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Polyurethane aqueous dispersion and preparation method thereof

A technology of polyurethane water dispersion and polyurethane prepolymer, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the difficulty of source of sulfonic acid type hydrophilic chain extender and the difficulty of large-scale industrial production , PUD solid content is not high and other problems, to achieve the effect of low preparation cost, broaden the source of synthetic raw materials, good storage stability

Inactive Publication Date: 2015-01-28
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing PUD synthesis often uses dimethylolpropionic acid (DMPA) or sulfonate compound as a hydrophilic chain extender. Among them, DMPA has a high melting point and low solubility, and N-methylpyrrolidone (NMP), which has a high boiling point and is toxic, is required. Dissolved, and the solid content of the prepared PUD is not high, the residual toxic NMP is not easy to remove, and the product is not environmentally friendly; the source of the sulfonic acid type hydrophilic chain extender is difficult, and the preparation process of the sulfonate containing the amino group is more complicated and large-scale Industrial production is more difficult
When using non-ionic polyoxyethylene ether to prepare PUD, the amount of hydrophilic components added is large, and the hardness of PUD coating film is low
In addition, the chemical resistance of PUD coatings, especially alcohol resistance, is generally poor, and these defects greatly limit the popularization and application of PUD.

Method used

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  • Polyurethane aqueous dispersion and preparation method thereof
  • Polyurethane aqueous dispersion and preparation method thereof
  • Polyurethane aqueous dispersion and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) In a dry flask equipped with an electric stirrer and a thermometer, add 1 mole of trimethylolpropane and 1 mole of phthalic anhydride, and heat up to 95°C for 3.5 hours under stirring within 30 minutes. The acid value of the reaction system was measured by GB / T601-1998. After the acid value reached the theoretical value, the reaction was stopped, the temperature was lowered to 50°C, and the material was discharged to obtain a new carboxylate hydrophilic monomer. The obtained hydrophilic compound is separated through a silica gel column, and the monoesterification component is collected, and the solvent is removed by a rotary evaporator to obtain the target carboxylic acid type hydrophilic chain extender trimethylolpropane phthalate monoester (TMPPs) .

[0035] Its reaction formula is as follows:

[0036]

[0037] The purified TMPPs were dissolved using a deuterated DMSO reagent, and nuclear magnetic resonance analysis was performed. figure 1 for TMPPs 1 H-NMR,...

Embodiment 2

[0049] (1) In a dry flask equipped with an electric stirrer and a thermometer, add 1 mole of trimethylolpropane and 0.85 mole of tetrahydrophthalic anhydride, and raise the temperature to 90°C for 4 hours under stirring within 30 minutes. The acid value of the reaction system was measured by GB / T601-1998. After the acid value reached the theoretical value, the reaction was stopped, the temperature was lowered to 50°C, and the material was discharged to obtain a new carboxylate hydrophilic monomer.

[0050] (2) The dosage of each component of polyurethane prepolymer:

[0051] table 3

[0052]

[0053] In a reaction kettle equipped with a stirring blade, a thermometer and a condenser, add polybutadiene diol, a hydrophilic chain extender trimethylolpropane tetrahydrophthalate monoester and a diisocyanate monomer hexacyclohexyl Diisocyanate, heat up to about 75°C, keep warm for 1.5 hours; add small molecule diol chain extender hexylene glycol, non-ionic hydrophilic chain exten...

Embodiment 3

[0058] (1) In a dry flask equipped with an electric stirrer and a thermometer, add 1 mole of trimethylolpropane and 1.25 moles of succinic anhydride, and raise the temperature to 100°C for 3 hours under stirring within 30 minutes. The acid value of the reaction system was measured by GB / T601-1998. After the acid value reached the theoretical value, the reaction was stopped, the temperature was lowered to 50°C, and the material was discharged to obtain a new carboxylate hydrophilic monomer.

[0059] (2) The dosage of each component of polyurethane prepolymer:

[0060] table 5

[0061]

[0062] In the reaction kettle equipped with stirring blade, thermometer and condenser, add polymer diol T-1136 polyester diol and N210 polyether diol, carboxylic acid type hydrophilic chain extender trimethylolpropane butane Diacid monoester and diisocyanate monomer diphenylmethane diisocyanate, heat up to about 75°C, keep warm for 2.0 hours; add small molecule diol chain extender propylene ...

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Abstract

The invention discloses a polyurethane aqueous dispersion and a preparation method thereof. The preparation method comprises the following steps: firstly, mixing trimethylolpropane or glycerol and acid anhydride and preparing a carboxylic acid type hydrophilic monomer; on the basis of molar parts, adding 20-60 parts of polymer dibasic alcohol, 4-10 parts of carboxylic acid type hydrophilic monomer and 30-60 parts of a diisocyanate monomer into a reactor, heating to 60 DEG C-100 DEG C and carrying out heat preservation; adding1-10 parts of small-molecular dibasic alcohol, 2-10 parts of a non-ionic hydrophilic chain extender and 1-6 parts of a cross-linking agent and reacting until the content of NCO is less than 5%; and adjusting the viscosity of the reactant, cooling, adding a neutralizing agent for neutralizing, adding water for emulsifying, adding an amine chain extender and removing the solvent by distillation to obtain the polyurethane aqueous dispersion. The carboxylic acid type hydrophilic monomer has stable performance and low cost, the polyurethane aqueous dispersion prepared from the carboxylic acid type hydrophilic monomer has high content of solids and the coating has relatively high hardness and excellent chemical product resistance.

Description

technical field [0001] The invention belongs to the field of organic high-molecular polymers, relates to high-molecular compounds using isocyanate, in particular to a preparation method and application of polyurethane aqueous dispersions. technical background [0002] Polyurethane aqueous dispersion (PUD) has the advantages of safety, non-toxicity and environmental protection, and is widely used in the fields of coatings, adhesives, leather finishing agents and inks. The existing PUD synthesis often uses dimethylolpropionic acid (DMPA) or sulfonate compound as a hydrophilic chain extender. Among them, DMPA has a high melting point and low solubility, and N-methylpyrrolidone (NMP), which has a high boiling point and is toxic, is required. Dissolved, and the solid content of the prepared PUD is not high, the residual toxic NMP is not easy to remove, and the product is not environmentally friendly; the source of the sulfonic acid type hydrophilic chain extender is difficult, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/66C08G18/42C08G18/48C08G18/44C08G18/62C08G18/34C08G18/12C07C67/08C07C69/80C07C69/75C07C69/40C07C69/60
Inventor 瞿金清朱延安
Owner SOUTH CHINA UNIV OF TECH
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