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Method for synthesizing ultrahigh-viscosity water-soluble block polyether by one-pot method

A block polyether, water-soluble technology, applied in the field of anode materials for sodium-ion batteries, can solve the problems of product viscosity drop, molecular weight not meeting the expected requirements, product turbidity, etc., and achieve the goal of increasing viscosity, increasing molecular weight, and reducing reaction rate Effect

Pending Publication Date: 2022-01-07
南京联智科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that it is very difficult to synthesize polyether with a molecular weight of more than 100,000 due to the limitation of traditional basic catalysts. The introduced ethylene oxide and propylene oxide are prone to self-polymerization, which will not only lead to turbidity of the product, but also lead to The molecular weight does not meet the expected requirements, resulting in a decrease in product viscosity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment 1

[0024] Step 1: Place the compound containing active hydrogen in a reaction kettle containing 9.21g (containing 0.3mol of hydroxyl) glycerol and 9g (containing 0.1mol of hydroxyl) propylene glycol monomethyl ether initial polyether, and add 2‰wt phosphazene Catalyst, which catalyzes the nucleophilic substitution reaction between the active hydrogen and the initial polyether. After vacuuming, the temperature in the reactor is raised to 130°C to ensure that the water content is within 0.1%wt, and an initiator with a total hydroxyl mole number of 0.4mol is obtained;

[0025] Step 2: Introduce a mixture of 792g (18mol) ethylene oxide and 5220g (50mol) propylene oxide into the reactor, so that the mixture of ethylene oxide and propylene oxide and the active hydrogen in the initiator will undergo nucleophilicity Substitution reaction to generate a new structure with active hydrogen, and the new structure with active hydrogen continues to undergo epoxy ring reaction with the mixture of...

specific Embodiment 2

[0030] Step 1: Put the compound containing active hydrogen in the initial polyether reaction kettle containing 7.6g 1,2-propanediol (containing 0.2mol of hydroxyl) and 26.4g of propylene glycol monobutyl ether (containing 0.2mol of hydroxyl), and add 2‰wt Phosphazene catalyst, which catalyzes the nucleophilic substitution reaction between the active hydrogen and the initial polyether. After vacuuming, the temperature in the reactor is raised to 150°C to ensure that the water content is within 0.1%wt, and the total molar number of hydroxyl groups is 0.4mol. agent;

[0031] Step 2: Introduce a mixture of 1584g (36mol) ethylene oxide and 2088g (36mol) propylene oxide into the reactor, so that the mixture of ethylene oxide and propylene oxide and the active hydrogen in the initiator will undergo nucleophilicity Substitution reaction to generate a new structure with active hydrogen, and the new structure with active hydrogen continues to undergo epoxy ring reaction with the mixture...

specific Embodiment 3

[0036] Step 1: Put the compound containing active hydrogen in the initial polyether reaction kettle containing 7.6g 1,2-propanediol (containing 0.2mol of hydroxyl) and 26.4g of propylene glycol monobutyl ether (containing 0.2mol of hydroxyl), and add 2‰wt Phosphazene catalyst, catalyzing the nucleophilic substitution reaction between the active hydrogen and the initial polyether. After vacuuming, the temperature in the reactor is raised to 140°C to ensure that the water content is within 0.1%wt, and the total molar number of hydroxyl groups is 0.4mol. agent;

[0037]Step 2: Introduce a mixture of 1320g (30mol) ethylene oxide and 2320g (30mol) propylene oxide into the reaction kettle to make the mixture of ethylene oxide and propylene oxide react with the active hydrogen in the initiator for nucleophilicity Substitution reaction to generate a new structure with active hydrogen, and the new structure with active hydrogen continues to undergo epoxy ring reaction with the mixture ...

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Abstract

The invention relates to a method for synthesizing ultrahigh-viscosity water-soluble block polyether by a one-pot process, which comprises the following steps: placing a compound containing reactive hydrogen in a reaction kettle, adding a phosphazene catalyst to catalyze nucleophilic substitution reaction between the reactive hydrogen and initial polyether, vacuumizing, and heating to 130-150 DEG C in the reaction kettle; introducing a mixture of ethylene oxide and propylene oxide into the reaction kettle, and carrying out nucleophilic substitution reaction on the mixture and reactive hydrogen to generate polyether polyol; introducing ethylene oxide into the reaction kettle to generate ethylene oxide-terminated polyether polyol; after the reaction is finished, aging until the pressure in the reaction kettle is unchanged; introducing an isocyanate cross-linking agent; reacting the primary hydroxyl group in the ethylene oxide terminated polyether polyol of the primary hydroxyl group to generate macromolecular polyether polyol; and vacuumizing to remove the solvent to obtain the ultrahigh-viscosity water-soluble block polyether. The alkali metal content in the polyether is reduced, the molecular weight of the polyether is improved, and the viscosity of the water-soluble block polyether is increased.

Description

technical field [0001] The invention relates to a method for synthesizing an ultra-high-viscosity water-soluble block polyether by a one-pot method, and belongs to the technical field of negative electrode materials for sodium-ion batteries. Background technique [0002] Water-soluble polymer polyether is an important raw material for synthetic and semi-synthetic metalworking fluids. The existing technology is to combine active hydrogen initiator compounds with ethylene oxide and propylene oxide under the action of a basic catalyst. Such compounds are polymerized to form high-viscosity macromolecular compounds. The disadvantage is that it is very difficult to synthesize polyether with a molecular weight of more than 100,000 due to the limitation of traditional basic catalysts. The introduced ethylene oxide and propylene oxide are prone to self-polymerization, which will not only lead to turbidity of the product, but also lead to The molecular weight does not meet the expect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/333C08G65/28
CPCC08G65/33358C08G65/2609C08G65/2675
Inventor 尹艳洪陈曦苏芬
Owner 南京联智科技有限公司
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