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Phosphoric terephthalic acid propylene glycol ester antiflaming block copolyester and preparation method thereof

A technology of polytrimethylene terephthalate and trimethylene phthalate, which is applied in the field of phosphorus-containing polytrimethylene terephthalate flame retardant block copolyester and its preparation field, can solve the problem of decreasing crystallization ability, decreasing, melting point, etc. Reduce problems such as easy control of the reaction, simple process operation, and improved product performance.

Active Publication Date: 2011-04-27
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the flame-retardant copolyester obtained by this method not only has excellent flame-retardant properties, but also overcomes the weaknesses of the existing technology such as uneven flame-retardant distribution and easy migration, it is a PTT flame-retardant with good industrial prospects. However, unfortunately, since the copolyester synthesized by the direct polycondensation method adopted by this method is a random copolyester, not only the melting point of the PTT flame retardant copolyester is lowered, but also the crystallization ability is greatly reduced (the DDP content is At 10wt%, the melting point drops by about 10°C, and the crystallization temperature drops by about 40°C), which affects the processing and mechanical properties of the material, especially the destruction of the crystal structure makes the unique excellent elastic recovery properties of PTT fibers also decline.

Method used

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  • Phosphoric terephthalic acid propylene glycol ester antiflaming block copolyester and preparation method thereof
  • Phosphoric terephthalic acid propylene glycol ester antiflaming block copolyester and preparation method thereof
  • Phosphoric terephthalic acid propylene glycol ester antiflaming block copolyester and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0039] First, add 291g dimethyl terephthalate, 286g 1,3-propanediol, and 0.31g zinc acetate catalyst into the reaction vessel, stir and raise the temperature under the protection of nitrogen, and carry out the transesterification reaction at 170-200°C under normal pressure until the system is stable. Until methanol is produced, add 0.12g of tetrabutyl titanate catalyst to the reaction system, and evacuate until the system pressure is 400Pa, heat up to 190-220°C for precondensation for 1 hour, and discharge to obtain polyterephthalic acid Propylene glycol ester prepolymer. The intrinsic viscosity of the prepolymer was 0.4 dL / g.

[0040]Mix 33.08g of BHPPO with the prepolymer prepared above in the solvent hexafluoroisopropanol (HFIP), and then remove the HFIP solvent by distillation to obtain a blend; then crush the blend into about 1000 grains / The specification of g is put into a vacuum solid-phase polymerization reactor and reacted at 200°C for 10 hours, and then the materia...

Embodiment 2

[0042] First, add 291g dimethyl terephthalate, 346g 1,3-propanediol, and 0.31g zinc acetate catalyst into the reaction vessel, stir and raise the temperature under the protection of nitrogen, and carry out the transesterification reaction at 190-210°C under normal pressure until the system is stable. Until methanol is produced, add 0.12g of tetrabutyl titanate catalyst to the reaction system, and evacuate until the system pressure is 400Pa, heat up to 190-220°C for precondensation for 1 hour, and discharge to obtain polyterephthalic acid Propylene glycol ester prepolymer. The intrinsic viscosity of the prepolymer was 0.3 dL / g.

[0043] Mix 16.12g of BHET (A) with the prepolymer prepared above in the solvent HFIP, and then remove the HFIP solvent by distillation to obtain a blend; then grind the blend into a specification of about 500 grains / g, Put it into a nitrogen-type solid-phase polymerization reactor and react at 210° C. for 5 hours, then discharge.

Embodiment 3

[0045] First add 291g of dimethyl terephthalate, 236g of 1,3-propanediol, and 0.31g of zinc acetate catalyst into the reaction vessel, stir and raise the temperature under the protection of nitrogen, and carry out the transesterification reaction at 160-180°C under normal pressure until the system is stable. Until methanol is produced, then add 0.12g of tetrabutyl titanate catalyst and 0.1g of triphenyl phosphite antioxidant to the reaction system, and evacuate the system until the system pressure is 400Pa, heat up to 190-210°C for precondensation for 1.4 Hours, the discharge made the polytrimethylene terephthalate prepolymer. The intrinsic viscosity of the prepolymer was 0.5 dL / g.

[0046] Mix 48.30g BHET (A) with the prepolymer prepared above in the solvent HFIP, and then remove the HFIP solvent by distillation to obtain a blend; then grind the blend into a specification of 100 grains / g, put Put it into a nitrogen-type solid-phase polymerization reactor and react at 225° C....

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Abstract

The invention discloses phosphoric terephthalic acid propylene glycol ester antiflaming block copolyester and a preparation method thereof. The copolyester is prepared by carrying out solid-phase polymerization on terephthalic acid or dimethyl terephthalate, 1,3-propylene glycol and a phosphoric component A, and the atacticity R of the copolyester is not more than 0.9, wherein the phosphoric component A accounts for 1-30% of the weight of the antiflaming block copolyester on the basis of a phosphoric monomer, the antiflaming block copolyester has the intrinsic viscosity number of 0.6-2.0dL / g, the melting point of 220-228 DEG C and the crystallization temperature of 165-185 DEG C. Compared with the pure polyterephthalic acid propylene glycol ester, for the antiflaming block copolyester prepared in the invention, the melting point and the crystallization temperature are basically kept unchanged, thereby avoiding the reduction of the processability, the mechanical property and particularly the elastic recovery property and the like of materials due to the adoption of a direct polycondensation mode for synthesizing random copolyester. The method is simple to operate and low in cost, and the reaction is easy to control, therefore continuous and mass production can be realized.

Description

technical field [0001] The invention belongs to the technical field of phosphorus-containing poly(trimethylene terephthalate) flame-retardant copolyester and its preparation technology, and in particular relates to a phosphorus-containing poly(trimethylene terephthalate) flame-retardant block copolyester and a preparation method thereof. Background technique [0002] Polytrimethylene terephthalate (PTT) is an aromatic polyester synthesized from terephthalic acid (TPA) and 1,3-propanediol (PDO) through esterification or transesterification and polycondensation. Since the aromatic polyester has PET's excellent heat resistance, chemical resistance, toughness, electrical insulation, safety, etc., it can be made into fibers, films, engineering plastics, etc., and has been industrialized since the 1990s. Since then, it has been widely used in various fields of people's daily activities. In addition, because PTT fiber also has the softness of nylon and the bulkiness of acrylic fib...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/692C08G63/80
Inventor 陈力陈洪兵王玉忠
Owner SICHUAN UNIV
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