Manufacturing method of powdery thermoplastic polyurethane urea resin

A technology of polyurethane urea and manufacturing method, which is applied in the direction of coating, etc., can solve the problems of poor melt moldability, blooming, difficulty in controlling the molecular weight of resin, etc., and achieve the effect of excellent melt moldability and excellent mechanical properties

Inactive Publication Date: 2010-11-17
NIPPON POLYURETHANE IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, in the production process of powdery thermoplastic polyurethane urea resin, there is such a problem: due to the partial reaction of isocyanate and water (the urea bond generated by the reaction of isocyanate and water exists locally due to its strong hydrogen bond force, which promotes local urea reaction, etc.), forming a refractory substance with an excessively large molecular weight (in gel permeation chromatography (hereinafter, referred to as "GPC"), a refractory substance that can be observed at a position that should have an ultrahigh molecular weight outflow), the powdery thermoplastic polyurethane urea resin containing the refractory substance has poor melt moldability
[0009] In addition, in the method of reacting the isocyanate group part of the isocyanate group-terminated prepolymer with a low-molecular polyol and the like, and then reacting the remaining isocyanate group part with water, there is a problem that it is difficult to pass the isocyanate group. Control the molar ratio of the active hydrogen group to control the molecular weight of the resin (the molecular weight design method that was often used in the past)
This is because the water is partially evaporated during the reaction, or it is used for side reactions, and the active hydrogen group of the specified amount (equivalent to the residual isocyanate group) cannot be reliably reacted with the residual isocyanate group.
[0010] On the other hand, in moldings of thermoplastic resins, blooming may occur over time

Method used

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  • Manufacturing method of powdery thermoplastic polyurethane urea resin
  • Manufacturing method of powdery thermoplastic polyurethane urea resin
  • Manufacturing method of powdery thermoplastic polyurethane urea resin

Examples

Experimental program
Comparison scheme
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Embodiment

[0273] Hereinafter, examples of the present invention will be described, but the present invention is not limited to these examples.

[0274] [Preparation example 1 (preparation of dispersant solution)]

[0275] Add 762 grams of adipic acid, 49 grams of maleic anhydride and 386 grams of ethylene glycol into a reaction vessel with a capacity of 2 liters that is equipped with a stirrer, a thermometer, a distillation tower and a nitrogen gas introduction pipe, and nitrogen gas is fed while Stir at 150°C under normal pressure to carry out esterification reaction.

[0276] When no condensation water was confirmed, 0.1 g of tetrabutyl titanate was added, and the pressure in the reaction system was slowly reduced to 0.07 kPa. At the same time, the temperature was slowly raised to 190° C. to continue the reaction, thereby obtaining polyester. The obtained polyester had a number average molecular weight of 2,000 and an iodine value of 12.7 g I / 100 g.

[0277] Then, 74 grams of the ab...

Embodiment I-1

[0281] (1) The first process

[0282] 756.9 g of a polyester diol (EA-2000) with a number average molecular weight of 2,000 obtained from ethylene glycol and adipic acid, and 133.6 g of a polymer with a number average molecular weight of 1,500 obtained from 1,6-HD and phthalic acid Ester diol (HoP-1500), 7.4 g of dispersant solution (1), and 818.2 g of isooctane "Kyowa Gel C-800" (manufactured by Kyowa Hakka Chemical Co., Ltd.) as a non-aqueous dispersion medium are put into the device Stir at 90-95°C for one hour in a reaction vessel with a capacity of 3L, equipped with a stirrer, a thermometer, a distillation column, and a nitrogen gas introduction pipe, thereby making the polymer polyol (a) (EA-2000 and Hop-1500) Disperse in isooctane to prepare non-aqueous dispersion.

[0283] (2) The second process

[0284] 102.2 g of hexamethylene diisocyanate (HDI) as organic polyisocyanate (b) and 0.050 g of bismuth-based catalyst "NEOSTANN U-600" (Nitto Kasei Co., Ltd.) reacted the...

Embodiment I-2-I-15

[0299] Through the following steps 1 to 4, various powdery thermoplastic polyurethane urea resins are prepared.

[0300] (1) The first process

[0301] According to the formula shown in the following table 1, except that the polymer polyol (a), dispersant solution, and non-aqueous dispersion medium (isooctane) are loaded into the reaction vessel, the other is the same as the first process of embodiment I-1, and the preparation non-aqueous dispersion. Again, in embodiment I-2, use 75.0 grams of plasticizers "PEG400 dibenzoate" obtained by polyethylene glycol 400 (1 mole) and benzoic anhydride (2 moles); In 5, use plasticizer "PEG200 dibenzoate" 50.0 g obtained from plasticizer "PEG400 dibenzoate", polyethylene glycol 200 (1 mole) and benzoic anhydride (2 mole) Gram; In embodiment I-11, use plasticizer " PEG200 dibenzoate " 50.0 grams.

[0302] (2) The second process

[0303] According to the formula shown in Table 1 below, except that HDI and a catalyst were added to the di...

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Abstract

It is intended to provide a process for producing a powdered thermoplastic polyurethane urea resin comprising the steps of forming a prepolymer with an isocyanate group at an end by reacting a polymer polyol (a), an organic polyisocyanate (b), a monofunctional active hydrogen group-containing compound (c) and preferably further a bifunctional active hydrogen group-containing compound (d) at a specific ratio and forming a polyurethane urea resin by carrying out a chain extension reaction of the prepolymer with an isocyanate group at an end and water (e) in a non-aqueous dispersion solvent. According to this production process, the powdered thermoplastic polyurethane urea resin excellent in melt moldability can be obtained and the control of the molecular weight of the polyurethane urea resin is easy.

Description

technical field [0001] The present invention relates to a method for producing a powdery thermoplastic polyurethane-urea resin suitable for slush molding and the like. Background technique [0002] The solidified shell molding method is widely used for automotive interior materials and the like because it can be effectively used for molding products with complex shapes and uniform wall thickness. [0003] Recently, as a solid shell molding material, a powdery thermoplastic polyurethane urea resin having excellent flexibility is used. [0004] As a method for producing a powdered polyurethane resin (polyurethaneurea resin) for solid shell molding that can obtain a molded product that is less prone to blooming and less prone to wrinkling, the present applicant has proposed the following production method: A step in which an isocyanate group-terminated prepolymer in a non-aqueous dispersion medium reacts with water to cause chain extension (see Patent Document 1). [0005] Al...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/65B29C41/18C08G18/10
Inventor 林政浩喜多求手钱英之南有里子
Owner NIPPON POLYURETHANE IND CO LTD
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