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Low free high compatibility toluene diisocyanate trimer curing agent and preparation method thereof

A technology of toluene diisocyanate and ‐toluene diisocyanate, applied in the field of low-free high-compatibility toluene diisocyanate trimer curing agent and its preparation, can solve the problems of limited improvement of xylene tolerance, low free TDI content, high NCO value, etc. , achieve less side reactions, improve reaction selectivity and reduce viscosity

Active Publication Date: 2018-06-29
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the disadvantage of these two methods is that they are limited to medium and short-chain monohydric alcohols in the liquid state at room temperature, which can only limitedly improve the tolerance of xylene
[0009] As far as the current technology is concerned, there is no toluene diisocyanate trimer curing agent that meets the requirements of low free TDI content, high tolerance, suitable viscosity, high NCO value, low cost and simple process at the same time.

Method used

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  • Low free high compatibility toluene diisocyanate trimer curing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] to a device with a stirrer, thermometer and 2 Add 100g TDI-80, 100g butyl acetate and 1gBHT (di-tert-butyl-p-cresol) to a protected 500mL four-neck flask, heat the water bath to 40°C, and then add 0.3g catalyst (2,4,6-tri(dimethyl Aminomethyl)phenol, referred to as DMP‐30), continued to stir and react at 40°C, and took samples every 0.5h to measure the NCO value. After 4 hours, the NCO value was 13.4wt%, and 0.15g DMP-30 was added for the second time to continue the incubation reaction. After 8 hours, the NCO value was 10.6wt%, and 0.15g DMP‐30 was added for the third time to continue the incubation reaction. After 12 hours, the NCO value was 9.5wt%, and 0.1g DMP-30 was added for the fourth time, and the temperature was raised to 70°C, and the reaction was stirred and kept warm. After 10h, the NCO value was 8.9wt%. Add 0.6g of polymerization inhibitor methyl p-toluenesulfonate, continue the heat preservation reaction for 0.5h, add 0.7g of isopropanol and 7g of butyl a...

Embodiment 2

[0041] to a device with a stirrer, thermometer and 2 Add 200g TDI‐80, 200g butyl acetate and 1g sodium hypophosphite into a protected 500mL four-neck flask, control the temperature of the water bath to 20°C, and then add 1.0g catalyst solution (2,2'‐bis[2,6‐bis( Dimethylaminomethyl)-4-hydroxyphenyl]propane, made into 25wt% DMF solution), continue to stir and react at 20°C, and take samples every 0.5h to measure the NCO value. After 6 hours, the NCO value was 12.2wt%, and 0.4g of catalyst solution was added for the second time, and the reaction was continued with heat preservation. After 8 hours, the NCO value was 10.3wt%, and 0.4g of the catalyst solution was added for the third time, and the reaction was continued at heat preservation. After 10 hours, the NCO value was 9.4 wt%, and 0.5 g of catalyst solution was added for the fourth time, heated to 60° C., stirred and kept warm for reaction. After 6 hours, the NCO value was 9.0wt%. Add 1g of polymerization inhibitor di-n-bu...

Embodiment 3

[0043] to a device with a stirrer, thermometer and 2 Add 300g TDI-80 and 300g butyl acetate and 2g antioxidant 1010 (tetra[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid] pentaerythritol ester) in the protected 1000mL four-necked flask, Control the temperature of the water bath to 35°C, then add 0.6g of catalyst (4‐methyl‐2,6‐bis(dimethylaminomethyl)phenol), continue to stir and react at 30°C, and take samples every 0.5h to measure the NCO value. After 6 hours, the NCO value was 12.5wt%, and 0.3g of catalyst was added for the second time, and the heat preservation reaction was continued. After 4 hours, the NCO value was 10.6wt%, and 0.4g of catalyst solution was added for the third time, and the heat preservation reaction was continued. After 15 hours, the NCO value was 9.4 wt%, and 0.4 g of catalyst solution was added for the fourth time, heated to 75° C., stirred and kept warm for reaction. After 3h, the NCO value was 9.1wt%. Add 1.5g of polymerization inhibitor methy...

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Abstract

The invention discloses a low-free high-compatibility toluene diisocyanate trimer curing agent and a preparation method thereof. The preparation method comprises the following steps: under nitrogen protection, putting a toluene diisocyanate monomer, a solvent and an antioxidant into a reaction vessel; controlling the reaction temperature to be 10-50 DEG C at an earlier stage; adding a catalyst in batches when NCO% is 12-14wt% and 10-11wt% and reaction is started; when NCO is 9.3-10wt%, adding the residual catalyst and controlling the temperature to be 50-100 DEG C; when NCO% is 8.0-9.3wt%, adding a polymerization inhibitor, reacting for 0.5-1 h, adding a component A, reacting for 2-4 h, adding a component B, reacting for 1-2 h, stopping reaction, cooling to room temperature and discharging materials so as to obtain the toluene diisocyanate trimer curing agent with free TDI less than 0.5%, xylene tolerance larger than 3, light color, quick drying and stable performance finally.

Description

technical field [0001] The invention relates to a polyurethane curing agent, in particular to a low free high compatibility toluene diisocyanate trimer curing agent and a preparation method thereof. Background technique [0002] As an important component of two-component polyurethane paint, polyurethane curing agent contains polyisocyanate groups, which can quickly cross-link and cure with other polyether polyol components at room temperature to form polyurethane paint films. TDI trimer is a special type of polyurethane curing agent, which has the characteristics of matte, fast drying, high hardness and high temperature resistance. As a very useful curing agent, TDI trimer curing agent is not only suitable for polyurethane systems, but also for a variety of coating formulation systems, such as containing epoxy resin, poly(meth)acrylate, polyacrylamide, phenolic Resin and other types of resin systems are also widely used in foam materials, elastomers, sealants, adhesives and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/79C09D175/04
CPCC08G18/794C09D175/04
Inventor 张心亚胡进
Owner SOUTH CHINA UNIV OF TECH
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