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Star-like oxazolidine latent curing agent and preparation method as well as use thereof

A technology of latent curing agent and oxazolidine, which is applied in the preparation and application field of star-shaped oxazolidine latent curing agent, which can solve the problems of difficult mixing, low crosslinking density, uneven defoaming, etc., and meet the requirements of synthesis equipment Not high, improved tensile strength, improved heat resistance

Active Publication Date: 2013-09-11
ZHEJIANG GREAT CHEM SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] This oxazolidine latent curing agent has only one oxazolidine unit structure, low curing efficiency, low crosslinking density, low molecular weight, poor compatibility with polyurethane prepolymers, difficult to mix evenly, resulting in uneven defoaming, Poor defoaming effect; mostly liquid, inconvenient storage and transportation; limited improvement in mechanical properties and heat resistance of cured materials

Method used

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  • Star-like oxazolidine latent curing agent and preparation method as well as use thereof
  • Star-like oxazolidine latent curing agent and preparation method as well as use thereof
  • Star-like oxazolidine latent curing agent and preparation method as well as use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] 1. Add 20.5g of diethanolamine and 50mL of toluene into the reaction flask, stir evenly, heat to 35°C, add 20g of acetone dropwise, continue the reaction for 1h, heat and reflux to divide the water, and stop the reaction when the water output reaches or approaches the theoretical value. After the reaction liquid is lowered to room temperature, heat and distill the toluene for reuse; the concentrated liquid is fractionated under reduced pressure, and the fraction at 65°C is collected at 100 Pa to obtain light yellow liquid 2,2-dimethyl-N-hydroxyethyl-1, 3-Oxazolidine (OX) 15.3 g.

[0055] 2. Add 10.5g of anhydrous diethyl malonate, 5.7g of 1,3-dibromopropane, 100mg of tetraethylammonium bromide, 3g of potassium carbonate powder, and 20mL of toluene into the reaction flask, stir evenly, and reflux the reaction 8h, the reaction solution was cooled to room temperature, distilled water was added to the reaction flask, tetraethylammonium bromide and potassium carbonate were r...

Embodiment 2

[0058] 1. Add 78.8g of diethanolamine and 150mL of toluene into the reaction flask, stir evenly, heat to 40°C, add 76.5g of acetone dropwise, continue the reaction for 1.2h, heat and reflux to divide the water, and stop the reaction when the water output reaches or approaches the theoretical value , when the reaction solution is lowered to room temperature, then heated to distill toluene and reused; the concentrated solution was fractionated under reduced pressure, and the fraction at 65°C was collected at 100 Pa to obtain light yellow liquid 2,2-dimethyl-N-hydroxyethyl-1 , 3-Oxazolidine (OX) 54.4g.

[0059] 2. Add 50.5g of anhydrous diethyl malonate, 25.5g of 1,3-dibromopropane, 200mg of tetraethylammonium bromide, 30g of potassium carbonate powder, and 120mL of toluene into the reaction flask, stir well, and reflux for 9h , the reaction solution was cooled to room temperature, distilled water was added to the reaction flask, tetraethylammonium bromide and potassium carbonate...

Embodiment 3

[0062] 1. Add 150.0g of diethanolamine and 300mL of toluene into the reaction flask, stir evenly, heat to 45°C, add 180.0g of acetone dropwise, continue the reaction for 1.5h, heat and reflux to divide the water, and stop the reaction when the water output reaches or approaches the theoretical value , when the reaction solution is lowered to room temperature, then heated to distill toluene and reused; the concentrated solution was fractionated under reduced pressure, and the fraction at 65°C was collected at 100 Pa to obtain light yellow liquid 2,2-dimethyl-N-hydroxyethyl-1 , 3-Oxazolidine (OX) 118.5g.

[0063] 2. Add 100g of anhydrous diethyl malonate, 50g of 1,3-dibromopropane, 400mg of tetraethylammonium bromide, 60g of potassium carbonate powder, and 200mL of toluene into the reaction flask, stir evenly, and reflux for 11 hours. Cool the reaction solution to room temperature, add distilled water to the reaction bottle, remove tetraethylammonium bromide and potassium carbon...

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Abstract

The invention discloses a star-like oxazolidine latent curing agent and a preparation method as well as an application of the latent curing agent. The latent curing agent is characterized by being prepared by the following steps of: adding 0.01-0.1 part of sodium ethoxide, 5-60 parts of tetraethyl 1,1,5,5-pentane-terminated tetraformate and 15-120 parts of 2,2-dimethyl-N-hydroxyethyl-1,3-oxazolidine into a reaction kettle, uniformly mixing the above raw materials, under the protection of nitrogen, increasing the temperature to 105-115 DEG C, carrying out reflux reaction for 2.5-3.5h, after the fractionation of ethanol is finished, increasing the temperature of a reaction solution to 115-125 DEG C to fractionate residual 2,2-dimethyl-N-hydroxyethyl-1,3-oxazolidine, when the amount of 2,2-dimethyl-N-hydroxyethyl-1,3-oxazolidine is not changed any more, stopping heating, dropwise adding 10-50 parts of butanone solution of p-toluenesulfonic acid at the concentration of 20-40% while stirring, carrying out reaction for 25-35min, neutralizing the reaction solution using acid until the pH (Potential of Hydrogen) is 7-7.5, adding 0.05-0.1 part of calcium oxide into the neutralized reaction solution, continuing the reaction for 0.5-1.5h, carrying out hot filtration at 75 DEG C to obtain 6-80 parts of thick semisolid tetra-2,2-dimethyl-N-hydroxyethyl-1,3-oxazolidinyl 1,1,5,5-pentane-terminated tetraformate.

Description

technical field [0001] The invention relates to a star-shaped oxazolidine latent curing agent, a preparation method and application thereof, and belongs to the field of preparation and application of star-shaped oxazolidine latent curing agents. Background technique [0002] One-component polyurethane (SPU) adhesive refers to the isocyanate-terminated polyurethane prepolymer directly reacts with water in the air to cure and extend the chain or cross-link. Compared with two-component polyurethane adhesives, SPU has the following advantages: no need to add other crosslinking agents and additives during use, and the cost is low; since it does not contain solvents, there is no solvent volatilization during curing, and no harmful gases will be released; the formula There is no stoichiometric error; the viscosity is low, there is no problem of mixing uniformity, and the construction is easy; the storage period is long, the performance is stable, and it can be cured only by a small...

Claims

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Application Information

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IPC IPC(8): C08G18/32C07D263/04C14C3/08A61P31/00
Inventor 高峻谭春斌雷景新
Owner ZHEJIANG GREAT CHEM SCI & TECH
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