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A kind of phthalocyanine metal salt modified polyol and its preparation method and application

A technology of polyols and metal salts, applied in the field of polyols, to achieve the effect of simple process and increased use temperature

Active Publication Date: 2022-05-13
南通北风橡塑制品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the existing polyurethane elastomer preparation technology, metal phthalocyanine salts are usually only used as pigments

Method used

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  • A kind of phthalocyanine metal salt modified polyol and its preparation method and application
  • A kind of phthalocyanine metal salt modified polyol and its preparation method and application
  • A kind of phthalocyanine metal salt modified polyol and its preparation method and application

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preparation example Construction

[0046] In a second aspect, the present application provides a method for preparing the above-mentioned metal phthalocyanine salt modified polyol, the preparation method comprising the following steps:

[0047] S1: In an inert atmosphere, and in the presence of a first basic catalyst, reacting 4-nitrophthalonitrile and a polyhydric alcohol in a first organic solvent at a first reaction temperature for a first predetermined period of time, obtaining phthalonitrile-terminated polyols; and

[0048] S2: In an inert atmosphere and in the presence of a second basic catalyst, make phthalonitrile, the metal salt and the phthalonitrile-terminated polyol obtained in step S1 in a second organic reacting in a solvent at a second reaction temperature for a second predetermined period of time to obtain the metal phthalocyanine salt-modified polyol.

[0049] In a specific embodiment, the preparation method of metal phthalocyanine salt modified polyol described herein comprises K 2 CO 3 , 4...

Embodiment 1

[0084] Will K 2 CO 3 (82.8g, 0.6mol), 4-nitrophthalonitrile (51.9g, 0.3mol) and PCL205U (633.6g, 1.2mol) were added to the reaction flask, under the protection of nitrogen, heated to 60 ° C, stirred for 24 Hour. After the reaction finishes, add phthalonitrile (38.4g, 0.3mol), ZnCl 2 (40.8g, 0.3mol), DBU (300ml) and DMF (800ml), the mixture was heated to 150°C under nitrogen protection and kept for 8 hours. After the reaction, cool to room temperature, first add water to precipitate, and wash the filtered solid with water until neutral. The solid was redissolved with ethyl acetate, the insolubles were filtered off, and then ethanol was added for precipitation. The filtered solid was dried in a vacuum oven to obtain zinc phthalocyanine modified polycaprolactone polyol (342.0g), and the hydroxyl value was measured It is 58.2mgKOH / g.

Embodiment 2

[0086] Will K2 CO 3 (82.8g, 0.6mol), 4-nitrophthalonitrile (51.9g, 0.3mol and BDO (108.1g, 1.2mol) were dissolved in DMF (800ml), under nitrogen protection, heated to 60 ° C, stirred Reaction 24 hours. After the reaction finishes, add phthalonitrile (38.4g, 0.3mol), ZnCl 2 (40.8g, 0.3mol), DBU (300ml), and the mixture was heated to 150°C under nitrogen protection for 8 hours. After the reaction, cool to room temperature, first add water to precipitate, and wash the filtered solid with water until neutral. The solid was re-dissolved with DMF, and then ethanol was added for precipitation. The filtered solid was dried in a vacuum oven to obtain butanediol-grafted zinc phthalocyanine (153.4 g), and the measured hydroxyl value was 152.1 mgKOH / g.

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Abstract

The application relates to a phthalocyanine metal salt modified polyol, which is obtained by reacting 4-nitrophthalonitrile, phthalonitrile, metal salt and starting polyol; the general structural formula of the metal salt for MX 2 , wherein M represents a divalent metal cation, and X represents a monovalent non-metal anion; the general structural formula of the starting polyol is HO‑R 1 -OH,R 1 Represents the carbon chain structure between the two terminal hydroxyl groups in the starting polyol with more than 2 carbon atoms; the polyalcohol modified by the metal phthalocyanine salt has a structure shown by the following general formula (1): The invention relates to the preparation method of the above-mentioned metal phthalocyanine salt modified polyol and its application in the preparation of polyurethane elastomer. The phthalocyanine-modified polyurethane elastomer prepared by using the phthalocyanine metal salt-modified polyol of the present application has relatively high heat resistance.

Description

technical field [0001] The present application relates to the technical field of polyols, in particular to a phthalocyanine metal salt-modified polyol and a preparation method thereof. Background technique [0002] Polyols may include small molecule polyols, polyether polyols, polyester polyols, and the like. The polyester polyol may include conventional polyester polyols, polycaprolactone polyols, and polycarbonate diols, which contain ester groups (COO) or carbonate groups (OCOO). Conventional polyester polyols are usually polyester polyols obtained by polycondensation reactions of dibasic carboxylic acids and diols. According to whether the polyester polyol structure contains benzene rings, conventional polyester polyols can be divided into aliphatic polyester polyols and aromatic polyester polyols. Common aliphatic polyester polyols include adipic acid-based polyester diols, and common aromatic polyester polyols include polyphthalic acid-based polyester polyols. Polye...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/333C08G65/328C08G65/338C08G63/91C08G64/42C08G18/66C08G18/10C08G18/12C08G18/32C08G18/42C08G18/48C07D487/22
CPCC08G65/33375C08G65/33396C08G65/328C08G65/338C08G63/912C08G64/42C08G18/664C08G18/10C08G18/12C08G18/3897C08G18/4277C08G18/4854C08G18/6633C08G18/6674C07D487/22C08G18/3206
Inventor 朱勇健李俊
Owner 南通北风橡塑制品有限公司