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Silicon-containing polyester polyol and preparation method thereof

A technology of polyester polyol and silicon polyester, applied in the field of polyester polyol, can solve the problems of difficulty in obtaining modification effect, many process steps, poor compatibility, etc., and achieve good heat resistance, high purity, and improved mechanical properties. performance effect

Active Publication Date: 2020-08-14
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Polyorganosiloxane usually has poor compatibility with polymer materials, and it is difficult to obtain a good modification effect
Patent CN 108047451 A discloses a synthesis method of grafted polycaprolactone-modified polyorganosiloxane, but the synthesis route involves many process steps, the operation is very complicated, and a large amount of organic solvent is used

Method used

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  • Silicon-containing polyester polyol and preparation method thereof
  • Silicon-containing polyester polyol and preparation method thereof
  • Silicon-containing polyester polyol and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-7

[0040] The synthesis of embodiment 1-7 silicon-containing initiator

[0041] The hydroxy group of butenol is protected by benzyl bromide to obtain butenol benzyl ether. The hydroxyl protection method is a well-known method in the industry, for details, please refer to Bull.Chem.Soc.Jpn.1987,60,1529. Under nitrogen protection and the reaction temperature of 50-80 ℃, the terminal hydrogen polysiloxane of butenyl alcohol benzyl ether and equimolar amount is in Castel catalyst (add-on: embodiment 1-3 is 30ppm, embodiment 4 -6 is 100ppm, calculated on the basis of the total mass of the raw materials) under the catalysis of hydrosilylation to prepare monohydroxypolysiloxane, and the product is filtered through activated carbon to remove the catalyst and a small amount of impurities. Under the protection of nitrogen and the reaction temperature of 50-80 ° C, the terminal alkenyl polysiloxane and the monohydroxy polysiloxane are subjected to a hydrosilylation reaction under the actio...

Embodiment 8

[0045] Example 8 Synthesis of silicon-containing polycaprolactone by initiator Ⅰ

[0046] Under the protection of nitrogen, add 1.0 mol of silicon-containing initiator I and 8.5 mol of caprolactone monomer into the reaction kettle, heat to 170°C for constant temperature dehydration for 2 hours, and add 10 ppm octanoic acid to the system, accounting for the total mass of silicon-containing initiator and caprolactone monomer For stannous catalyst, maintain the reaction temperature at 170°C for 3 hours under normal pressure, continue to react under vacuum until the hydroxyl value and acid value are qualified, cool down and pack. The hydroxyl value is 56.90 mgKOH / g, and the acid value is 0.50 mgKOH / g. The obtained polycaprolactone is designated as Product A.

Embodiment 9

[0047] Example 9 Synthesis of silicon-containing polycaprolactone by initiator II

[0048] Under the protection of nitrogen, add 1.0mol of silicon-containing initiator II and 13.0mol of caprolactone monomer into the reactor, heat to 180°C for constant temperature dehydration for 2 hours, and add 10ppm octanoic acid to the system, accounting for the total mass of silicon-containing initiator and caprolactone monomer For stannous catalyst, maintain the reaction temperature at 180°C for 2 hours under normal pressure, continue to react under vacuum until the hydroxyl value and acid value are qualified, cool down and pack. The hydroxyl value is 28.06 mgKOH / g, and the acid value is 0.30 mgKOH / g. The obtained polycaprolactone is designated as Product B.

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Abstract

The invention provides silicon-containing polyester polyol and a preparation method thereof. According to the silicon-containing polyester polyol, monohydroxy polysiloxane and alkenyl-terminated polysiloxane are subjected to an addition reaction to prepare a silicon-containing initiator; and then a ring-opening polymerization reaction is performed on the silicon-containing initiator and a lactonemonomer. The obtained polyester polyol has the advantages of good heat resistance, good flame retardancy and the like, and has good intersolubility with polyol and isocyanate.

Description

technical field [0001] The invention belongs to the field of polyester polyols, in particular to a silicon-containing polyester polyol and a preparation method thereof. Background technique [0002] Polyesters such as polycaprolactone have good flexibility, weather resistance, solvent resistance and chemical resistance, and their low molecular weight polymers are widely used in the fields of polyurethane coatings, adhesives, sealants and elastomers, and their high molecular weight polymers It can be used as a thermoplastic material in many fields of industry and life. However, this type of polyester has no significant advantages in terms of heat resistance, impact resistance and flame retardancy. [0003] Polyorganosiloxane can endow products with good product heat resistance, impact resistance, and has a certain flame retardant effect. Polyorganosiloxane usually has poor compatibility with polymer materials, and it is difficult to obtain a good modification effect. Paten...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/695C08G63/85C08G18/46C08G101/00
CPCC08G63/6952C08G63/85C08G18/4692C08G2101/00
Inventor 张存玉孙令民黄岐善
Owner WANHUA CHEM GRP CO LTD
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