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Preparation method of polytrimethylene terephthalate

A polytrimethylene terephthalate and terephthalic acid technology, applied in the direction of one-component polyester rayon, etc., can solve the problems of difficult reaction control, affecting the molecular weight of polymers, etc., and achieve outstanding substantive characteristics, The effect of small catalyst dosage and mild reaction conditions

Active Publication Date: 2014-03-19
临沂星火知识产权服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the disadvantage is that the reaction system is a heterogeneous system in which solid-phase PTA and liquid-phase PDO coexist, and the reaction control is difficult. With the growth of molecular chains in the PTT polymerization process, some side reactions such as the formation of cyclic oligomers and the degradation of chain ends , interchain degradation, etc. will affect the molecular weight of the polymer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The preparation method of polytrimethylene terephthalate of the present invention, take terephthalic acid and 1,3-propanediol as raw material,

[0041] Step (1) Add tetraethyl titanate, terephthalic acid and 1,3-propanediol into the esterification reaction tank, and at the same time add oxalic acid dropwise, and carry out the esterification reaction at normal pressure for 30 minutes, wherein the temperature of the esterification reaction is 220°C; the molar ratio of terephthalic acid and 1,3-propanediol is: terephthalic acid: 1,3-propanediol = 1:1.05; the amount of tetraethyl titanate is the molar amount of terephthalic acid 0.001%; ​​the dosage of oxalic acid is 0.0005% of the molar weight of terephthalic acid.

[0042] Step (2) Then add tetraethyl titanate for stirring, and drop oxalic acid for polycondensation reaction at the same time, react for 5 hours, the reaction temperature is 220°C, and the reaction pressure is 0.05MPa; the amount of tetraethyl titanate ...

Embodiment 2

[0045] The preparation method of polytrimethylene terephthalate of the present invention, take terephthalic acid and 1,3-propanediol as raw material,

[0046] Step (1) Add tetraethyl titanate, terephthalic acid and 1,3-propanediol into the esterification reaction tank, and at the same time dropwise add oxalic acid to carry out the esterification reaction at normal pressure for 60 minutes, wherein the temperature of the esterification reaction is 240°C; the molar ratio of terephthalic acid and 1,3-propanediol is: terephthalic acid: 1,3-propanediol = 1:1.3; the amount of tetraethyl titanate is the molar amount of terephthalic acid 0.0001%; ​​the amount of oxalic acid is 0.001% of the molar amount of terephthalic acid.

[0047]Step (2) Then add tetraethyl titanate for stirring, and drop oxalic acid for polycondensation reaction at the same time, react for 3 hours, the reaction temperature is 240°C, and the reaction pressure is 0.01MPa; the amount of tetraethyl titanate is ter...

Embodiment 3

[0050] The preparation method of polytrimethylene terephthalate of the present invention, take terephthalic acid and 1,3-propanediol as raw material,

[0051] Step (1) Add tetraethyl titanate, terephthalic acid and 1,3-propanediol into the esterification reaction tank, and at the same time dropwise add oxalic acid to carry out the normal pressure esterification reaction for 45 minutes, wherein the temperature of the esterification reaction is 230°C; the molar ratio of terephthalic acid and 1,3-propanediol is: terephthalic acid: 1,3-propanediol = 1:1.1; the amount of tetraethyl titanate is the molar amount of terephthalic acid 0.0005%; the amount of oxalic acid is 0.0008% of the molar amount of terephthalic acid.

[0052] Step (2) Then add tetraethyl titanate for stirring, and drop oxalic acid for polycondensation reaction at the same time, react for 4 hours, the reaction temperature is 230°C, and the reaction pressure is 0.03MPa; the amount of tetraethyl titanate is tereph...

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Abstract

The invention belongs to technical field of polyester fiber preparation, and specifically relates to a preparation method of polytrimethylene terephthalate. According to the preparation method, terephthalic acid and 1, 3-propanediol are taken as raw materials. The preparation method comprises following steps: (1) titanium ethoxide, terephthalic acid and 1, 3-propanediol are delivered into an esterification reaction tank, oxalic acid is added dropwise so as to obtain a mixture, and the mixture is subjected to normal pressure esterification for 30 to 60min at a temperature of 220 to 240 DEG C; and (2) titanium ethoxide is added for stirring, and at the same time oxalic acid is added dropwise for condensation polymerization for 3 to 5h, at a temperature of 220 to 240 DEG C, under a reaction pressure of 0.01 to 0.05 MPa so as to obtain polytrimethylene terephthalate. Technology of the preparation method is simple, and effect is excellent.

Description

technical field [0001] The invention belongs to the technical field of polyester fiber preparation, in particular to a preparation method of polytrimethylene terephthalate. Background technique [0002] Polytrimethylene terephthalate (PTT or PPT) fiber is a new type of polyester fiber with excellent performance developed by Shell. It is formed by polycondensation of terephthalic acid (PTA) and 1,3-propylene glycol (PDO). into, and its molecular structure is ((CH 2 )3O O=C O=CO)). [0003] PPT / PTT is a new type of polyester after PET and PBT. The advantages are comprehensive: [0004] 1. The softness of nylon (better color fastness than nylon); [0005] 2. The bulkiness of acrylic fiber (to avoid the disadvantage of easy wear and pilling of acrylic fiber); [0006] 3. The stain resistance of polyester, (but has a better hand feel). [0007] 4. It has inherent good elasticity. [0008] It integrates various excellent performances into one. It has become the latest hot n...

Claims

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Application Information

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IPC IPC(8): C08G63/183C08G63/16C08G63/78C08G63/85D01F6/62
Inventor 张成如
Owner 临沂星火知识产权服务有限公司
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