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Biomass base structure flame retardant polyol and preparation method and application thereof

A structural flame-retardant, biomass-based technology, applied in the field of biomass-based structural flame-retardant polyurethane foam and its preparation, can solve the problems of complex synthesis process, general flame-retardant performance of polyurethane, and poor binding performance of lignin components and polyurethane. Achieve high reactivity, less catalyst consumption, excellent heat resistance and mechanical properties

Active Publication Date: 2014-04-09
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are not many patents on biomass-based flame-retardant polyurethane foam plastics, especially structural flame-retardant polyurethane foam plastics. The main method is to prepare polyols from biomass, and then add flame retardants to the formula to prepare flame-retardant polyurethane foam plastics. CN1543478A Disclosed is a method for preparing polyurethane from lignin, which comprises polycondensing a polyol solution containing ligninsulfonic acid or a partially neutralized salt thereof in a dissolved state with polyisocyanate, since the lignin component cannot play a large role in polyurethane The role of molecular multi-functionality cross-linking core causes poor binding performance of lignin components and polyurethane, and the flame retardancy of the prepared polyurethane is general
CN102585143A discloses a kind of biomass-based flame-retardant polyurethane foam and its preparation method, including the preparation of flame-retardant polyurethane foam plastics by using lignin modification and other raw materials, and the synthesis process is relatively complicated

Method used

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  • Biomass base structure flame retardant polyol and preparation method and application thereof
  • Biomass base structure flame retardant polyol and preparation method and application thereof
  • Biomass base structure flame retardant polyol and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0018] Add 302g of cardanol and 162g of 37%wt formaldehyde solution into the reactor and mix evenly, raise the temperature to 70°C, add 210g of diethanolamine dropwise, and the dropping time is 1h. Pressure dehydration, when the moisture content is ≤1.5%wt, 66g of ethylene oxide and 87g of propylene oxide are circulated for alkoxylation reaction, the reaction temperature is controlled at 120-130°C, the pressure is controlled at 0.3-0.5MPa, and the ring is completed After oxidizing, react at constant temperature and pressure for 60 minutes. At 120°C / 10mmHg, decompress and evacuate for 30 minutes to obtain a structural flame-retardant polyol with a hydroxyl value of 386mg / g KOH and a viscosity of 2100mPa·s at 25°C. Then obtain the combination polyol according to the preparation formula of rigid polyurethane foam in Table 1, stir evenly, then mix with isocyanate and stir at high speed for 20-30s at a speed of 3000-3500r / min, pour into a mold, and mature for 48h.

Embodiment 2

[0020] Add 302g of cardanol, 60g of paraformaldehyde, and 30g of melamine into the reactor and mix evenly, raise the temperature to 70°C, add 210g of diethanolamine dropwise, and the dropwise addition time is 1h. Dehydration under reduced pressure. When the moisture content is ≤1.5%wt, 80g of ethylene oxide and 97g of propylene oxide are circulated for alkoxylation reaction. The reaction temperature is controlled at 120-130°C and the pressure is controlled at 0.3-0.5MPa. After epoxidation, react at constant temperature and pressure for 60 minutes, and at 120°C / 10mmHg, decompress and evacuate for 30 minutes to obtain a structural flame-retardant polyol. Its hydroxyl value is 406mg / g KOH, and its viscosity at 25°C is 5100mPa·s. Then obtain the combination polyol according to the preparation formula of rigid polyurethane foam in Table 1, stir evenly, then mix with isocyanate and stir at high speed for 20-30s at a speed of 3000-3500r / min, pour into a mold, and mature for 48h.

Embodiment 3

[0022]Add 302g of cardanol, 243g of 37%wt formaldehyde solution, and 60g of melamine into the reactor and mix evenly, raise the temperature to 80°C, add 315g of diethanolamine dropwise, and the dropping time is 2h. ℃, dehydration under reduced pressure, when the moisture content is ≤1.5%wt, 134g ethylene oxide and 163g propylene oxide are circulated for alkoxylation reaction, the reaction temperature is controlled at 120-130℃, and the pressure is controlled at 0.3-0.5MPa, After passing the epoxide, react at constant temperature and pressure for 60 minutes, and at 120°C / 10mmHg, depressurize and evacuate for 30 minutes to obtain a structural flame-retardant polyol. Its hydroxyl value is 460mg / g KOH, and its viscosity at 25°C is 8500mPa·s. Then obtain combined polyol according to the preparation formula of rigid polyurethane foam in Table 1, stir evenly, then mix with isocyanate and stir at high speed for 20-30s at a speed of 3000-3500r / min, pour into a mold, and age for 48h.

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Abstract

The invention discloses biomass base structure flame retardant polyol and a preparation method and an application thereof. An intermediate is obtained by utilizing the Mannich reaction of biomass anacardol, diethanolamine, melamine or urea, and formaldehyde, and the biomass base structure flame retardant polyol can be prepared through further alkoxylation with epoxy ethane and epoxy propane, with a hydroxyl value of 200-500mg / gKOH, moisture being less than or equal to 1.0%, and viscosity of 2000-10000mPa.s (25 DEG C), and the biomass base structure flame retardant polyol is applied in polyurethane foam as a polyol component. According to the biomass base structure flame retardant polyol as well as the preparation method and the application, an intermediate process does not need separation, the cost is low, the process is easy, and the prepared polyurethane foam is good in flame retardance, has the advantages that a product does not drip liquid, the shape is kept, the smoke density is low and the like, and can be used in construction, heat preservation and some special fields.

Description

technical field [0001] The invention relates to a flame-retardant polyurethane foam with a biomass-based structure and a preparation method thereof, mainly relates to the preparation of a flame-retardant polyol with a biomass-based structure and its application in polyurethane foam as a polyol component, and is especially suitable for the preparation of a ring Preparation of flame retardant polyurethane spray insulation material with pentane foaming system. Background technique [0002] Polyurethane is a kind of high polymer containing carbamate group (-NHCOO-) in its molecular chain. With the different raw materials, additives and process conditions during synthesis, products with different properties can be synthesized, such as foam plastics, rubber, coatings, adhesives, elastic fibers, etc. Polyurethane foam is currently the best thermal insulation material in the world. Because developed countries such as Europe and the United States attach great importance to building ...

Claims

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Application Information

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IPC IPC(8): C08G65/28C08G18/50C08J9/14C08G101/00
Inventor 张猛周永红张立强
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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