Method for preparing high-stability caprolactam blocking isocyanate binder emulsion

A technology of blocking isocyanate and caprolactam, which is applied in polyurea/polyurethane adhesives, adhesive types, adhesives, etc., can solve problems such as poor stability and short settling time, and achieve high stability, good dispersion, and improved The effect of stability and dispersion effect

Inactive Publication Date: 2008-08-27
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at the problems of poor stability and short settling time in existing adhesive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] First, caprolactam was dehydrated in vacuum at room temperature for three hours; after toluene was added with molecular sieve, sealed and stirred overnight, anhydrous calcium chloride was added to remove water by distillation. Then, 37.38 g (0.33 mol) caprolactam and 80 ml of toluene were added to a 250 ml three-necked flask with magnetic stirring, a condenser was installed, and nitrogen protection was carried out, and the temperature of the oil bath was 60-80 °C. 37.5g (0.15mol) MDI (in order to ensure that MDI can be completely capped, the molar ratio of caprolactam and MDI should be greater than 2, preferably around 2.2) and 64.95ml toluene are mixed into a solution, and then slowly added dropwise with a constant pressure funnel In a three-necked bottle, the dropwise addition was completed within 30 minutes. Then, the reaction is carried out at 60-80° C. for 5-7 hours, and the reaction process is always carried out under the protection of nitrogen. Finally, after th...

Embodiment 2

[0020] 100 g of caprolactam-terminated MDI white solid (prepared according to the method described in Example 1, the same in the following examples) was added to the grinding jar, and pre-milled for 7 minutes to make it a uniform white powder. 3.0 g of polyethylene glycol and 106 ml of distilled water were heated to 80-90° C. in a water bath. After the polyethylene glycol was completely dissolved, the solution was added to the grinding jar. Then add 0.5 g polyethylene glycol octyl phenyl ether, 1.0 g sodium lauryl sulfate, 0.3 g sodium butylnaphthalene sulfonate and 1.2 g modified polysiloxane defoamer to the grinding jar, and then add After grinding for 1.5 hours, sieve, and the obtained white emulsion is the binder emulsion.

[0021] The adhesive emulsion is a white suspension with a solid content of 49.43%, and the viscosity is appropriate. No obvious sedimentation and stratification occurs after the emulsion is stored for one month. The caprolactam-terminated MDI was unif...

Embodiment 3

[0023] 100 g of caprolactam-terminated MDI white solid was added to the milling jar and pre-milled for 15 minutes to make it a homogeneous white powder. 3.0 g of polyethylene glycol and 106 ml of distilled water were heated to 80-90° C. in a water bath. After the polyvinyl alcohol was completely dissolved, the solution was added to the grinding jar. Then add 1.45g of sodium cetyl sulfonate, 0.55g of sodium butylnaphthalene sulfonate and 0.8g of polyether defoamer into the grinding jar, grind for 2.5 hours and then sieve, and the obtained white emulsion is viscous Mixture lotion.

[0024] The adhesive emulsion is a white suspension with a solid content of 50.27%, and the viscosity is appropriate. No obvious sedimentation and stratification occurs after the emulsion is stored for one month. The caprolactam-terminated MDI was uniformly distributed in the emulsion without aggregation, and the average particle size was about 2 microns.

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Abstract

The invention discloses a process for preparing caprolactam end capping isocyanate binder emulsion, which comprises the following steps: firstly, dewatering caprolactam with vacuum under constant temperature, distilling toluene to remove water after adding molecular sieve, secondly, making caprolactam which is dried and toluene into solution to add into a three-necked bottle with a stirring condensing device, dripping toluene solution of 4, 4-diphenylmethane diisocyanate, scouring white solid which is obtained under reaction with nitrogen protection, and obtaining 4, 4-diphenylmethane diisocyanate of caprolactam end capping after vacuum drying, thirdly, milling the white solid of 4, 4-diphenylmethane diisocyanate of caprolactam end capping for 7-15 minutes, then adding host stabilizer, viscosity controlling stabilizer, defoaming agent and water, and obtaining lacte suspending liquid which is obtained through dispersion after 1.5-2.5 hours of milling, namely binder emulsion. The binder emulsion which is prepared by the invention has appropriate emulsion viscosity and settling rate, high stability and excellent dispersibility, and meets application requirements.

Description

technical field [0001] The invention relates to a preparation method of a high-stability caprolactam-terminated isocyanate adhesive emulsion. Background technique [0002] Cord fabric is one of the necessary materials for the production of various tires. The "three major pieces" of tire materials are rubber, carbon black and cord fabric, of which cord fabric accounts for about 60% of the total cost, which shows the important position of cord fabric in tire manufacturing. With the improvement of the "meridian" rate of car tires, polyester (also known as: polyester fiber) cord fabric, which is one of the ideal skeleton materials for radial tires, has developed rapidly. The main characteristics of polyester cord fabric are high modulus and low elongation, so the dimensional stability of the tire is good and the deformation is small. These properties are far superior to nylon. In the rubber products such as passenger car tires, V-belts, coal mine conveyor belts, high-pressure ...

Claims

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Application Information

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IPC IPC(8): C08G18/02C09J175/00
Inventor 曾钫陈启明
Owner SOUTH CHINA UNIV OF TECH
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