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Preparation method of secondary hydroxyl-terminated allyl polyether polyol

A technology of sealing allyl polyether and secondary hydroxyl group, which is applied in the field of polyether synthesis, can solve the problems such as the preparation technology of allyl polyether that is not mentioned, and achieve the effects of excellent mechanical properties, high molecular weight and narrow distribution.

Active Publication Date: 2017-05-31
SHANDONG INOV NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Patent CN102634035A reports a kind of silicone polyether polyol and its preparation method, and the method for preparing polyurethane elastomer, and this patent mentions the use of The allyl polyether polyol with the structure is used to prepare silicone polyether polyol, the preparation method is novel, and the product is used in the preparation of polyurethane elastomers, but it does not mention the specific preparation technology of allyl polyether

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  • Preparation method of secondary hydroxyl-terminated allyl polyether polyol
  • Preparation method of secondary hydroxyl-terminated allyl polyether polyol

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Embodiment 1

[0026] The preparation method of the allyl polyether polyol of described secondary hydroxyl termination, concrete steps are as follows:

[0027] (1) Add 116kg of allyl alcohol and 1.6kg of KOH to the autoclave, replace nitrogen to test the oxygen content of 50ppm, stir and heat up to 80°C, start to add 1890kg of ethylene oxide dropwise, and gradually heat up to 110°C for continuous Reaction, after the addition of ethylene oxide, fill nitrogen to 0.15MPa, aging reaction for 0.5h; cool down to 80°C, add 40kg of pure water, 3.2kg of phosphoric acid, stir for 0.5h, then add adsorbent 2kg of magnesium silicate and 1 kg of aluminum silicate, stirred for 0.5 h; vacuum dehydrated for 8 h, tested for a moisture content of 0.030%, circulated and filtered to a clear liquid, and the initiator polyether 1 was obtained.

[0028] (2) Add 1000kg starter polyether 1 and 0.2kg solid powder bimetallic catalyst (DMC) into the autoclave, evacuate to -0.095MPa, vacuumize and dehydrate while heating...

Embodiment 2

[0030] The preparation method of the allyl polyether polyol of described secondary hydroxyl termination, concrete steps are as follows:

[0031] (1) Add 116kg of allyl alcohol and 2.1kg of NaOH into the autoclave, nitrogen replacement to test the oxygen content of 60ppm, stir and heat up to 75°C, start to add 1290kg of ethylene oxide dropwise, and gradually heat up to 112°C for continuous Reaction, after the addition of ethylene oxide, fill nitrogen to 0.15MPa, aging reaction for 1h; cool down to 85°C, add 42kg of pure water, 4.4kg of phosphoric acid, stir for 1h, then add adsorbent 2.1kg of magnesium silicate and 1. 12 kg of aluminum silicate, stirred for 0.5 h; vacuum dehydrated for 6 h, tested for a moisture content of 0.032%, circulated and filtered to a clear and transparent liquid, and the initiator polyether 2 was obtained.

[0032] (2) Add 700kg of initiator polyether 2 and 0.18kg of solid powdery bimetallic catalyst (DMC) into the autoclave, vacuumize to -0.095MPa, va...

Embodiment 3

[0034] (1) Add 232kg of allyl alcohol and 7kg of KOH into the autoclave, nitrogen replacement to test the oxygen content of 40ppm, stir and heat up to 70°C, start to continuously add 1770kg of ethylene oxide dropwise, and gradually heat up to 112°C for continuous reaction , after the addition of ethylene oxide, fill nitrogen to 0.15MPa, aging reaction for 1h; cool down to 85°C, add 80kg of pure water, 14.68kg of phosphoric acid, stir for 1h, then add adsorbents 4kg of magnesium silicate and 2kg of silicon Aluminate, stirred for 0.5h; vacuum dehydrated for 6h, tested for moisture content of 0.031%, circulated and filtered to a clear and transparent liquid, and the initiator polyether 3 was obtained.

[0035] (2) Add 1000kg of initiator polyether 3 and 0.30kg of emulsion bimetallic catalyst (DMC) into the autoclave, vacuumize to -0.095MPa, and dehydrate while heating up. When the temperature rises to 115°C , add 100kg of propylene oxide to induce the reaction, after the inductio...

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Abstract

The invention relates to a preparation method of secondary hydroxyl-terminated allyl polyether polyol, belonging to the technical field of polyether synthesis. The method comprises the following steps: (1) in the front phase, preparing coarse allyl polyether having the molecular weight of 300-1000 via ring opening polymerization of ethylene oxide by using allyl alcohol as an initiator under the action of an alkali metal catalyst, then neutralizing, adsorbing, drying and filtering to obtain fine allyl polyether; and (2) in the rear phase, preparing allyl polyether polyol having the molecular weight of 1000-10000 via ring opening polymerization of propylene epoxide by using the fine allyl polyether as an initiator under the action of a bimetallic catalyst. The polyoxyethylene chain segment and the polypropylene oxide chain segment in the polyether molecular structure are skillfully copolymerized via the two-phase synthetic process in combination with the synthetic process of a polyether, so that the prepared polyether polyol has the characteristics of high molecular weight, narrow distribution and regular structure, the synthesis efficiency is high, and the C=C bond is kept good.

Description

technical field [0001] The invention relates to a preparation method of secondary hydroxyl-terminated allyl polyether polyol, which belongs to the technical field of polyether synthesis. Background technique [0002] Allyl polyether polyol is one of the main raw materials for synthesizing silicone oil. Its synthesis is generally obtained by using allyl alcohol as the initiator, and ring-opening polymerization of ethylene oxide and propylene oxide under the action of an alkali metal catalyst. Due to the presence of terminal active hydroxyl groups, allyl polyether polyols are not resistant to acid, alkali and high temperature. When reacting with hydrogen-containing polymethylsiloxane, one terminal hydroxyl group of allyl polyether is easy to condense with silicon-oxygen bonds, resulting in side reactions. , during the application process as a polyurethane foam stabilizer, the hydroxyl group can participate in the polyurethane synthesis reaction. Therefore, allyl polyether poly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/26C08G65/30
CPCC08G65/2609C08G65/2645C08G65/2648C08G65/30
Inventor 孙兆任杨凯周玉波李剑锋张士虎王玉
Owner SHANDONG INOV NEW MATERIALS CO LTD
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