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Lignin-based polyol, modified lignin-based polyurethane material, modified lignin-based polyurethane film, preparation method and application

A polyurethane material and polyurethane film technology, applied in polyurea/polyurethane coatings, polyurea/polyurethane adhesives, anti-corrosion coatings, etc., can solve problems such as poor mechanical properties and thermal stability, and achieve improved heat resistance and light resistance Aging properties, good mechanical properties, effects of improving mechanical properties and heat resistance

Active Publication Date: 2020-05-22
SOUTH CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the lignin-based polyurethane produced by substituting chemical polyols with lignin still has problems to be overcome, such as the technical defects of poor mechanical properties and thermal stability of lignin-based polyurethane

Method used

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  • Lignin-based polyol, modified lignin-based polyurethane material, modified lignin-based polyurethane film, preparation method and application
  • Lignin-based polyol, modified lignin-based polyurethane material, modified lignin-based polyurethane film, preparation method and application
  • Lignin-based polyol, modified lignin-based polyurethane material, modified lignin-based polyurethane film, preparation method and application

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preparation example Construction

[0035] The invention provides a kind of preparation method of lignin-based polyol, comprising the following steps:

[0036] Mix lignin, sodium hydroxide solution, ethanol and allyl compound for allylation reaction to obtain allylated modified lignin;

[0037] The allylated modified lignin, the organic solvent and the mercapto compound are mixed, and the mercapto-ene click reaction is carried out to obtain the lignin-based polyol.

[0038] The invention mixes lignin, sodium hydroxide solution, ethanol and allyl compound to carry out allylation reaction to obtain allylated modified lignin.

[0039] In the present invention, unless otherwise specified, the raw materials used are conventional commercially available products in this field.

[0040] In the present invention, the lignin preferably includes one or more of enzymatic lignin, alkali lignin and organic solvent lignin. In the present invention, the mass concentration of the sodium hydroxide solution is preferably 1-5%, m...

Embodiment 1

[0083] Weigh 10g of enzymatic lignin dissolved in NaOH solution and ethanol (the volume ratio of NaOH solution to ethanol is 1:1), add 7g of bromopropene, and carry out allylation reaction at 55°C for 24 hours Finally, the allylation reaction product was obtained. After the allylation reaction product was cooled to room temperature, an equal mass of ice-water mixture was added, and the pH value was adjusted to 2-3 with 1mol / L HCl, and the supernatant was filtered off overnight. liquid, put the solid filter residue in a vacuum oven, and after overnight at 50°C, crush it to obtain allylated modified lignin.

[0084] Weigh 10g of allylated modified lignin and dissolve it in THF, add 10g of mercaptoethanol, and carry out the mercapto-ene click reaction at 65°C. After 24 hours of reaction, the mercapto-ene click reaction product is obtained. The reaction product was cooled to room temperature, and an equal mass of deionized water was added, the product was precipitated and suction ...

Embodiment 2

[0095] The lignin-based polyol was prepared according to the method of Example 1.

[0096] Mix the modified lignin and HDI according to the ratio of isocyanate to 1.5, and dissolve it in absolute dry DMAC, put the reaction solution in a shaker at 250r / min and react for 30min to obtain a modified lignin-based polyurethane material, pour it into a glass sheet On the surface, the wet film thickness is 0.4mm, pre-cured at 60°C for 2 hours, the heating rate to 60°C is 0.5°C / min, and then heated to 120°C and cured for 2 hours, and the heating rate to 120°C is 0.5°C / min to obtain the modified lignin-based polyurethane film LPU-2 with a film thickness of 0.1 mm, which can be used to prepare sealing materials.

[0097] The performance of the modified lignin-based polyurethane film LPU-2 in Example 2 is tested, and the test results can be found in Figure 6-9 , Figure 11 And Table 2-3.

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Abstract

The invention provides lignin-based polyol, a modified lignin-based polyurethane material, a modified lignin-based polyurethane film, a preparation method and application, and belongs to the technicalfield of polyurethane industry. The preparation method provided by the invention comprises the following steps: mixing lignin, a sodium hydroxide solution, ethanol and an allyl compound, and carryingout an allylation reaction to obtain allylation modified lignin; and mixing the allylation modified lignin, an organic solvent and a sulfhydryl compound, and carrying out a sulfhydryl-alkene click reaction to obtain the lignin-based polyol. The lignin-based polyol prepared by the invention is used for preparing the modified lignin-based polyurethane material, and the prepared modified lignin-based polyurethane material has good mechanical properties, heat resistance and light aging resistance.

Description

technical field [0001] The invention belongs to the technical field of polyurethane industry, and specifically relates to lignin-based polyols, modified lignin-based polyurethane materials, modified lignin-based polyurethane films, preparation methods and applications. Background technique [0002] Polyurethane material has many advantages, such as low density, low thermal conductivity, moisture permeability, high strength-to-weight ratio, high dimensional stability, etc. Therefore, it can be prepared into products with different properties to suit various purposes, and is widely used in thermal insulation, construction , transportation, decoration and other fields, and are made into various products such as building materials, leather clothing, and wear-resistant soles. With a growing global market, polyurethane materials have rapidly developed into one of the most diverse and versatile polymer materials. At present, the raw materials for the production of polyester and po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00C08G18/64C08J5/18C08L75/04C09D175/04C09D5/08C09J175/04
CPCC08G18/6492C08H6/00C08J5/18C08J2375/04C09D5/08C09D175/04C09J175/04
Inventor 郭垂根刘涛曹一丁王清文李丽萍刘珍珍欧荣贤孙理超
Owner SOUTH CHINA AGRI UNIV
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