Aromatic-aliphatic copolyester and synthetic method thereof

A technology of aliphatic copolyester and synthesis method, which is applied in the direction of adhesives, etc., can solve the problems of slow polymerization reaction speed, long reaction cycle, and many side reactions, and achieve less by-product generation, short polymerization reaction time, good heat The effect of stability

Inactive Publication Date: 2012-07-11
SHANGHAI LIGHT IND RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chinese patents CN1807485, CN1796433, and CN1796434 have invented a method for the synthesis of aromatic-aliphatic copolyesters by ordinary titanium, tin, and germanium catalysts, which have the disadvantages of slow polymerization reaction speed, many side reactions, toxicity, and yellowish color of the product. A new non-toxic or low-toxic rare earth catalyst, which can significantly increase the reaction speed of DMT, aliphatic dibasic acid and aliphatic dibasic alcohol, inhibit side reactions, improve product color, and increase molecular weight
[0006] The following problems exist in the preparation of aromatic-aliphatic copolyesters by DMT transesterification process: first, the amount and price of DMT raw materials are high, and the cost of copolyester raw materials is high; second, the product of transesterification reaction is methanol, and the by-products have recovery problems; Third, the DMT transesterification reaction and the aliphatic dibasic acid esterification reaction are carried out simultaneously, and the feeding needs to be carried out step by step, such as single-pot operation, the reaction cycle is long, and the heat source consumption is high.
However, due to the toxicity of antimony catalysts, the application of the PBTA copolyester obtained by this preparation method in some fields is limited.

Method used

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  • Aromatic-aliphatic copolyester and synthetic method thereof
  • Aromatic-aliphatic copolyester and synthetic method thereof

Examples

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preparation example Construction

[0014] In a preferred embodiment, the synthetic method of the present invention comprises the following specific reaction steps:

[0015] 1) Esterification reaction. Will C 6 -C 10 Aromatic dicarboxylic acid, C 4 -C 12 Aliphatic dicarboxylic acids and C 2 -C 6 The aliphatic dihydric alcohol and the catalyst are added directly or made into a slurry into the reaction kettle, and the esterification reaction is carried out at a temperature of 140-240°C under normal pressure stirring, and the retort temperature is kept at 100±5°C. The progress of the esterification reaction is based on the water output. When the total water output reaches more than 98% of the theoretical water output, the esterification reaction is considered to be over.

[0016] C 6 -C 10 Aromatic dicarboxylic acids and C 4 -C 12 The molar ratio of the aliphatic dicarboxylic acid is 95:5-5:95, preferably 85:15-15:85, more preferably 70:30-30:70.

[0017] C 6 -C 10 Aromatic dicarboxylic acids and C 4 ...

Embodiment 1

[0052] Add 2565 grams of 1,4-butanediol (28.5 mol) and 18.4 grams of 1,2,3 glycerol (0.2 mol) into a 10L stainless steel reactor with a thermometer, mechanical stirrer, fractionating column and condenser , heating up, and then continue to add 1577 g of PTA (9.5 mol), 1919 g of 1,8-sebacic acid (9.5 mol) and 3 g of tetraethyl titanate under stirring. Heating to raise the temperature, when the temperature in the kettle reaches 160°C, the distillation temperature rises to 98-100°C, water begins to flow out, and the temperature continues to rise but the temperature does not exceed 230°C. When the water output reaches 99% of the theoretical amount, the esterification reaction ends. The entire esterification reaction took 4 hours. Add 2 grams of tetraethyl titanate and 3 grams of triphenyl phosphate into the reaction kettle, continue to heat up to 230-270 ° C, and perform a pre-condensation reaction for 1 hour to remove excess 1,4-butanediol. When the amount of 1,4-butanediol relea...

Embodiment 2-8

[0054] The above seven embodiments are carried out according to the steps and methods of Example 1, except that the raw materials and consumption are as shown in Table 1 below, and the analysis results of the products obtained are also listed in Table 1.

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Abstract

The invention provides a new aromatic-aliphatic copolyester and a synthetic method thereof. The synthetic method comprises the following steps of: performing esterification and condensation polymerization reaction on C6-C10 aromatic dicarboxylic acids, C4-C12 aliphatic dicarboxylic acids and C2-C6 aliphatic diols in the presence of a catalyst, and adding 0.01 to 2 weight percent of polyol containing three or more hydroxyls, polybasic acid containing three or more carboxyls, compound containing two or more carboxyls and more than one hydroxyl or compound containing two or more hydroxyls and more than one carboxyl based on the total weight of the aromatic-aliphatic copolyester. By the method, the polymerization reaction time is short, a few byproducts are generated, and the product is white, has good thermal stability and is particularly suitable to be used as hot melt adhesive.

Description

technical field [0001] The present invention relates to an aromatic-aliphatic copolyester and a synthesis method thereof, more particularly to a synthesis method for preparing an aromatic-aliphatic copolyester by direct esterification and the prepared aromatic-aliphatic copolyester polyester. Background technique [0002] Aromatic-aliphatic copolyester mainly refers to the copolyester of aromatic polyester and aliphatic polyester, which is a kind of copolyester with excellent comprehensive performance, which can be used in plastics, hot melt adhesives, biodegradable materials and other fields . [0003] At present, the traditional preparation process of aromatic-aliphatic copolyester is made of dimethyl terephthalate (DMT), long carbon chain aliphatic dibasic acid and long carbon chain dibasic alcohol after transesterification and esterification , and then reduced compression polymerization to obtain. For example, in its publications US5817721, US6114042, US6046248, and U...

Claims

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Application Information

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IPC IPC(8): C08G63/20C08G63/60C08G63/78C09J167/02
Inventor 祝爱兰李人未何文祥
Owner SHANGHAI LIGHT IND RES INST
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