A kind of biodegradable polyester and preparation method thereof

A biodegradable polyester and esterification technology, applied in the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of increasing production costs, complex catalyst preparation processes, and small molecule residues.

Active Publication Date: 2021-04-27
FUHAI (DONGYING) ADVANCED MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] To sum up, the method of reducing the acid value of PBAT products in the prior art is mainly to add expensive carboxyl-terminated scavengers and carbodiimide anti-hydrolysis agents, which not only increases the production cost, but also has the precipitation of small molecules, and the product application is affected. limit problem
In addition, by preparing a highly efficient hydrolysis-resistant catalyst to reduce the amount of the catalyst, this method has a complex catalyst preparation process, high cost, and the prepared catalyst components are complex, which easily leads to poor product quality stability
Most patents increase the degree of branching by adding multifunctional polycarboxylic acids, polyols or chain extenders, thereby improving the mechanical properties and melt strength of the product, but there are risks such as excessive crosslinking and small molecule residues in the use of multifunctional compounds

Method used

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  • A kind of biodegradable polyester and preparation method thereof
  • A kind of biodegradable polyester and preparation method thereof
  • A kind of biodegradable polyester and preparation method thereof

Examples

Experimental program
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preparation example Construction

[0057] The invention provides a kind of preparation method of biodegradable polyester, it comprises the steps:

[0058] First carry out esterification-precondensation, then carry out copolycondensation and final polycondensation.

[0059] Specifically, esterification-precondensation includes: using methanesulfonic acid as an esterification catalyst, catalyzing the esterification reaction of terephthalic acid (PTA) and 1,4-butanediol (BDO), removing methyl After sulfonic acid, add a titanium-based catalyst for pre-condensation to obtain oligoesterification (BHBT) of terephthalic acid and 1,4-butanediol;

[0060] Use methanesulfonic acid as the catalyst for esterification reaction to catalyze the esterification reaction of 1,6-adipic acid (AA) and 1,4-butanediol. After removing methanesulfonic acid, add titanium catalyst for precondensation , to obtain the oligoesterification of 1,6-adipic acid and 1,4-butanediol (BHBA);

[0061] Co-polycondensation includes: co-condensation o...

Embodiment 1

[0110] Table 1 The feed list of Example 1.

[0111]

[0112] The present embodiment provides a kind of preparation method of biodegradable polyester, comprises following steps carried out in sequence:

[0113] (1) Esterification-precondensation:

[0114] Weighed 1661.7g of terephthalic acid (wt%≥99.90%), 994.3g of 1,4-butanediol (wt%≥99.70%) and 67.1g of methanesulfonic acid (wt%≥99.00%) ) into 10L esterification kettle 1, turn on the heating, stir evenly, raise the temperature to 180°C, carry out the esterification and dehydration reaction, and react for 2 hours. , Reaction 0.5h, removal of methanesulfonic acid.

[0115] Then adjust the temperature, add 0.54g tetrabutyl titanate, the reaction temperature is 200°C, the reaction pressure is 100kPa, pre-condensation is carried out, the reaction is 0.6h, and the molecular weight is measured by sampling.

[0116] Weighed 1789.4g of 1,6-hexanedioic acid (wt%≥99.80%), 1213.0g of 1,4-butanediol (wt%≥99.70%) and 105g of methanes...

Embodiment 2

[0121] Table 2 Feeding table of Example 2.

[0122]

[0123] The present embodiment provides a kind of preparation method of biodegradable polyester, comprises following steps carried out in sequence:

[0124] (1) Esterification-precondensation:

[0125] Weighed 1661.7g of terephthalic acid (wt%≥99.90%), 994.3g of 1,4-butanediol (wt%≥99.70%) and 67.1g of methanesulfonic acid (wt%≥99.00%) ) into 10L esterification kettle 1, turn on the heating, stir evenly, raise the temperature to 180°C, carry out the esterification dehydration reaction, and react for 2 hours. When the water output of the reaction reaches the theoretical value of 360.0g, no more water will be distilled out, and the temperature is raised to 168°C , Reaction 0.5h, removal of methanesulfonic acid.

[0126] Then adjust the temperature, add 0.66g of tetrabutyl titanate, the reaction temperature is 200°C, the reaction pressure is 100kPa, carry out pre-precondensation, react for 0.5h, and sample for molecular we...

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Abstract

The invention discloses a biodegradable polyester and a preparation method thereof, and relates to the technical field of biodegradable materials. The present invention replaces easily hydrolyzed titanate with methanesulfonic acid as the catalyst in the esterification reaction stage that generates a large amount of water, and then adds the titanate catalyst in batches during the pre-condensation and co-polycondensation reactions that do not produce water, avoiding the need for catalyst Hydrolysis reduces the amount of catalyst used, thereby effectively inhibiting the thermal degradation reaction of PBAT, reducing the acid value of the product, and the acid value of the prepared PBAT is less than 15mol / t. The block copolymer with longer BHBT and BHBA segment structure can be obtained by precondensation after esterification, and then copolycondensation. The regularity of its molecular chain structure is compared with that of PBAT prepared by traditional random copolymerization method. Higher, the BHBT chain segment with longer hard segment structure in this molecular structure makes the mechanical properties of PBAT resin better.

Description

technical field [0001] The invention relates to the technical field of biodegradable materials, in particular to a biodegradable polyester and a preparation method thereof. Background technique [0002] With the increasing white pollution, biodegradable polyester has become one of the most effective solutions to the problem of plastic pollution. Biodegradable polyester can be degraded into environmentally harmless carbon dioxide and water under composting conditions or natural conditions. Among biodegradable polyesters, polybutylene terephthalate-co-polybutylene adipate (PBAT) is a combination of butylene adipate (PBA) and butylene terephthalate (PBT) copolymer, the structure of the copolymer has both rigid and flexible segments, not only has high ductility and elongation at break, but also has good heat resistance and impact resistance, and blown film Good, good biodegradability, is one of the current research hotspots. [0003] There are water-sensitive ester groups in t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/85C08G63/183C07C67/08C07C69/82C07C69/44B01J31/02
CPCB01J31/0225B01J2231/49C07C67/08C08G63/183C08G63/85C08G2230/00C07C69/82C07C69/44
Inventor 王敏岳林黄森彪廖广明
Owner FUHAI (DONGYING) ADVANCED MATERIAL TECH CO LTD
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