Ionic waterborne curing agent based on bio-based pentamethylene diisocyanate and preparation method thereof

A technology of pentamethylene diisocyanate and water-based curing agent, applied in the field of ionic water-based curing agent and its preparation, can solve the problems of the influence of hydroxyl components on film formation, complicated production and preparation process, and large environmental pollution, and achieve curing Fast speed, easy to master operation process, good compatibility effect

Inactive Publication Date: 2019-10-29
CNOOC CHANGZHOU PAINT & COATINGS IND RES INST +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, on the one hand, the viscosity of hexamethylene diisocyanate becomes very large after modification, and in some fast-drying occasions, polyisocyanate trimers with more polymers and higher viscosity are used, which are difficult to disperse in water , the film formation of the hydroxyl group will also be affected; on the other hand, the synthesis process of hexamethylene diamine, the precursor of hexamethylene diisocyanate, relies on fossil resources and requires highly toxic cyanide as a raw material. The production process is complicated and pollutes the environment. It is very large, so it is necessary to develop an environmentally friendly and excellent performance ionic water-based curing agent preparation method

Method used

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  • Ionic waterborne curing agent based on bio-based pentamethylene diisocyanate and preparation method thereof
  • Ionic waterborne curing agent based on bio-based pentamethylene diisocyanate and preparation method thereof
  • Ionic waterborne curing agent based on bio-based pentamethylene diisocyanate and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0037] The preparation method of the ionic water-based curing agent based on bio-based pentamethylene diisocyanate of the present embodiment may further comprise the steps:

[0038] 1) The bio-based pentamethylene diisocyanate trimer is subjected to vacuum distillation with a rotary evaporator at a pressure of 20 mbar and a temperature of 170° C. to remove impurities and free monomers therein to obtain the impurity-removed Bio-based pentamethylene diisocyanate trimer;

[0039] 2) Add 120g of bio-based pentamethylene diisocyanate trimer, 5.8g of 2-cyclohexylaminoethanesulfonic acid, 2.58g of N,N-dimethyl Cyclohexylamine, then stirred and raised to 80°C under nitrogen atmosphere to fully react for 5 hours, and when the product in the bottle was clear and transparent, the temperature was lowered to 25°C, discharged, sampled and titrated to obtain the product.

[0040] The calculated -NCO content of the bio-based pentamethylene diisocyanate ionic water-based curing agent is 22.5%...

Embodiment 2

[0043] The preparation method of the ionic water-based curing agent based on bio-based pentamethylene diisocyanate of the present embodiment may further comprise the steps:

[0044] 1) The bio-based pentamethylene diisocyanate trimer is distilled under reduced pressure with a rotary evaporator at a pressure of 30 mbar and a temperature of 160° C. to remove impurities and free monomers therein to obtain the impurity-removed Bio-based pentamethylene diisocyanate trimer;

[0045] 2) Add 450g of bio-based pentamethylene diisocyanate trimer and 3.5g of dimethylcyclohexylamine after removing impurities in step 1) to the four-necked flask, and then add 6.3g of 3-cyclohexylaminopropyl During the reaction process, add sulfonic acid into the four-neck flask in batches, then stir and raise the temperature to 110°C for 6 hours in a nitrogen atmosphere to fully react.

[0046] The -NCO content of the bio-based pentamethylene diisocyanate-based ionic water-based curing agent obtained in th...

Embodiment 3

[0048] The preparation method of the ionic water-based curing agent based on bio-based pentamethylene diisocyanate of the present embodiment may further comprise the steps:

[0049] 1) The bio-based pentamethylene diisocyanate trimer (Mitsui Chemicals) was subjected to vacuum distillation with a rotary evaporator at a pressure of 25 mbar and a temperature of 170 ° C to remove impurities and free monomers therein, Obtain bio-based pentamethylene diisocyanate trimer after impurity removal;

[0050] 2) Add 200g of the bio-based pentamethylene diisocyanate trimer, 4.5g of sodium cyclamate, and 3.2g of o-toluidine to the four-necked flask after removing impurities in step 1), and then in a nitrogen atmosphere Under stirring, raise the temperature to 70°C and fully react for 7 hours. When the reactants in the bottle are clear and transparent, cool down to 30°C, discharge the material, take a sample for titration, and obtain the product.

[0051] The -NCO content of the bio-based pe...

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Abstract

The invention relates to the technical field of curing agents, specifically to an ionic waterborne curing agent based on bio-based pentamethylene diisocyanate and a preparation method thereof. The preparation method for the ionic waterborne curing agent based on the bio-based pentamethylene diisocyanate provided by the invention comprises the following steps: mixing an impurity-removed bio-based pentamethylene diisocyanate trimer, a sulfamic acid substance and organic amine, then carrying out heating to 60 DEG C to 110 DEG C under the protection of nitrogen, carrying out a reaction for 3 to 7hours, and when a product is transparent, carrying out cooling to 25 DEG C to 40 DEG C. The preparation method provided by the invention has the following advantages: the process of synthesis is simple; the flow of operation is easy to be mastered; the raw material namely the bio-based pentamethylene diisocyanate trimer has a clean source and is free of pollution to the environment; and through addition of a small amount of sulfonate and the organic amine, the ionic waterborne curing agent with a solid content of 100%, an NCO content of up to 22.3%, low viscosity and rapid curing rate can be obtained.

Description

technical field [0001] The invention relates to the technical field of curing agents, in particular to an ionic water-based curing agent based on bio-based pentamethylene diisocyanate and a preparation method thereof. Background technique [0002] In the field of research and development and utilization of coating products, polyurethane coatings have very prominent performance advantages and application value. Two-component polyurethane coatings are widely used in various occasions due to their excellent chemical properties, tolerance, and coating hardness. With the increasing awareness of environmental protection, water-based coatings with very few volatile organic compounds have been vigorously developed. Greening the coatings industry has become an inevitable trend. Water-based coatings, adhesives, inks and leather have developed rapidly. Water-based polyurethane curing agents With the research and application of water-based polyurethane has been vigorously developed. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/79C09D175/04
CPCC08G18/792C09D175/04
Inventor 谭伟民雒新亮史立平刘仲阳郁飞何毅
Owner CNOOC CHANGZHOU PAINT & COATINGS IND RES INST
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