Preparation method of trichlorophenol blocked isocyanate prepolymer micelle

A technology of blocked isocyanate and trichlorophenol, which is applied in the direction of adhesives, adhesive types, polyurea/polyurethane coatings, etc., and can solve problems such as limiting the application of low-temperature bonding occasions

Inactive Publication Date: 2013-10-09
NORTHEAST FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, blocking isocyanate prepolymers with a higher R (molar ratio of isocyanate to hydroxyl) value can be stable in aqueous solution and maintain activity while deblocking reaction at lower temperature requirements (<120°C) has become a research problem.
It has been reported that blocked isocyanate prepolymer micelles can be stable for more than three months when the R value is low (≤2.5), but the unblocking temperature is above 120 ° C, which greatly limits the application of low temperature bonding occasions

Method used

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  • Preparation method of trichlorophenol blocked isocyanate prepolymer micelle
  • Preparation method of trichlorophenol blocked isocyanate prepolymer micelle
  • Preparation method of trichlorophenol blocked isocyanate prepolymer micelle

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specific Embodiment approach 1

[0026] Embodiment 1: The isocyanate in this embodiment is hexamethylene diisocyanate (HDI), and the preparation method of trichlorophenol-blocked isocyanate prepolymer micelles is carried out according to the following steps:

[0027] Step 1, drying the polyethylene glycol in vacuum at 120° C. for 3 hours;

[0028] Step 2: Add 0.0183mol of polyethylene glycol treated in Step 1, 0.0071mol of 2,2-dimethylolpropionic acid (DMPA), and 10mL of composite solvent into a four-necked flask, and mechanically stir and mix at a speed of 105r / min for 30min , the composite solvent is a mixture of acetone and methyl ethyl ketone at a volume ratio of 1:3, and then nitrogen is passed through at a flow rate of 5mL / min for 30 minutes, heated to 70°C, and kept for 29 minutes;

[0029] Step 3. Add 0.0276 mol of hexamethylene diisocyanate (HDI) dropwise to the four-necked bottle at a rate of 4 drops / s. After the dropwise addition, raise the temperature to 84°C, keep the temperature for 3.2 hours, a...

specific Embodiment approach 2

[0040] Specific embodiment two: The isocyanate of this embodiment is toluene-2,4-diisocyanate (TDI), and the preparation method of trichlorophenol-blocked isocyanate prepolymer micelles is carried out according to the following steps:

[0041] Step 1, drying the polyethylene glycol in vacuum at 120° C. for 3 hours;

[0042] Step 2: Add 0.0169 mol of polyethylene glycol treated in step 1, 0.0106 mol of 2,2-dimethylolpropionic acid (DMPA), and 13 mL of composite solvent into a four-necked flask, and mechanically stir and mix at a speed of 105 r / min for 30 min , the composite solvent is a mixture of acetone and methyl ethyl ketone at a volume ratio of 1:3, and then nitrogen is passed through at a flow rate of 5mL / min for 30 minutes, heated to 70°C, and kept for 25 minutes;

[0043] Step 3. Then add 0.0305 mol of toluene-2,4-diisocyanate (TDI) dropwise to the four-necked bottle at a rate of 2-3 drops / s. After the dropwise addition, the temperature is raised to 80°C, and the temper...

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Abstract

The invention relates to a preparation method of a trichlorophenol blocked isocyanate prepolymer micelle. The invention provides a trichlorophenol blocked isocyanate prepolymer micelle which can be stable in a water solution for more than 3 months under the condition of high R value and can be subjected to unblocking reaction at low temperature (110 DEG C). The method comprises the following steps: 1. carrying out vacuum drying on polyethyleneglycol; 2. mixing and stirring the polyethyleneglycol, DMPA (dimethylolpropionic acid) and a composite solvent, introducing nitrogen, and keeping the temperature to react; 3. dropwisely adding HDI (hexamethylene diisocyanate) or TDI (toluene diisocyanate) to prepare the prepolymer; 4. blocking; 5. emulsifying; and 6. removing the solvent to obtain the trichlorophenol blocked isocyanate prepolymer micelle. The product provided by the invention can be used as an adhesive for artificial boards, a crosslinking agent or a single-component environment-friendly adhesive; and the product can be used in the fields of wood paints, leather coating agents, water-based adhesives and the like, and can also be used in the fields of enamel wires, textiles, leather, paper conditioning agents and the like.

Description

technical field [0001] The invention relates to a preparation method of blocked isocyanate prepolymer micelles. Background technique [0002] Because of its excellent wear resistance, outstanding flexibility, high strength and low temperature resistance, isocyanate compounds can also endow products with strong adhesion, good gloss and excellent solvent resistance, and can be made into various An elastomer material with excellent performance, additives, adhesives, leather finishing agents and coatings. Especially in the field of adhesives and coatings, due to many advantages such as excellent bonding performance, no formaldehyde release, excellent low temperature resistance and aging resistance, and strong adaptability to the materials to be bonded, it has been widely used. However, the isocyanate group is chemically active, easily reacts with water and substances containing active hydrogen, and is very sensitive to moisture. As a result, the prepared isocyanate adhesive is ...

Claims

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Application Information

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IPC IPC(8): C08J3/03C08L75/08C08G18/76C08G18/66C08G18/48C08G18/32C08G18/12C08G18/30C08G18/83C09D175/04C09J175/04
Inventor 李志国邬洪川顾继友
Owner NORTHEAST FORESTRY UNIVERSITY
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