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Preparation method of pyridine sulfonic acid type water-based polyurethane emulsion

A water-based polyurethane, pyridine sulfonic acid technology, applied in the direction of polyurea/polyurethane adhesives, adhesive types, adhesives, etc., can solve the problem of water-based polyurethane crystallization properties, initial viscosity, physical shrinkage resistance, and yellowing resistance. and other problems, to achieve the effect of good resistance to physical shrinkage, improve crystallization performance, and improve initial bond strength

Inactive Publication Date: 2012-08-01
JIAXING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The polyisocyanate and hydrophilic chain extender used in this patent are all aliphatic, therefore, the crystallization performance, initial tack and physical shrinkage resistance of the prepared waterborne polyurethane cannot meet the requirements of waterborne adhesives
In 2007, Sun Yat-sen University's master's degree thesis "Preparation of Water-based Polyurethane Adhesive for Shoes" (Qin Changhuang) reported that water-based polyurethane was prepared by using sulfonic acid-type aromatic ring diamine as a hydrophilic chain extender, and the crystallization performance and initial viscosity were improved. However, due to the use of The hydrophilic chain extender contains a benzene ring structure, so it is not resistant to yellowing

Method used

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  • Preparation method of pyridine sulfonic acid type water-based polyurethane emulsion
  • Preparation method of pyridine sulfonic acid type water-based polyurethane emulsion
  • Preparation method of pyridine sulfonic acid type water-based polyurethane emulsion

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preparation example Construction

[0014] The preparation method of this pyridine sulfonic acid type aqueous polyurethane emulsion comprises the following steps:

[0015] (1) Carry out vacuum dehydration treatment to polyester polyol, then carry out prepolymerization reaction with organic diisocyanate, dimethylol propionic acid (DMPA) in the presence of catalyst, the reaction time is 2~5 hours, preferably 4h; Reaction The temperature is 70-100°C, preferably 75-85°C;

[0016] (2) Cool the prepolymer obtained in the previous step to below 50°C, then dissolve it with acetone, then add a salt-forming reagent to neutralize, and the neutralization time is 10 to 30 minutes;

[0017] (3) Add pyridine sulfonic acid diamine hydrophilic chain extender to the material obtained in the previous step to carry out chain extension reaction to obtain a polymer with an NCO group in the end group. The reaction temperature is 10-60°C, and the reaction time is 0.5- 1h. The described pyridinesulfonic acid diamine hydrophilic chain ...

Embodiment 1

[0036] In the reactor with agitator, thermometer and cooler, add 200g of PBA (the number average molecular weight is 2000), melt at 100~120°C, vacuum dehydrate for 1h, and start to cool down when the moisture content is less than 0.1% by sampling; When the temperature dropped to 80°C, 13.3g IPDI, 19.5g HDI, 11g DMPA and 0.05g DBTDL catalyst were added for prepolymerization reaction, and the prepolymer was obtained after stirring for about 4 hours. Cool the above prepolymer to 50°C, add 170g of acetone to dissolve the prepolymer, then add 0.7g of triethylamine for neutralization, and the neutralization time is 15min; add 4.2g of 2-[6-(2-aminoethylamino) Pyridyl]sodium ethyl sulfonate was subjected to a chain extension reaction, and the reaction time was 0.5h to obtain a polymer with an NCO group in the end group; 210g of deionized water was added to the above polymer, stirred at a high speed to disperse into an emulsion, and then added 1.5g of ethylenediamine was used for secon...

Embodiment 2

[0039]In the reactor with stirrer, thermometer, cooler, add 200g PBA (the number average molecular weight is 2000), melt at 100~120 ℃, vacuum dehydration 1h, begin to cool down when the water content of sampling measurement is less than 0.1%; When the temperature dropped to 80°C, 38.1g IPDI, 3.1g DMPA and 0.05g DBTDL catalyst were added for prepolymerization reaction, and the prepolymer was obtained after stirring for about 4 hours. Cool the above prepolymer to 50°C, add 210g of acetone to dissolve the prepolymer, then add 2.1g of triethylamine for neutralization, and the neutralization time is 15min; add 3.5g of 2-[6-(2-aminopropylamino) Pyridyl]sodium ethyl sulfonate was subjected to a chain extension reaction, and the reaction time was 0.5h to obtain a polymer with an NCO group in the end group; 225g of deionized water was added to the above polymer, stirred at a high speed to disperse into an emulsion, and then added 1.5g of ethylenediamine was used for secondary chain ext...

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Abstract

The invention relates to a preparation method of a pyridine sulfonic acid type water-based polyurethane emulsion, which comprises the following steps: (1) carrying out prepolymerization reaction on polyester polyol, organic diisocyanate and dihydroxymethylpropionic acid in the presence of a catalyst; (2) dissolving in acetone, and neutralizing by adding a salifying reagent; (3) adding a pyridine sulfonic acid diamine hydrophilic chain extender to carry out chain extension reaction, thereby obtaining a polymer of which the terminal group contains an NCO group; (4) adding deionized water, stirring at high speed to be dispersed into an emulsion, and adding low-molecular weight polyamine to carry out secondary chain extension reaction; and (5) distilling under reduced pressure to remove the acetone, thereby obtaining the pyridine sulfonic acid type water-based polyurethane emulsion. Since the diamine containing pyridine sulfonic acid structure is used as the hydrophilic chain extender, the prepared polyurethane emulsion has the advantages of high adhesive strength and yellowing resistance.

Description

technical field [0001] The invention belongs to the field of fine polymers, and relates to a preparation method of pyridinesulfonic acid type water-based polyurethane emulsion. Background technique [0002] As an environmentally friendly polymer material, water-based polyurethane has the characteristics of no solvent, no odor, no pollution, no combustion, easy to mix with other emulsions, and favorable for modification. It has been widely used in adhesives, coatings, and paper coatings. Among the products such as layer, leather finishing agent, fiber or fabric treatment agent, it is most widely used in the field of adhesives and coatings. [0003] U.S. Patent No. 3,036,998 and US No. 3,756,992 once reported the preparation method of water-based polyurethane emulsion, but the solid content of the water-based polyurethane emulsion prepared by this method is relatively low. Due to the slow moisture volatilization rate of low solid content adhesives, many times of gluing, stora...

Claims

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Application Information

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IPC IPC(8): C08G18/66C08G18/42C08G18/32C08G18/12C09J175/06
Inventor 屠晓华吴建一沈连根徐欣欣张洋郦聪
Owner JIAXING UNIV
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