Novel aromatic high-fire-retardant polyester polyol as well as preparation method and application thereof

A technology of polyester polyol and aromatic dibasic acid, which is applied in the field of new aromatic high flame-retardant polyester polyol and its preparation, can solve the problem of inability to meet the requirements of high flame-retardant performance and physical and mechanical processing performance of building insulation materials. Reduction, migration of flame retardant performance and other problems, to achieve the effect of superior flame retardant performance, good activity and flame retardancy, high flame retardant performance

Inactive Publication Date: 2015-03-25
滕州市科米特新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The oxygen index of ordinary polyurethane rigid foam is generally 16% to 20%, and it can no longer meet the requirements of high flame retardancy for building insulation materials, so it is particularly important to improve the high flame retardancy of polyurethane foam
At present, the industrial production of rigid polyurethane foam mainly includes polyester type and polyether type, but in practical applications, the polyol raw material component of rigid polyurethane foam is mainly polyester polyol, and because of the aromatic ring structure, The synthesized polyurethane polyol foam is significantly better than polyether polyol in temperature resistance, thermal stability and flame retardancy, so the polyester polyol used in the field of building insulation and flame retardancy is mainly based on halogenated phthalic anhydride polyester polyol. Mainly, the organic flame retardant products are mainly additive type and reactive type. The additive type needs to add a large amount of flame retardants, which often greatly reduces the physical and mechanical processing properties of the material, and the longer the time, the flame retardant performance will occur. Migration, the flame retardant effect is greatly reduced, but there are safety hazards

Method used

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  • Novel aromatic high-fire-retardant polyester polyol as well as preparation method and application thereof
  • Novel aromatic high-fire-retardant polyester polyol as well as preparation method and application thereof

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Experimental program
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preparation example Construction

[0026] Preparation method of the present invention mainly comprises the following steps:

[0027] The first step: synthesis of hydroxyl-terminated polyester under the condition of excess alcohol. Add monomer raw materials, catalysts, antioxidants, etc. into the reactor, gradually raise the temperature to 220-240°C, and react for 8-10 hours. In the early stage of the reaction, it is carried out under normal pressure and under the protection of nitrogen. When it reaches the set acid value, hydroxyl value and viscosity range, under reduced pressure, 190-230 ° C, react for 1.5-2 hours, and the reaction can be carried out when the required index is reached. complete. ,

[0028] A novel highly flame-retardant aromatic polyester polyol of the present invention is obtained by esterification of naphthalene-containing aromatic dibasic acids, dibasic acids and small molecule alcohols or acids under the action of catalysts and antioxidants. The average functional group degree is 2, the...

Embodiment 1

[0041] The preparation of polyester polyol: take by weighing 2,6-naphthalene dicarboxylic acid, terephthalic acid, adipic acid, glycerol, diethylene glycol and catalyst tetraisopropyl titanate according to the proportioning ratio of embodiment 1 in the table , Antioxidants 1010 and 626 were added to the reaction kettle, and nitrogen was introduced for protection, then the temperature was raised, stirred, and gradually raised to 150°C, and after 2 hours of normal pressure reaction, the temperature was programmed to rise to 190°C, and water distillation began When it reaches 240°C, keep it warm for 5 hours. When the water output reaches 80% of the water output, stop feeding nitrogen, cool down to 180°C, start vacuuming in sections, and gradually increase the vacuum degree until the pressure reaches 0.01MPa. Heating while evacuating to raise the temperature to 230° C., and reacting under the above conditions for 1.5 to 2 hours. After testing, the acid value of the product was red...

Embodiment 2

[0044] Proportion of New Aromatic High Flame Retardant Polyester Polyol

[0045]

[0046] 2,6-NDA is 2,6-naphthalene dicarboxylic acid,

[0047] PTA is terephthalic acid,

[0048] AA is adipic acid,

[0049] Gly is glycerol,

[0050] DEG is diethylene glycol,

[0051] TTIP is tetraisopropyl titanate.

[0052] The new aromatic highly flame-retardant polyester polyol prepared in Embodiment 1 and Embodiment 2 of the present invention is compounded with the commonly used polyether polyol 4110 as the base polyol, and the polyether (white material) is configured and combined according to the formula in Table 1, and then mixed with Multi-subunit polyphenyl polyisocyanate PM-200 (black material) was mixed with high-speed stirring for foaming experiments; and the flame retardancy and mechanical properties of the prepared polyurethane rigid foam were tested; and the commonly used polyester polyol 4110 was used as a comparison.

[0053]

[0054] The results of comparative ...

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Abstract

The invention discloses a novel aromatic high-fire-retardant polyester polyol as well as a preparation method and an application thereof. The novel aromatic high-fire-retardant polyester polyol is applied to a fire-retardant polyurethane material, and is applied to the field of building heat preservation. The novel aromatic high fire-retardant polyester polyol is obtained by esterification reaction of naphthalene-based aromatic dibasic acid, binary acid and small molecular alcohol or acid under the action of a catalyst and an antioxidant; the mass ratio of naphthalene-based aromatic dibasic acid to binary acid to the small molecular alcohol or acid is (0.7-1.5) to (2.8-4.6) to (5.7-8.6); the average functional group degree is 2; the acid value is smaller than 1mgKOH / g; the average hydroxyl value is 400-660mgKOH / g; the average molecular weight is 170-300g / mol; and the viscosity is 2500-4500mPa.s. The polyester polyol disclosed by the invention has high flame retardant property and excellent mechanical property; the polyurethane foam prepared by the method has thermal stability, good activity and good fire-retardant property, and also has good physical properties such as compression strength, closed porosity, abrasive resistance, ageing resistance and heat resistance. The novel aromatic high-fire-retardant polyester polyol is simple in synthesis process, is good in compatibility with other polyesters and polyester polyol; and the rigid polyurethane foam prepared by the novel aromatic high fire-retardant polyester polyol has relatively good heat resistance and fire resistance, and is applied to the field of building heat preservation.

Description

technical field [0001] The present invention relates to a novel aromatic polyester polyol that can be used for flame-retardant polyurethane materials and its preparation method and use. Further, the present invention relates to a novel aromatic highly flame-retardant polyester polyol and its preparation method. And use it as a polyester polyol component in polyurethane foam, especially in rigid foam. Background technique [0002] Polyurethane is a rapidly developing multifunctional polymer synthetic material. Due to the variety of raw materials and the adjustable molecular structure, it can be made into foam plastics, elastomers, adhesives, coatings, etc., and has a wide range of uses. Similarly, by adjusting its raw materials and formulations, it is possible to design materials suitable for different properties and products for different purposes. Polyurethane rigid foam is a polymer composite material with excellent performance. It has good thermal insulation effect, elec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/668C08G18/48C08G18/42C08G101/00
Inventor 严来春孙志武钟东南王世昌陈志强
Owner 滕州市科米特新材料有限责任公司
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