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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 product, low free TDI polyurethane curing agent

Inactive Publication Date: 2007-04-04
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 danguil alcohol into the reaction kettle, raise the temperature to about 40°C, turn off the heat pump, and when the temperature rises naturally to about 60°C, keep it warm for 30 minutes After measuring the NCO value, when the NCO value is about 30%, lower the temperature to 40°C, add 200kg of solvent petroleum ether, 0.2kg of tributylphosphine, and carry out phase transfer reaction. When the NCO value is about 20%, add tributyl Phosphine 0.2kg, when the detected NCO value is about 15%, add benzoyl chloride 0.6kg.

[0020] Then add 200 kg of butyl acetate, and after the petroleum ether is removed by distillation under reduced pressure, the solid content is adjusted to about 46% with butyl acetate. Filter and pack 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°C, turn off the heat pump, and when the temperature rises naturally to about 50°C, keep it warm for 30 Measure the NCO value after a few minutes. When the NCO value is about 40%, lower the temperature to 40°C, add 200kg of dimethyl carbonate and 0.2kg of tributylphosphine to carry out the phase transfer reaction. When the NCO value is about 25%, add 0.1kg of tributylphosphine, when the NCO value is about 15%, continue to add 0.15kg of tributylphosphine, when the detected NCO value is about 13%, add 0.6kg of phosphoric acid.

[0023] Then add 205 kg of butyl acetate, and after removing dimethyl carbonate by distillation under reduced pressure, adjust the solid content to 46% with butyl acetate. Filter and pack 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°C, turn off the heat pump, and naturally heat up to about 50°C, Measure the NCO value after 30 minutes of heat preservation. When the NCO value is about 30%, lower the temperature to 40°C, add 200kg of cyclohexane and 0.2kg of KOH 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 add 210 kg of butyl acetate, and after decompression distillation removes cyclohexane, the solid content is adjusted to 46% with butyl acetate. Filter and pack 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 invention relates to a method for producing a low-free TDI (toluene diisocyanate) polyurethane curing agent, and further relates to the low-free TDI polyurethane curing agent produced by the method, and its final product. Background technique [0002] At present, the method of domestic production of polyurethane curing agent is to use TDI to undergo self-polymerization in a suitable solvent under the action of a catalyst. If a conventional synthesis method is adopted, there will be a large amount of unpolymerized free TDI in the production process of the curing agent. Depending on the process conditions and synthetic route up to 8% to 15%. [0003] TDI is the main raw material of polyurethane industry. In polyurethane paint, TDI is the main raw material of synthetic polyurethane paint curing agent. TDI has low vapor pressure and high toxicity. All countries have clear restrictions on the content of free TDI monomers in TDI polymers. [0004] In ...

Claims

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Application Information

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IPC IPC(8): C08G18/42
Inventor 陈寿生陈冰
Owner BEIJING ZHANCHEN CHEM
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