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Method of synthesizing polyurethane curing agent by multi-batch charging manner and product thereof

A polyurethane curing agent, polyurethane prepolymer technology, applied in chemical instruments and methods, polyurea/polyurethane coatings, preparation of organic compounds, etc., can solve the problems of complicated processing technology and high cost, and avoid yellowing and cost. The effect of low and lower production cost

Active Publication Date: 2015-01-07
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] At present, the process of synthesizing polyurethane curing agent generally adopts a one-step method to synthesize TDI trimer. In order to improve the quality of the product, it mainly focuses on subsequent processing of the product to produce high-performance products, but the post-processing process is complicated and the cost is high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A polyurethane curing agent is synthesized by a multi-batch feeding method. The specific steps are as follows:

[0039] (1) Preparation of Mannich base: Mix 94g bisphenol A with 225g 40% dimethylamine solution and 86g 37% formaldehyde, add 3g10wt% dilute hydrochloric acid at 90℃ Reaction under solution catalysis for 4 hours, cooling and standing for separation, discarding the water phase, and distilling the organic phase under reduced pressure at 120°C and -0.95 MPa to obtain the Mannich base catalyst;

[0040] (2) On pass N 2 Under protection, first react with 1.77g ethanol and 100g TDI-80 at 60℃ for 2h to obtain 101.77g polyurethane prepolymer; in the TDI-80, the mass fraction of 2,4-TDI accounts for 80%, and the mass fraction of 2,6-TDI The score is 20%, the same below;

[0041] (3) Pass N 2 For protection, first put 5g of the Mannich base catalyst prepared above and 95g of the butyl acetate solvent that has been dewatered in advance into a reaction vessel with stirring an...

Embodiment 2

[0046] A polyurethane curing agent is synthesized by a multi-batch feeding method. The specific steps are as follows:

[0047] (1) Preparation of Mannich base: mix 120g of phenol with 300g of dimethylamine solution with a mass fraction of 40% and 100g of formaldehyde with a mass fraction of 37%. At 80℃, add 5g of 10wt% dilute hydrochloric acid solution to catalyze React for 4 hours, cool and stand for separation, discard the water phase, and distill the organic phase under reduced pressure at 120° C. and -0.95 MPa to obtain the Mannich base catalyst;

[0048] (2) On pass N 2 Under protection, first use 8.57g n-dodecanol and 100g TDI-80 to react at 50℃ for 3h to obtain 108.57g polyurethane prepolymer;

[0049] (3) Pass N 2 For protection, first put 5g of the Mannich base catalyst prepared above and 120g of butyl acetate solvent that has been dewatered in advance into a reaction vessel with a stirring and reflux device, and then heat to 50°C for preheating for 30 minutes; then, the pol...

Embodiment 3

[0052] A polyurethane curing agent is synthesized by a multi-batch feeding method. The specific steps are as follows:

[0053] (1) Preparation of Mannich base: Mix 80g of tert-butylphenol with 180g of 40% dimethylamine solution and 100g of 37% formaldehyde. At 85°C, add 2g of 10wt% dilute The reaction was carried out under the catalysis of the hydrochloric acid solution for 4 hours, and after cooling and standing for separation, the aqueous phase was discarded, and the organic phase was distilled under reduced pressure at 120° C. and -0.95 MPa to obtain the Mannich base catalyst;

[0054] (2) On pass N 2 Under protection, first use 3.41g of n-butanol and 100g of TDI-80 to react at 45°C for 2.5h to obtain 103.41g of polyurethane prepolymer;

[0055] (3) Pass N 2 For protection, first put 5g of the Mannich base catalyst prepared above and 100g of butyl acetate solvent that has been dewatered in advance into a reaction vessel with a stirring and reflux device, and then heat to 50°C for ...

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Abstract

The invention belongs to the field of polyurethane curing agents and discloses a method of synthesizing a polyurethane curing agent by a multi-batch charging manner and a product thereof. The method includes following steps of: mixing a small molecule alcohol with single hydroxy and an isocyanate monomer, reacting at 20-60 DEG C for 1-2 h to obtain a polyurethane prepolymer, mixing a Mannich base catalyst and a polar solvent, stirring, heating to 30-100 DEG C, preheating for 20-40 min, dividing the polyurethane prepolymer into equal parts according to mass, adding the equal polyurethane prepolymer parts into a mixed solvent in batch, adding a polymerization inhibitor to terminate the reaction after the addition is finished, and adding a small molecule alcohol for modification to obtain the product that is the polyurethane curing agent. In the polyurethane curing agent, the solid content is 50+ / -2%, the NCO group content is 7.0-8.0%, and the percentage of free TDI is not more than 0.5%. The polyurethane curing agent has advantages of light color, narrow molecular weight distribution and capability of rapidly curing at room temperature.

Description

Technical field [0001] The invention belongs to the field of polyurethane curing agents, and relates to a method for synthesizing a polyurethane curing agent with low free isocyanate monomers, in particular to a method for synthesizing a polyurethane curing agent in a multi-batch feeding manner and a product thereof. Background technique [0002] Due to its excellent physical and mechanical properties, good thermal properties and chemical resistance, polyurethane materials are widely used in the decoration of architectural and household coatings, adhesives, bionic materials, and the protection of automobiles, ships and aerospace industries. Among them, the polyurethane curing agent, as an important component containing polyisocyanate groups, can be matched with components containing hydroxyl amino groups to obtain polyurethane paint films that can react quickly at room temperature and have high crosslinking density, and can be applied to a variety of In the formulation design of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/76C09D175/04C07C271/28C07C269/02
Inventor 张心亚郭纪帅
Owner SOUTH CHINA UNIV OF TECH
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