Bleaching and dyeing; fluid treatment and chemical modification – Nontextile – dyeing process or product – including inorganic... – Polymer from polyol and a polycarboxylic acid or derivative...
Patent
1996-12-12
1998-07-21
Einsmann, Margaret
Bleaching and dyeing; fluid treatment and chemical modification
Nontextile, dyeing process or product, including inorganic...
Polymer from polyol and a polycarboxylic acid or derivative...
8922, D06P 354
Patent
active
057829357
DESCRIPTION:
BRIEF SUMMARY
BACKGROUND OF THE INVENTION
The invention relates to a process for colouring polytrimethylene terephthalate fibrrs using disperse colorants in aqueous liquors at or below the boiling point of the liquor and use of the fibres coloured according to the invention.
BACKGROUND
Polytrimethylene terephthalate (PTMT) is a polyester which has 1,3-propanediol as the diol component and terephthalic acid as the dicarboxylic acid component. Large-scale synthesis of polyesters may basically be performed by two different methods (H-D. Schumann in Chemiefasern/Textilind. 40/92 (1990), p. 1058 et seq.).
On the one hand, the older process, which was exclusively used up to about 1960, involving transesterification of dimethyl terephthalate with a diol to give bis-hydroxyalkyl terephthalate and subsequent polycondensation. On the other hand, the method extensively used today, involving direct esterification of terephthalic acid with a diol and subsequent polycondensation.
During transesterification, dimethyl terephthalate is transesterified with 1,3-propanediol using catalysts at temperatures of 160.degree.-210.degree. C. and the methanol being released is distilled out of the reaction mixture at atmospheric pressure. The reaction mixture, which comprises mostly bis-(3-hydroxypropyl) terepthalate, is further heated to 250.degree.-280.degree. C. under reduced pressure and the 1,3-propanediol being released is removed. Formation of polytrimethylene terephthalate from bis-(3-hydroxylpropyl) terephthalate may be catalysed by the same catalyst as used for transesterification or, after deactivation of the same, a different polycondensation catalyst may be added. ##STR1##
The preparation of polytrimethylene terephthalate has already been described in GB 578079. Transesterification of dimethyl terephthalate with 1,3-propanediol is catalysed by sodium and magnesium. The alcohols released are distilled off at atmospheric pressure and the reaction mixture is further heated under reduced pressure until polymeric polytrimethylene terephthalate is obtained.
A compound fibre made from polyethylene terephthalate and polytrimethylene terephthalate is described in GB 1075689. When preparing the polytrimethylene terephthalate, dimethyl terephthalate and 1,3-propane diol are used as starting materials and titanium tetrabutylate is used as transesterification and polycondensation catalyst.
Two catalyst systems for preparing polytrimethylene terephthalate are known from FR 2038039. In both cases, dimethyl terephthalate and 1,3-propanediol used as transesterification and polycondensation catalyst and in the other process "Tyzor TBT" from Du Pont and MgCO.sub.3 are used as transesterification catalysts and an antimony compound is used as the polycondensation catalyst.
German document OS 19 54 527 relating to catalysts for preparing polyesters, describes another possibility for catalysis during the production of polytrimethylene terephthalate. Here again, dimethyl terephthalate and 1,3-propanediol are used as starting materials.
Manganese(II) acetate tetrahydrate is used as the transesterification catalyst and hexagonal crystalline germanium dioxide with a particle size of less than 2 .mu.m is used as the polycondensation catalyst. These catalysts may also be used for producing dipolymers from terephthalic acid, 1,2-ethanediol and 1,3-propanediol.
A further catalyst mixture which is not based on titanium is described in U.S. Pat. No. 4,167,541. In this case cobalt acetate and zinc acetate are described as catalysts for the transesterification of dimethyl terephthalate using 1,3-propanediol and antimony oxide is used as the catalyst for polycondensation.
A new type of catalyst system is described in U.S. Pat. No. 4,611,049 and DE-OS 34 22 733. Again starting from dimethyl terephthalate and 1,3-propanediol, titanium tetrabutylate is added as catalyst. In addition, p-toluenesulphonic acid is added as promoter, thus achieving a higher molecular weight.
In 1988, C. C. Gonzalez, J. M. Perena and A. Bello (J. Polym. Sci., Part B: Polymer Physics 26 (198
REFERENCES:
patent: 3841831 (1974-10-01), Miller
Herlinger Heinz
Hirt Peter
Kuhl Gilbert
Piana Hermann
Traub Hansjorg
Degussa - Aktiengesellschaft
Einsmann Margaret
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