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Bio-based degradable multi-block copolyester elastomer and preparation method thereof

A technology of copolyester elastomer and multi-block copolymer, which is applied in the field of bio-based degradable multi-block copolyester elastomer and its preparation, can solve the problem of affecting strength and recovery rate, non-biodegradable, bio-based carbon Low content and other problems, to achieve the effect of adjustable performance, adjustable strength and elongation, and light color of the product

Pending Publication Date: 2022-07-15
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The current research on polyester elastomers mainly has these problems: 1) The bio-based carbon content is low, and the raw materials are strongly dependent on fossil energy; 2) The molecular weight of thermoplastic polyester elastomers containing dimer acid decreases significantly with the increase of dimer acid. Affect the final strength and recovery rate; 3) non-biodegradable

Method used

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  • Bio-based degradable multi-block copolyester elastomer and preparation method thereof
  • Bio-based degradable multi-block copolyester elastomer and preparation method thereof
  • Bio-based degradable multi-block copolyester elastomer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of bio-based degradable multi-block copolyester elastomers based on dimethyl 2,5-furandicarboxylate and dimethyl dimer acid:

[0029] Using 98% concentrated sulfuric acid as a catalyst, high-purity dimer acid (dimer content>98%) and methanol are refluxed for 2 hours under the condition that the molar ratio is 1:8 to obtain dimethyl dimer acid.

[0030] Add 0.23mol (42.32g) dimethyl 2,5-furandicarboxylate, 0.59mol (53.10g) ethylene glycol, 0.067mol (39.40g) of dimethyl dimer acid and 0.08g of tetraisopropyl titanate were reacted under nitrogen atmosphere at 160°C for 2 hours, 170°C for 2 hours, and 180°C for 2 hours to obtain a transesterification product.

[0031] Cool down to 140-150°C, continue to add 0.29mol (53.36g) dimethyl 2,5-furandicarboxylate, heat up to 160°C, and react to 200°C at a heating rate of 10°C / h under nitrogen atmosphere to obtain oligomerization thing.

[0032] Add 0.08g of zinc acetate, stir and gradually heat up to 200°C, pump the s...

Embodiment 2

[0035] Bio-based degradable multi-block copolyester elastomers based on dimethyl 2,5-furandicarboxylate and dimethyl dimer:

[0036] Using concentrated sulfuric acid as a catalyst, high-purity dimer acid (dimer content > 98%) and methanol are refluxed for 2 hours under the condition that the molar ratio is 1:8 to obtain dimethyl dimer acid.

[0037] 0.22mol (40.48g) dimethyl 2,5-furandicarboxylate, 0.68mol (42.16g) 1,4- Butanediol, 0.09mol (52.92g) dimethyl ester dimer, 0.12g tetrabutyl titanate, react under nitrogen atmosphere at 160 ℃ for 2 hours, 170 ℃ for 2 hours, 180 ℃ for 2 hours to obtain transesterification product.

[0038] Cool to 140-150°C, continue to add 0.25mol (46.00) dimethyl 2,5-furandicarboxylate, heat up to 160°C, and react to 200°C at a heating rate of 10°C / h under nitrogen atmosphere to obtain oligomers .

[0039] Add 0.06 g of germanium oxide, stir and gradually heat up to 200 ° C, pump the system pressure to 40 ± 5 Pa within 30 minutes, then increase ...

Embodiment 3

[0042] Bio-based degradable multi-block copolyester elastomers based on dimethyl 2,5-furandicarboxylate and dimethyl dimer:

[0043] Using concentrated sulfuric acid as a catalyst, high-purity dimer acid (dimer content > 98%) and methanol are refluxed for 2 hours under the condition that the molar ratio is 1:8 to obtain dimethyl dimer acid.

[0044] 0.33mol (60.72g) dimethyl 2,5-furandicarboxylate, 0.44mol (63.36g) 1,4- Cyclohexanedimethanol, 0.035mol (20.58g) dimethyl ester dimer, 0.10g lanthanum acetylacetonate, react under nitrogen atmosphere at 160°C for 2 hours, 170°C for 2 hours, and 180°C for 2 hours to obtain transesterification products .

[0045] Cool down to 140-150°C, continue to add 0.29mol (53.36g) dimethyl 2,5-furandicarboxylate, heat up to 160°C, and react to 200°C at a heating rate of 10°C / h under nitrogen atmosphere to obtain oligomerization thing.

[0046] Add 0.1g of antimony trioxide, stir and gradually heat up to 200°C, pump the system pressure to 40±5...

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Abstract

The invention relates to a bio-based degradable multi-block copolyester elastomer and a preparation method thereof, in the presence of a catalyst A, 2, 5-dimethyl furandicarboxylate, dimer acid dimethyl ester and small molecule diol are mixed, stirred and heated for transesterification to obtain furandicarboxylate dihydroxyalkyl ester and dimer acid dihydroxyalkyl ester; carrying out second-step ester exchange reaction on the mixture of furandicarboxylic acid dihydroxyalkyl ester and dimer acid dihydroxyalkyl ester and 2, 5-furandicarboxylic acid dimethyl ester, so as to obtain a low-molecular-weight polyester prepolymer; and carrying out polycondensation on the obtained low-molecular-weight polyester prepolymer under the action of a catalyst B. The preparation method disclosed by the invention has the advantages of low energy consumption, few side reactions, light product color, adjustable performance and the like, and is beneficial to industrial application.

Description

technical field [0001] The invention belongs to the technical field of thermoplastic polyester elastomers, in particular to a bio-based degradable multi-block copolyester elastomer based on dimethyl 2,5-furandicarboxylate and dimethyl dimer acid and a preparation method thereof . Background technique [0002] Due to the unique high elasticity of rubber materials, it has been widely used in industrial production, national defense, daily life, etc., and is considered to be an important strategic resource. However, the main raw materials of synthetic rubber, styrene, isoprene, butadiene, etc., all come from non-renewable petrochemical resources. As a large consumer of petrochemical resources, the rubber industry produces a large amount of waste water and waste gas. To solve this outstanding problem, an effective method is to prepare novel bio-based elastomer materials with engineering application potential based on bio-based chemicals. [0003] Furandicarboxylic acid polyest...

Claims

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Application Information

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IPC IPC(8): C08G63/52C08G63/83C08G63/86
CPCC08G63/52C08G63/83C08G63/863C08G63/866
Inventor 汪宏生王春鹏
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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