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Preparation method of polybutadiene modified polyurethane-acrylate emulsion

A technology of polybutadiene and acrylate, which is applied in the field of polymer material preparation, can solve the problems of low terminal double bond activity, high tendency of polymerization, and low monomer conversion rate, so as to improve and reduce the monomer conversion rate. Tendency to phase separation, high mechanical strength effect

Active Publication Date: 2015-11-11
阜阳市华轩睿创生产力促进中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the impact of the polyurethane segment on the terminal double bond, the activity of the terminal double bond is low, the tendency of polymerization between unsaturated monomers is large, and the generated PUA copolymer is less, and the product actually contains a small amount of PUA copolymer, polyurethane and Polyacrylate mixture, poor compatibility between polymers
Moreover, the polyurethane-acrylic ester copolymer obtained by this method is a linear block copolymer, which has great deficiencies in water resistance and mechanical strength.
In addition, in the soap-free emulsion polymerization, because the monomer swells into the interior of the colloidal particles, the water-soluble initiator is used alone, the conversion rate of the monomer is low, and the amount of gel in the polymerization process is high

Method used

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  • Preparation method of polybutadiene modified polyurethane-acrylate emulsion
  • Preparation method of polybutadiene modified polyurethane-acrylate emulsion
  • Preparation method of polybutadiene modified polyurethane-acrylate emulsion

Examples

Experimental program
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Embodiment 1

[0026] Embodiment 1: Preparation of polybutadiene modified polyurethane-acrylate emulsion

[0027] in N 2 Under protection, in a reaction vessel with a reflux condenser and a thermometer, add isophorone diisocyanate (IPDI) 57g, polybutylene adipate diol with a hydroxyl value equal to 55mgKOH / g after vacuum dehydration (PBA) and hydroxyl-terminated polybutadiene (HTPB) 50g each, react at a constant temperature of 90°C for 1.5h under mechanical stirring; cool down to 50°C, add 8.5g of dimethylolpropionic acid (DMPA) Diol (DEG) 6.2g, 3 drops of dibutyltin dilaurate (T-12) and 1 drop of stannous octoate (T-9), styrene 15g, butyl acrylate 5g, continue to react at 75°C for 3h, add Dissolve 15g of methyl methacrylate (MMA) and 5g of butyl acrylate (BA) with 0.05g of azobisisobutylcyanide (AIBN), stir evenly, and add 6.4g of triethylamine under high shear force to neutralize After 1 minute, under high-speed stirring, add 250 g of deionized water below 15 °C and 50 g of an aqueous so...

Embodiment 2

[0029] Embodiment 2: the preparation of polybutadiene modified polyurethane-acrylate emulsion

[0030] in N 2Under protection, in a reaction vessel with a reflux condenser and a thermometer, add 45g of isophorone diisocyanate (IPDI), and 80g of hydroxyl-terminated polybutadiene (HTPB) with a hydroxyl value equal to 110mgKOH / g after vacuum dehydration , react at a constant temperature of 85°C for 2 hours under mechanical stirring; cool down to 50°C, add 8.5g of dimethylolpropionic acid (DMPA), 3 drops of dibutyltin dilaurate (T-12) and 1 drop of stannous octoate ( T-9), styrene 15g, butyl acrylate 5g, continue to react at 70°C for 3.5h, cool down, add 5g of methyl methacrylate (MMA) dissolved in 0.05g of azobisisobutylcyanide (AIBN), butyl acrylate Esters (BA) 15g, stir evenly, add 7.4g of triethylamine under high shear force to neutralize for 1min, add 250g of deionized water below 15°C successively under high-speed stirring, dissolve 12.8g of isophorone di Aqueous solution ...

Embodiment 3

[0032] Embodiment 3: the preparation of polybutadiene modified polyurethane-acrylate emulsion

[0033] in N 2 Under protection, in a reaction vessel with a reflux condenser and a thermometer, add 78g of dicyclohexylmethane diisocyanate (HMDI), and 50g of polycaprolactone diol (PCL) with a hydroxyl value equal to 110mgKOH / g after vacuum dehydration 20g of hydroxyl-terminated polybutadiene (HTPB) with a hydroxyl value equal to 55mgKOH / g was reacted at a constant temperature of 90°C for 1.5h under mechanical stirring; the temperature was lowered to 50°C, and 7.2g of dimethylolbutyric acid (DMBA) was added, 1 , 4-butanediol (BDO) 6.5g, 3 drops of dibutyltin dilaurate (T-12), styrene 15g, butyl acrylate 5g, heat up to 65°C and continue the reaction for 3.5h, add dissolved 0.05g Benzoyl oxide (BPO) styrene 15g, stir evenly, add triethylamine 6.4g under high shear force for neutralization for 1min, then add 250g deionized water below 15°C under high speed stirring, dissolve 12.7 50...

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Abstract

The invention discloses a preparation method of a polybutadiene modified polyurethane-acrylate emulsion, belonging to the technical field of preparation of high polymer materials. A synthetic process comprises the following steps: firstly prepolymerizing hydroxy-terminated polybutadiene with oligomer polyols, diisocyanate and polyhydric alcohol chain extenders, then adding unsaturated monomers dissolved with an initiator to decrease the viscosity of a system, adding water to carry out emulsification, carrying out chain extension so as to obtain a polybutadiene modified polyurethane emulsion containing the unsaturated monomers and an oil-soluble initiator, and carrying out in-situ soap-free emulsion polymerization, so as to prepare polybutadiene modified polyurethane-acrylate emulsion. The emulsion prepared emulsion prepared by virtue of the preparation method has the advantages of good stability, high solid content, low VOC content, low gel content and the like; materials prepared from the emulsion have high consistency and good low temperature resistance and water resistance and can be widely applied to the fields of coatings, leather finishing agents, additives and the like, and the adhesive force to nonpolar substrates is very strong.

Description

technical field [0001] The invention relates to the technical field of preparation of polymer materials, in particular to a preparation method of polybutadiene-modified polyurethane-acrylate emulsion. Background technique [0002] Polyurethane-acrylate emulsion (PUA) is prepared by chemical copolymerization or physical blending of polyurethane (PU) and polyacrylate (PA), because it has excellent wear resistance, toughness and adhesion of polyurethane It is known as "the third generation of water-based polyurethane" because of its mechanical strength and good weather resistance of acrylate. At present, most of the PUA emulsions are prepared by chemical copolymerization by first synthesizing vinyl-terminated PU emulsions, and then using the PU emulsions as seeds to carry out acrylate seed emulsion polymerization. For example, Yang Jianjun of Anhui University and others used hydroxypropyl methacrylate (HPMA)-terminated polyurethane (PU) emulsion as the seed emulsion, ammonium ...

Claims

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Application Information

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IPC IPC(8): C08F283/00C08F212/08C08F220/18C08F220/14C08F2/22C08G18/75C08G18/42C08G18/62
Inventor 高明志
Owner 阜阳市华轩睿创生产力促进中心有限公司