl and n is 0 or 1, the compounds containing at least two R 3 O-CH 2 - groups. The acid curing catalyst may be aluminium sulphate, zinc chloride, zinc nitrate, ammonium chloride, ammonium nitrate, ammonium phosphate and salts of ethanolamine, diethanolamine, 2- hydroxy - 2 - methylpropylamine with hydrochloric acid, magnesium chloride and magnesium sulphate. The compounds (a), (b) and (c) may be applied to the fabrics from an aqueous bath which may also contain wetting agents, e.g. salts of alkylnaphthalene sulphonic acids, alkali metal salts of sulphonated dioctyl succinate and adducts of alkylene oxides with fatty alcohols, alkyl phenols or fatty amines, water repelling agents, e.g. paraffin wax emulsions containing aluminium or zirconium, silicon containing formulations and perfluorinated aliphatic compounds, softeners, e.g. ethenoxylation products of high molecular weight fatty acids, fatty alcohols or fatty amides, high molecular weight polyglycol ethers and esters thereof, high molecular weight fatty acids, fatty alcohol sulphonates, stearyl-N,N-ethyleneurea and stearylamidomethyl pyridimium chloride, finishes, e.g. cellulose ethers and esters, alginates, polyamides, ether-oxylated polyamides, polyvinyl ethers, polyvinyl alcohol, polyacrylic or methacrylic acid or esters or amides thereof, polyvinyl propionate, polyvinyl pyrrolidone, copolymers of vinyl chloride and acrylic esters, butadiene and styrene or acrylonitrile, α-dichloroethylene, #-chloroalkyl acrylic esters or vinyl-#-chloroethyl ether and acrylamide or amides of crotonic or maleic acid, or N-methylolmethacrylamide and other polymerizable compounds, or polyethylene, and optical brighteners. In examples the aminoplast mixtures are: dimethylol ethyleneurea plus (1) dimethylol glyoxal monoureine or (2) dimethylol ethyl - urethane or (4) dimethylol urea and dimethylol glyoxal monoureine; or (3) dimethylol propyleneurea plus dimethylol 4-methoxy-5: 5- dimethylpropyleneurea; or (5) dimethylol glyoxal monoureine plus dimethylol 5-isobutyl hexahydro - 1: 3: 5 - triazinone - 2. These are used in aqueous solution containing MgCl 2 or Mg(SO 4 ) 2 and optionally polyethylene emulsion and/or a copolymer of butyl acrylate/butylene diacrylate / methylol methacrylamide / acrylamide and optionally ethoxylated iso-octylphenol.

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