Preparation method of polyether ester multi-block alternating copolymer

A technology of alternating copolymers and polyether esters, which is applied in the field of preparation of new high-performance polymers, can solve problems such as difficult to obtain polyether ester copolymers, reduce high-temperature polymerization time, and complex product structures, and achieve high polymer molecular weight, The effect of fast polymerization reaction rate and low reaction temperature

Inactive Publication Date: 2015-06-10
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And, the polyether ester copolymer that adopts this method to synthesize, the length of its polyester hard segment is difficult to control, is usually very short, and product structure is very complex, and reaction repeatability is bad, and homopolymer is mixed in reactant
In addition, due to the high t

Method used

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  • Preparation method of polyether ester multi-block alternating copolymer
  • Preparation method of polyether ester multi-block alternating copolymer
  • Preparation method of polyether ester multi-block alternating copolymer

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0029] See figure 1 As shown, a synthetic preparation method of a novel polyether ester multi-block alternating copolymer includes the following steps:

[0030] Step 1) Add the corresponding cyclic oligopolyester and polyether glycol into the reaction device, mechanically stir and evacuate;

[0031] Step 2) Heat to 120-180°C, add the catalyst after the reactants are evenly mixed, and vacuum;

[0032] Step 3) Raise the temperature to 220-280°C and continue the reaction to obtain the desired target product.

Example Embodiment

[0033] Example 1:

[0034] Under vacuum conditions, an alternating multi-block copolymer with a mass ratio of polyethylene adipate (PEA) and polytetrahydrofuran (PTMO) of 3:1 was prepared by a ring-opening-condensation polymerization method:

[0035] In a 50mL three-necked flask was added polyethylene adipate cyclic oligomers (COEAs, 15g) and polytetrahydrofuran (M n, PTMO =2900g / mol, 45g), place the device in a salt bath at 120°C, evacuate and mechanically stir. After stirring evenly, add 60μL (0.1wt%) tetrabutyl titanate catalyst, evacuate, the vacuum degree is 1×10 -3 MPa. Place the reaction device in a 220°C salt bath, start the reaction, and take samples every 30 minutes to obtain multi-block polymers with different block numbers (PEA-b-PTMO-b-PEA) n . The structural formula is as follows:

[0036]

[0037] See the proton nuclear magnetic resonance spectrum figure 2 , Proving that the target product has been successfully synthesized; in addition, the volume exclusion chromat...

Example Embodiment

[0038] Example 2:

[0039] Under vacuum conditions, an alternating multi-block copolymer with a mass ratio of polybutylene terephthalate (PBT) and polytetrahydrofuran of 3:1 was prepared by a ring-opening-condensation polymerization method:

[0040] Add polybutylene terephthalate cyclic oligomers (COBTs, 15g) and polytetrahydrofuran (M n, PTMO =2900g / mol, 45g), place the device in a salt bath at 180°C, evacuate and mechanically stir. After stirring evenly, add 60μL (0.1wt%) tetrabutyl titanate catalyst, evacuate, the vacuum degree is 1×10 -3 MPa. Place the reaction device in a salt bath at 240°C, start the reaction, and sample every 30 minutes to obtain multi-block polymers with different block numbers (PBT-b-PTMO-b-PBT) n . The structural formula is as follows:

[0041]

[0042] See the proton nuclear magnetic resonance spectrum Figure 4 , Proving that the target product has been successfully synthesized; in addition, the volume exclusion chromatogram is shown in Figure 5 , Als...

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Abstract

The invention discloses a preparation method of a polyether ester multi-block alternating copolymer. The preparation method comprises the following steps: 1) adding a cyclic oligoester and polyether glycol to a reaction device, stirring mechanically and vacuumizing; step 2) heating to the range of 120-180 DEG C, adding a catalyst after the reactants are mixed evenly, and vacuumizing; 3) increasing the temperature to the range of 220-280 DEG C for reacting, performing ring opening polymerization on the cyclic oligoester in the presence of the polyether glycol, thereby obtaining a polyether ester three-block copolymer, and then performing condensation polymerization on the three-block copolymer to obtain the polyether ester multi-block alternating copolymer. The polyether ester multi-block alternating copolymer identified in structure is obtained by performing ring-opening condensation polymerization on the cyclic oligoester monomers by use of the polyether glycol in vacuum; the preparation method has the advantages of simple reaction, few by-products and no aftertreatment; besides, the product can be directly used without being purified.

Description

technical field [0001] The invention belongs to the field of preparation of novel high-performance polymers, and relates to a preparation method for preparing polyether ester multi-block alternating copolymers through melt polymerization of polyether diol and cyclic oligoester. Background technique [0002] The synthesis methods of polyether ester copolymers mainly include the direct hydroxyl-terminated polyether esterification method, the acetoxy-terminated polyether method, and the transesterification method directly using polyester and polyether as raw materials. In industrial production, polyether ester elastomers are mainly prepared by esterification of hydroxyl-terminated polyether. That is to say, the diacid (or dimethyl ester) is mixed and melted with an excess of small molecule diol and hydroxyl-terminated polyether, and under the action of a catalyst, a transesterification reaction occurs at a lower temperature (below 200°C) to obtain a prepolymer, and then the rea...

Claims

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Application Information

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IPC IPC(8): C08G81/00C08G65/332
Inventor 屠迎锋黄卫春陈健英卢敏李志凯朱祥杨晓明
Owner SUZHOU UNIV
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