Method for preparing alkyl naphthalene polycondensation catalyst

A technology of polycondensation catalyst and alkylnaphthalene, which is applied in the field of preparation of polycondensation catalyst, can solve the problems of inability to realize large-scale industrial production, non-compliance, low catalytic selectivity and conversion rate of cobalt salt catalyst, and achieve improved catalytic activity selectivity As well as the effect of high moldability, catalytic selectivity and high conversion rate

Inactive Publication Date: 2013-06-26
YUEYANG PENGCHENG TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalytic selectivity and conversion rate of cobalt salt catalysts are all low, about ≤95%, which cannot meet the requirements of polyester polymerization and cannot realize large-scale industrial production

Method used

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  • Method for preparing alkyl naphthalene polycondensation catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] A molecular sieve containing Ti, Mg, Al, Si is used as a catalytically active monomer, and it is ultrafinely pulverized to d 50 =9.8μm, modified, the modified medium is a mixture of ammonium chloride, tetrapropylammonium hydroxide and methanol with a mass ratio of 2:0.08:0.3, the modified condition is 160°C, 1.4Mpa, modified Sexual treatment for 8 hours. The modified catalytically active monomer was vacuum-dried at a low temperature of 60°C, a high-purity silica sol was selected as a binder, and sample 1 was obtained through extrusion molding, drying and roasting.

Embodiment 2

[0018] A ZSM-5 molecular sieve containing Ti, Co, Al and Si is used as a catalytically active monomer, which is ultrafinely pulverized to d 50 =10.5μm, modified, the modified medium is ammonium nitrate, ammonium sulfate, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, ethanol and For the solution of the mixture of propanol, the modification condition is 160°C, 1.6Mpa, and the modification treatment is 12 hours. The modified catalytically active monomer was vacuum-dried at a low temperature of 45°C, a high-purity silica sol was selected as a binder, and sample 2 was obtained through extruding, drying and roasting.

Embodiment 3

[0020] A ZSM-5 molecular sieve containing Ti, Mg, Co, and Si was used as a catalytically active monomer, which was ultrafinely pulverized to d 50 =11.2μm, modified, the modified medium is a solution of ammonium nitrate, ammonium carbonate, tetramethylammonium hydroxide, ethanol and methanol with a mass ratio of 1.2:0.8:0.12:0.25:0.12, the modified condition 180°C, 2.3Mpa, modification treatment for 11 hours. The modified catalytically active monomer was vacuum-dried at a low temperature of 50°C, a high-purity silica sol was selected as a binder, and sample 3 was obtained through extruding, drying and roasting.

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Abstract

The invention discloses a method for preparing an alkyl naphthalene polycondensation catalyst. The method is characterized by comprising the following steps of: (1) performing ultra-fine crushing on a molecular sieve serving as a catalytically active monomer and containing Ti, Mg, Co, Al and Si; (2) putting the ultra-fine crushed catalytically active monomer into 20 to 35 mass percent modification medium solution, performing closed stirring, heating to the temperature of between 150 and 200 DEG C, and performing modification treatment for 8 to 1 hours under the pressure of 1.0 to 3.0MPa, wherein the modification medium solution consists of ammonium salt, organic amine and ethanol in a mass ratio of 2:(0.05-0.15):(0.2-0.5); and (3) performing low-temperature vacuum drying on the modified catalytically active monomer, adding a silicon-containing high-purity adhesive, performing extrusion molding, drying and roasting, thereby obtaining the alkyl naphthalene polycondensation catalyst. The compressive strength of the polyethylene naphthalate (PEN) polyester catalyst is more than or equal to 15N per granule, the polycondensation catalytic conversion rate and the selectivity of PEN polyester can be improved by more than or equal to 98 percent, and the one-way stability life test exceeds 700 hours.

Description

technical field [0001] The invention relates to a method for preparing a polycondensation catalyst, in particular to a method for preparing a polycondensation catalyst for polycondensing 2,6-naphthalene dicarboxylic acid (NDA) and ethylene glycol (EG) to generate PEN polyester. Background technique [0002] Polyethylene naphthalate (PEN polyester) is polycondensed from dimethyl 2,6-naphthalene dicarboxylate (NDC) or 2,6-naphthalene dicarboxylic acid (NDA) and ethylene glycol (EG). It is an emerging excellent polymer. Its chemical structure is similar to that of PET, except that the benzene ring in PET is replaced by a more rigid naphthalene ring in the molecular chain. The naphthalene ring structure makes PEN have higher physical and mechanical properties, gas barrier properties, chemical stability and heat resistance, ultraviolet resistance, radiation resistance and other properties than PET. Polyethylene naphthalate (PEN) is a new variety of modern commercialized polyest...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/87C08G63/85C08G63/83C08G63/82C08G63/84C08G63/189
Inventor 李鹏袁政荣
Owner YUEYANG PENGCHENG TECH DEV
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