Extraction of polylactams
    2.
    发明授权
    Extraction of polylactams 失效
    聚内酰胺的提取

    公开(公告)号:US3905946A

    公开(公告)日:1975-09-16

    申请号:US39224473

    申请日:1973-08-28

    Applicant: BASF AG

    CPC classification number: C08G69/46

    Abstract: Continuous extraction of polylactam granules for the removal of monomers and/or oligomers therefrom by means of hot water flowing countercurrently in an extraction zone, which extraction zone is divided into subzones by at least one heating zone and the water is accelerated, at certain time intervals, cocurrently and countercurrently to the flow of granules.

    Abstract translation: 连续提取多内酰胺颗粒以通过在提取区域中逆流流动的热水从其中除去单体和/或低聚物,该提取区通过至少一个加热区被分成次区域,并以特定的时间间隔加速水 与流动的流动并流逆流。

    Optically brightened and stabilized polyamides

    公开(公告)号:GB916610A

    公开(公告)日:1963-01-23

    申请号:GB2335361

    申请日:1961-06-28

    Applicant: BASF AG

    Abstract: An optically brightened and stabilized polyamide contains (A) a derivative of 1:4-bisstyrylbenzene having free carboxy groups, carboxylic acid ester groups, carboxylic acid amide groups and/or nitrile groups combined with both terminal phenyl radicals in the styryl groups as claimed in the parent Specification, and (B) an alkali or alkaline earth metal salt of phosphorous acid. The polyamides may contain additionally Ti(III) and cerium (III) salts, e.g. cerium (III) chloride and acetate and titanium (III) chloride hexahydrate, sulphate hexahydrate and acetate hexahydrate. Many polyamides and 1:4-bis-styryl benzene derivatives are specified. Specified phosphorus acid salts are sodium hydrogen phosphite and barium hydrogen phosphite. Examples (1) and (2) describe the addition to polyhexamethylene adipamide of:-(1) sodium phosphite pentahydrate, 1:4-bis(p-cyanostyryl)-benzene and titanium trichloride and (2) 1:4-bis-(p-carboxymethyl-styryl) benzene, sodium phosphite pentahydrate and titanium trichloride hexahydrate whist Examples (3) and (4) describe the addition to polycaprolactam of:-(3) the morpholide of 1:4-bis(p-carboxystyryl)-benzene, sodium phosphite and titanium trichloride hexahydrate and (4) sodium phosphite, 1:4-bis-(p-cyanostyryl) benzene and cerium trichloride heptahydrate.

    Extracting low molecular weight material from polyamides

    公开(公告)号:GB1107860A

    公开(公告)日:1968-03-27

    申请号:GB3260965

    申请日:1965-07-30

    Applicant: BASF AG

    Abstract: Low molecular weight constituents are extracted from a polylactam composition by passing a solvent downward through the composition in particle form at elevated temperature. The polymer which may be in the form of flakes or granules may be derived by polymerization of an o -amino-carboxylic acid or an amide forming derivative thereof. Suitable solvents are those of lower S.G. than the polymer and extractible material e.g. water, MeOH, EtOH and PriOH. The process may be carried out at 70-120 DEG C. and may be continuous, the polymer being raised in counter-current to the falling solvent. In Example (1) the solvent is allowed to flow down a stationary column of polycaprolactam. In Example (2) the apparatus of Fig. 2 is used. Solvent is run down the column and the polymer is raised by removing containers of treated polymer from the top of the column and replacing them by fresh ones inserted at the bottom. In Example (3) the solvent is run down a column of polymer which is raised by supplying fresh polymer at the bottom with a screw feeder and removing treated polymer from the top.

    Simultaneous recovery of pure ammonium sulphate and pure lactams from rearrangement mixtures of alicyclic ketoximes

    公开(公告)号:GB996322A

    公开(公告)日:1965-06-23

    申请号:GB1568962

    申请日:1962-04-25

    Applicant: BASF AG

    Abstract: A process for continuously recovering pure ammonium sulphate in the preparation of lactams (see Division C2) by Beckmann rearrangement of a cycloalkanone oxime having 6 to 10 ring carbon atoms with 98 to 100% wt. sulphuric acid or oleum containing up to 35% wt. of free sulphur trioxide, which reaction mixture contains 30 to 50% wt. lactam, followed by neutralizing said reaction mixture by contact with ammonia in the presence of 5 to 50 times the amount (with reference to the weight of reaction mixture) of 25 to 45% wt. ammonium sulphate solution, comprises separating the resulting lactam and ammonium sulphate phases, evaporating the ammonium sulphate phase until ammonium sulphate has been precipitated in an amount corresponding to the sulphuric acid in the rearrangement mixture, diluting the mother liquor with such an amount of water as is necessary to restore the ammonium sulphate solution to its original concentration, and returning the diluted mother liquor to the neutralization zone. Concentration of the ammonium sulphate fraction may be effected by evaporation under reduced pressure. Preferably 5 to 50 times the weight of mother liquor (with reference to the weight of rearrangement mixture) is returned to the neutralization zone.ALSO:A process for the recovery of pure lactams and pure ammonium sulphate from reaction mixtures obtained by Beckmann re-arrangement of a cycloalkanone oxime having 6 to 10 ring carbon atoms with 98 to 100% wt. sulphuric acid or oleum containing up to 35% wt. of free sulphur trioxide, which reaction mixture contains 30 to 50% wt. of lactam, comprises neutralizing said reaction mixtures by contact with ammonia in the presence of 5 to 50 times the amount (with reference to the weight of the reaction mixture) of 25 to 45% wt. ammonium sulphate solution, separating the resulting lactam and ammonium sulphate phases, evaporating the ammonium sulphate phase until ammonium sulphate has been precipitated in an amount corresponding to the sulphuric acid in the re-arrangement mixture, diluting the mother liquor with such an amount of water as is necessary to restore the ammonium sulphate solution to its original concentration, returning the diluted mother liquor to the neutralization zone, extracting the lactam phase with at least three times its weight of benzene, toluene or xylene, and distilling to obtain the lactam. Preferably 5 to 50 times the amount of mother liquor (with reference to the weight of re-arrangement mixture) is returned to the neutralization zone. Concentration of the ammonium sulphate solution may be effected by evaporation under reduced pressure. The lactam may be extracted by a countercurrent extraction in a one-stage or multi-stage process. In specific examples caprolactam and caprylolactam are produced from cyclohexanone oxine and cyclooctanone oxine respectively.

    Production of bonded non-woven fabrics

    公开(公告)号:GB978834A

    公开(公告)日:1964-12-23

    申请号:GB3128463

    申请日:1963-08-08

    Applicant: BASF AG

    Abstract: Now-woven fabrics are bonded by treatment both with an aqueous solution of a polyamine, polyalcohol or polyphenol and also with a solution (the solvent being one which is substantially insoluble in water) of an acid chloride which contains two acid chloride groups in the molecule; the sequence of the treatments with the two solutions is immaterial. Examples of the polyamines, polyalcohols and polyphenols are hexamethylene-diamine, tetramethylene-triamine, phenylene-diamine, ethylene glycol, glycerol, butanediol, butenediol, cyclohexanediol, neopentyl glycol and resorcinol. The acid chlorides used to react with these components are aromatic or aliphatic acid dichlorides such as the dichlorides of oxalic, malonic, succinic, glutaric, adipic, sebacic, maleic and terephthalic acids, or itaconic acid trichloride. Suitable solvents for these acid chlorides include hexane, heptane, cyclohexane, benzene, toluene, chloroform and trichloroethylene. Fibres which may be bonded by the above treatment include nylon 6, nylon 66, linear polyesters, acrylic fibres, natural fibres such as cotton and wool, and inorganic fibres such as glass or mineral wool. The preferred range of concentrations of the solutions with which the fabric is impregnated is from 1 to 10% by weight and impregnation may be effected by repeated dipping in a bath of the solution. Excess liquid may be removed by passage between squeeze rollers. Temperatures above atmospheric may be used if desired. Hydrogen chloride may be liberated by reaction between the two components and suitable alkalis may be included in the aqueous solution to prevent its escape. In Example 1 the aqueous solution contains 0.05% by weight of the adduct of 6 moles of ethylene oxide and 1 mole of p-isooctylphenol; in Example 8 the solution of acid chloride contains 10% by weight of p-hydroxybenzoic acid 2 ethylhexanol ester as plasticizer.

    10.
    发明专利
    未知

    公开(公告)号:FR1350455A

    公开(公告)日:1964-01-24

    申请号:FR927800

    申请日:1963-03-13

    Applicant: BASF AG

    Abstract: Fine fibres suitable for use in making papers, or cardboards are made by dissolving a polymer in an acid and reprecipitating it by diluting the acid solution with water with the use of a high shearing stress. In the example, polyhexamethylene adipamide is dissolved in sulphuric acid and the solution is dripped into water in a vessel provided with stirring means and baffles. After separation of the fibres, the diluted acid may be concentrated for reuse. Other acids referred to are hydrochloric, phosphoric and formic. Suitable polymers are polyhexamethylene - adipamide, polycaprolactam, polyacrylonitrile and polyethylene terephthalate. The fibres obtained may be processed alone or mixed with other natural or synthetic fibres on a paper-making machine to form non-woven fabrics, papers or cardboards. The fibres can be made to cohere by heating in the presence of water at temperatures below the softening points of the polymers.

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