Preparation method and applications of reaction type Mannich polyether polyol with permanent flame retardant effect

A Mannich polyether and reactive technology, which is applied in the field of preparation of reactive Mannich polyether polyols, can solve problems such as difficulty in use, high brittleness, powder drop, etc., and achieve the effect of broad application prospects

Inactive Publication Date: 2014-01-29
JIANGSU YOKE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Phenolic foam board is a material with excellent fire resistance and good thermal insulation performance; but it is brittle and difficult to use, and it is easy to break, fall off, and powder during construction

Method used

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  • Preparation method and applications of reaction type Mannich polyether polyol with permanent flame retardant effect

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. Add 105g of diethanolamine and 30g of paraformaldehyde into a three-necked flask equipped with a mechanical stirrer, a thermometer and a condenser, raise the temperature to 70°C and keep it warm for 3 hours; then collect the fractions at 125-130°C / 8000Pa by vacuum distillation The product 3-hydroxyethyl-1,3-oxazolidine.

[0034] 2. Add 47g of phenol into a three-necked flask with mechanical stirring, thermometer and condenser and heat it to 70°C, stir and add 117g of 3-hydroxyethyl-1,3-oxazolidine dropwise, and keep warm for 5h after the dropwise addition. The intermediate Mannich base is obtained.

[0035] 3. Take 164g of the intermediate Mannich base and add it to the autoclave, add 3.3g of KOH, raise the temperature to 80°C and depressurize for 1h, replace the nitrogen for 3 times and then depressurize to -0.1MPa; feed ethylene oxide and raise the temperature React at 110°C, keep the reaction pressure at 0.4MPa, until the amount of ethylene oxide added reaches 8...

Embodiment 2

[0037] 1. Add 105g of diethanolamine and 83g of formaldehyde aqueous solution (37%) into a three-necked flask equipped with mechanical stirring, a thermometer and a condenser, raise the temperature to 80°C and keep it warm for 2h; then collect under reduced pressure distillation at 125-130°C / 8000Pa The fractions gave the product 3-hydroxyethyl-1,3-oxazolidine.

[0038] 2. Add 55g of hydroquinone to a three-necked flask equipped with a mechanical stirrer, a thermometer and a condenser and heat it to 90°C, stir and add 117g of 3-hydroxyethyl-1,3-oxazolidine dropwise, and the dropwise addition ends Incubate for 2h to obtain the intermediate Mannich base.

[0039] 3. Take 172g of the intermediate Mannich base and add it to the autoclave, add 1.3g of DMC catalyst, raise the temperature to 90°C and depressurize for 1h, replace the nitrogen for 3 times and then depressurize to -0.1MPa; feed propylene oxide and raise the temperature React at 120°C, keep the reaction pressure at 1MPa...

Embodiment 3

[0041] 1. Add 105g of diethanolamine and 30g of paraformaldehyde into a three-necked flask equipped with a mechanical stirrer, a thermometer and a condenser, raise the temperature to 60°C and keep it warm for 4 hours; then collect the fractions at 125-130°C / 8000Pa by vacuum distillation to obtain The product 3-hydroxyethyl-1,3-oxazolidine.

[0042] 2. Add 42g of melamine and 42g of deionized water into a three-necked flask equipped with mechanical stirring, a thermometer and a condenser, stir and heat to 60°C, add 117g of 3-hydroxyethyl-1,3-oxazolidine dropwise, drop After the addition, the temperature was kept for 7 hours, and the intermediate Mannich base was obtained after removing water under reduced pressure.

[0043] 3. Take 159g of the intermediate Mannich base and add it to the reactor, add 0.16g of Et2O·BF3 catalyst, 153g of epichlorohydrin (the molar ratio of the epoxy compound to the intermediate Mannich base is 3.3:1), and then Raise the temperature to 80°C and r...

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Abstract

The invention provides a preparation method of reaction type Mannich polyether polyol with permanent flame retardant effect. The preparation method of reaction type Mannich polyether polyol with permanent flame retardant effect comprises the following steps: reacting paraformaldehyde or formaldehyde solution with diethanol amine to obtain 3-ethoxyl-1,3-oxazolidine reaction liquid, and then carrying out reduced pressure distillation to obtain the product 3-ethoxyl-1,3-oxazolidine; reacting aromatic phenol compounds or / and melamine compounds with 3-ethoxyl-1,3-oxazolidine to obtain Mannich base as intermediate; and carrying out polymerization reaction between the intermediate Mannich base and epoxy compound to obtain crude product of reaction type Mannich polyether polyol with permanent flame retardant effect, then carrying out reduced pressure distillation to remove impurities with low boiling points, and thus obtaining finished product. The reaction type Mannich polyether polyol simultaneously has the high stability and thermal stability of rigid polyurethane foam and the flame resistance of phenolic foam, is applied to foaming rigid polyurethane foam, and has wide application prospect.

Description

technical field [0001] The invention relates to a preparation method and application of a reactive Mannich polyether polyol with permanent flame-retardant effect. technical background [0002] Polyurethane rigid foam processed from rigid polyether polyol and isocyanate has many advantages such as low thermal conductivity and good thermal insulation performance; strong foam stability, strong combination with other materials, not easy to fall off; easy processing and wide application. However, rigid polyurethane foam is extremely flammable, and toxic and harmful gases and smoke will be produced during the combustion process, which is harmful to the human body and the environment; as people become more and more aware of fire hazards, the requirements for flame retardancy of materials are also increasing. higher. Phenolic foam board is a material with excellent fire resistance and good thermal insulation performance; however, it is brittle and difficult to use, and it is easy t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C08G65/26C08G18/48C08G18/50C08G101/00
Inventor 沈琦褚昭宁曹恒邢秀涛陈俊
Owner JIANGSU YOKE TECH
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