Composite calcium-based catalyst and application thereof

A composite calcium-based catalyst technology, applied in the field of composite calcium-based catalysts, can solve the problems of polyethylene glycol molecular weight distribution, low catalyst activity, difficult product separation, etc. simple effect

Active Publication Date: 2017-06-30
SHANGHAI DONGDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is in order to overcome the existence of the catalyst used in the ethoxylation reaction in the existing polyethylene glycol preparation method and cannot prepare the polyethylene glycol with molecular weight above 8000, or the catalyst activity is low, induces However, it has the disadvantages of being long-term, unable to be applied to the industrialized production of polyethylene glycol, having a great influence on the molecular weight distribution of polyethylene glycol, being difficult to separate from the product, and having certain safety hazards, etc., and provides a complex calcium-based Catalysts and their applications

Method used

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  • Composite calcium-based catalyst and application thereof
  • Composite calcium-based catalyst and application thereof
  • Composite calcium-based catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031]Drop into 400g diethylene glycol, 1.6g composite calcium-based catalyst (wherein potassium hydroxide accounts for 20% of catalyst weight, calcium hydroxide accounts for 70%, sulfuric acid accounts for 10%) in the dry 2L pressure reactor, seal reactor; Replace the air in the reaction kettle with nitrogen for 3 times, start stirring; raise the temperature to 100°C, dehydrate under the pressure of -0.09MPa for 60min; Add the alkanes at a rate to keep the reaction pressure at 0.3MPa, and the reaction temperature at 130°C for 417min; after the reaction, mature at 130°C for 30min, degas at -0.09MPa for 15min, and then cool to 90 After ℃, the pH was adjusted to 7.0 with acetic acid to obtain polyethylene glycol. The number average molecular weight and molecular weight distribution of the product were characterized by GPC gel chromatography, and the results are listed in Table 1.

Embodiment 2

[0033] In the dry 2L pressure reactor, drop into the product described in 250g embodiment 1, 3.75g composite calcium base catalyst (wherein sodium hydroxide accounts for 30% of catalyst weight, 2-ethylhexanoate calcium accounts for 60%, oxalic acid accounts for 10%), seal the reactor; replace the air in the reactor with nitrogen for 3 times, start stirring; heat up to 100°C, dehydrate under the pressure of -0.09MPa for 60min; heat up to 100°C, slowly add 1000g of ethylene oxide for polymerization Reaction; wherein, by controlling the addition rate of ethylene oxide so that the reaction pressure is maintained at 0.25MPa, the reaction temperature is maintained at 140°C for 99min; After degassing for 20 minutes, and then cooling to 90°C, the pH was adjusted to 7.0 with lactic acid to obtain polyethylene glycol. The number average molecular weight and molecular weight distribution of the product were characterized by GPC gel chromatography, and the results are listed in Table 1.

Embodiment 3

[0035] In dry 2L pressure reactor, drop into the product described in 150g embodiment 1, 3.75g composite calcium-based catalyst (wherein potassium hydroxide accounts for 30% of catalyst weight, and calcium phosphate accounts for 55%, and citric acid accounts for 15%), Seal the reaction kettle; replace the air in the reaction kettle with nitrogen for 3 times, start stirring; raise the temperature to 100°C, dehydrate under the pressure of -0.09MPa for 60min; raise the temperature to 120°C, slowly add 1350g of ethylene oxide to carry out the polymerization reaction; among them, By controlling the addition rate of ethylene oxide to keep the reaction pressure at 0.3MPa and the reaction temperature at 150°C for 144min; after the reaction, mature at 150°C for 30min, then degas at -0.09MPa for 20min , and then cooled to 90° C., and adjusted to pH 7.0 with lactic acid to obtain polyethylene glycol. The number average molecular weight and molecular weight distribution of the product were...

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Abstract

The invention discloses a composite calcium-based catalyst and an application thereof. The composite calcium-based catalyst comprises the following components in percent by weight: 10%-40% of alkali metal hydroxide, 40%-80% of calcium salt and 10%-30% of cocatalyst. The composite calcium-based catalyst can be used for preparing polyethylene glycol with the molecular weight of more than 8000, is simple in process, strong in operability, easy in implementation, fast in reaction speed, and is beneficial to large-scale industrial production; simultaneously, the molecular weight of the prepared polyethylene glycol is accurate in control and narrow in molecular-weight distribution, no residual toxic metal ions are generated, so that the safety is good; in addition, the composite calcium-based catalyst has the advantages that the material is low in price, the activity is high and the induction period is short.

Description

technical field [0001] The invention relates to a composite calcium-based catalyst and its application. Background technique [0002] Polyethylene glycol (PEG) is a linear polymer produced by the reaction of ethylene oxide with water or ethylene glycol, and its structural formula is H(OCH 2 CH 2 ) n OH, where n represents the average addition number of ethylene oxide. The outstanding characteristics of PEG are wide range of viscosity and hygroscopicity, and wide compatibility with solvents. PEG also has good lubricity, thermal stability, low volatility and low toxicity. [0003] Polyethylene glycol (or high molecular weight polyethylene glycol) is obtained by stepwise polymerization of ethylene oxide through ethoxylation under the action of a catalyst. The catalysts used in the ethoxylation reaction in the prior art mainly contain the following types: [0004] (1) Alkali metal catalysts, such as KOH, NaOH; yet traditional alkali metal catalysts such as KOH and NaOH can...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28
CPCC08G65/269
Inventor 方洇董建国何志强杨学园周林
Owner SHANGHAI DONGDA CHEM
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