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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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  • 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 temperature instability of polyether, cyclization and degradation will occur quickly under acidic catalysts, so neutral or basic catalysts must be used, and the high temperature polymerization time must be reduced, so it is difficult to obtain high molecular weight polyether ester copolymerization thing

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

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preparation example Construction

[0029] see figure 1 Shown, the synthetic preparation method of a kind of novel polyether ester multi-block alternating copolymer comprises the following steps:

[0030] Step 1) Adding the corresponding cyclic oligoester and polyether diol in the reaction device, mechanically stirring, and vacuumizing;

[0031] Step 2) heating to 120-180°C, adding the catalyst after the reactants are evenly mixed, and vacuuming;

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

Embodiment 1

[0034] Under the vacuum condition, prepare polyethylene adipate (PEA) and polytetrahydrofuran (PTMO) mass ratio as the alternating multi-block copolymer of 3:1 with ring-opening-condensation polymerization method:

[0035] Add polyethylene adipate cyclic oligomers (COEAs, 15g) and polytetrahydrofuran (M n,PTMO =2900g / mol, 45g), the device was placed in a 120°C salt bath, vacuumed, and mechanically stirred. After stirring evenly, add 60 μL (0.1wt%) tetrabutyl titanate catalyst, vacuumize, and 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] The H NMR spectrum is shown in figure 2 , proving that the target product has been successfully synthesized; in addition, the size exclusion chromatogram is shown in image 3 , which also demonstrated the succ...

Embodiment 2

[0039] Alternating multi-block copolymers with a mass ratio of polybutylene terephthalate (PBT) and polytetrahydrofuran of 3:1 were prepared by ring-opening-condensation polymerization under vacuum conditions:

[0040] In a 50mL three-necked flask, polybutylene terephthalate cyclic oligomers (COBTs, 15g) and polytetrahydrofuran (M n,PTMO =2900g / mol, 45g), the device was placed in a 180°C salt bath, vacuumed, and mechanically stirred. After stirring evenly, add 60 μL (0.1wt%) tetrabutyl titanate catalyst, vacuumize, and the vacuum degree is 1×10 -3MPa. Place the reaction device in a 240°C salt bath, start the reaction, and take samples 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] The H NMR spectrum is shown in Figure 4 , proving that the target product has been successfully synthesized; in addition, the size exclusion chromatogram is shown in Figure 5 , whic...

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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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