Production of low-free TDI polyurethane curing agent, curing agent therefrom and its products

A polyurethane curing agent, low-free technology, applied in the field of its final products, low-free TDI polyurethane curing agent

Inactive Publication Date: 2008-12-03
BEIJING ZHANCHEN CHEM +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The object of the present invention is to provide a kind of phase transfer method for the manufacture of low free TDI trimer curing agent for the problems existing in the above-mentioned various existing polyurethane curing agent manufacturing methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Put 800kg of TDI, 100kg of butyl acetate, 0.4kg of potassium acetate, 2kg of hypophosphorous acid, and 20kg of tannamyl alcohol into the reactor, raise the temperature to about 40℃, turn off the heat pump, and when the temperature rises to about 60℃, keep it warm for 30 minutes After measuring the NCO value, when the NCO value is about 30%, the temperature is lowered to 40°C, and 200 kg of solvent petroleum ether and 0.2 kg of tributyl phosphine are added to carry out the phase transfer reaction. When the NCO value is about 20%, add tributyl When the phosphine is 0.2kg and the NCO value is about 15%, 0.6kg of benzoyl chloride is added.

[0020] Then, 200 kg of butyl acetate was added, and after the petroleum ether was removed by vacuum distillation, the solid content was adjusted to about 46% with butyl acetate. Filter packaging after passing the test.

Embodiment 2

[0022] Put 800kg of TDI, 100kg of butyl acetate, 0.3kg of tributylphosphine, 2kg of BHT, and 25kg of cetyl alcohol into the reactor, raise the temperature to about 35℃, turn off the heat pump, and when the temperature rises to about 50℃, keep it warm for 30 Measure the NCO value in minutes. When the NCO value is about 40%, cool down to 40°C, add 200 kg of dimethyl carbonate and 0.2 kg of tributyl phosphine to carry out the phase transfer reaction. When the NCO value is about 25%, add more 0.1kg of tributylphosphine, when the NCO value is about 15%, continue to add 0.15kg of tributylphosphine, and when the NCO value is about 13%, add 0.6kg of phosphoric acid.

[0023] Then 205 kg of butyl acetate was added, and after dimethyl carbonate was removed by distillation under reduced pressure, the solid content was adjusted to 46 kg with butyl acetate. Filter packaging after passing the test.

Embodiment 3

[0025]Put 800kg of TDI, 100kg of butyl acetate, 0.2kg of lithium acetate, 0.2kg of KOH, 2kg of BHT, and 30kg of stearyl alcohol into the reactor, raise the temperature to about 40℃, turn off the heat pump, and naturally heat up to about 50℃, Measure the NCO value after 30 minutes of incubation. When the NCO value is about 30%, the temperature is lowered to 40°C, and 200kg of cyclohexane and 0.2kg of KOH are added to carry out the phase transfer reaction. When the NCO value is about 20%, add KOH 0.1 kg, when the NCO value is about 16%, add 0.18 kg of KOH, and when the NCO value is about 13%, add 0.6 kg of phosphoric acid.

[0026] Then, 210 kg of butyl acetate was added, and cyclohexane was removed by vacuum distillation, and then the solid content was adjusted to 46% with butyl acetate. Filter packaging after passing the test.

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PUM

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Abstract

A low-free radical TDI polyurethane curing agent, its production and product are disclosed. The process is carried out by putting tolylene-diisoester cyanate, solvent S and catalyst A into reactor, adding into antioxidant and long-chain alcohol, agitating in reactor, heating, keeping temperature, inspecting NCO value, adding into phase-transferring solvent X while reaching NCO value to 20-40%, adding into catalyst B till reaching NCO value to 10-15, adding into inhibitor to stop reaction, adding into solvent S, decreasing pressure, distilling and removing phase-transferring solvent X. It's cheap and convenient.

Description

Technical field [0001] The present invention relates to a method for manufacturing a low-free TDI (toluene diisocyanate) polyurethane curing agent, and further relates to a low-free TDI polyurethane curing agent manufactured by the method and the final product thereof. Background technique [0002] At present, the domestic method of producing polyurethane curing agent is to use TDI to self-polymerize in a suitable solvent under the action of a catalyst. If the conventional synthesis method is adopted, there will be a large amount of unpolymerized free TDI in the curing agent production process. Depending on the process conditions and synthesis route, it is as high as 8% to 15%. [0003] TDI is the main raw material for the polyurethane industry. In polyurethane paint, TDI is the main raw material for the synthetic polyurethane paint curing agent. TDI has low vapor pressure and high toxicity. All countries have clear limits on the free TDI monomer content in TDI polymers. [0004]...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/42
Inventor 陈寿生陈冰
Owner BEIJING ZHANCHEN CHEM
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