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Method for preparing polymer polyether polyol by semi-continuous dispersion polymerization process

A technology of polyether polyol and dispersion polymerization, which is applied in the field of semi-continuous dispersion polymerization to prepare polymer polyether polyol, which can solve the difficulty of controlling macromonomer structure and molecular weight, unsatisfactory reproducibility, and reduced dispersion efficiency, etc. problem, to achieve the effect of structurally controllable chain transfer ability, strong stability, and low viscosity increase

Active Publication Date: 2019-11-12
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These complex reactions and process control make it difficult to control the structure and molecular weight of macromonomers, and the reproducibility is not ideal.
In addition, macromonomers will also undergo self-aggregation during long-term storage, which will reduce the dispersion efficiency
However, there are no reports on the use of macromolecular RAFT agents as stabilizers for the preparation of polymer polyether polyols

Method used

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  • Method for preparing polymer polyether polyol by semi-continuous dispersion polymerization process
  • Method for preparing polymer polyether polyol by semi-continuous dispersion polymerization process
  • Method for preparing polymer polyether polyol by semi-continuous dispersion polymerization process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Embodiment 1 Polyether 210 is the preparation of medium, solid containing 45% POP

[0068] (1) Stabilizer S (ABPO600-MA) 50 20 Preparation of:

[0069] Z group is phenyl, R 1 for H, R 2 is butyl, R 3 for H, R 4 for-COOCH 3 , R is benzyl;

[0070] p=1, x=0.5, m=10, n=20;

[0071]Take by weighing 32.7g (50mmol) polyether acrylate (ABPO600), 4.3g (50mmol) methyl acrylate (MA), 1.67g (5mmol) benzyl N-carbazole dithioformate (BCBD) and 0.192g ( Add 1.0mmol) azobisisovaleronitrile (ABMN) into a 50ml four-necked reaction flask. After the dissolution is complete, pass nitrogen to remove oxygen for 30min, place it in a water bath at 70°C and stir for 12h under dark conditions to obtain the stabilizer S (ABPO600-MA) 50 20 .

[0072] figure 1 Be the stabilizer S (ABPO600-MA) prepared by embodiment 1 50 20 of 1 H NMR spectrum. like figure 1 As shown, the chemical shift is at 2.32ppm, and the peak at 1.55ppm belongs to S(ABPO600-MA) 50 20 The methine (a) and meth...

Embodiment 2

[0080] Embodiment 2 Polyether 220 is the preparation of medium, solid containing 30% POP

[0081] (1) Stabilizer S (MBPO600-MMA) 40 40 preparation of

[0082] Z group is phenyl, R 1 for CH 3 , R 2 is butyl, R 3 for CH 3 , R 4 for-COOCH 3 , R is isobutyronitrile;

[0083] p=1, x=0.4, m=10, n=40;

[0084] Weigh 26.7g (40mmol) polyether methacrylate (MBPO600), 6.0g (60mmol) methyl methacrylate (MMA), 0.55g (2.5mmol) isobutyronitrile dithiobenzoate (CPDB) and Add 0.248g (1.0mmol) of azobisisoheptanonitrile (ABVN) into a 50ml four-necked reaction flask. After the dissolution is complete, pass nitrogen to remove oxygen for 30min, place it in a water bath at 70°C and stir for 12h under dark conditions to obtain Stabilizer S (MBPO600-MMA) 40 40 .

[0085] Product S(MBPO600-MMA) 40 40 of 1 The H NMR spectrum shows: signal peaks at 3.21-3.62ppm and 1.1ppm from propylene oxide in the polyether side chain, from methyl (0.86ppm) and methylene (1.20-ppm) in the terminal but...

Embodiment 3

[0091] Embodiment 3-6 is the preparation of POP with 42% solid content

[0092] (1) Preparation of stabilizer

[0093] Weigh polyether acrylate (compound (Ⅱ)), small molecule monomer (M), RAFT reagent (compound (Ⅲ)) and 0.164g (1.0mmol) azobisisobutyronitrile (AIBN), add 50ml four-port In the reaction bottle, after the dissolution is complete, pass nitrogen to deoxygenate for 30 minutes, place in a constant temperature water bath, stir and react for a certain period of time under dark conditions to obtain a stabilizer. The specific materials, dosage and reaction conditions are shown in Table 1.

[0094] Synthetic formula and reaction conditions of different structural stabilizers of table 1

[0095] (the numerical value in the table is the weight and the number of moles of each material, g (mmol))

[0096]

[0097] The prepared product of embodiment 3 1 The H NMR spectrum shows the characteristic peaks of polyether ester side chains at 3.21-3.62ppm, 1.1ppm, 0.86ppm and ...

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Abstract

The invention belongs to the technical field of preparation of polymer polyether polyol, and discloses a method for preparing polymer polyether polyol by a semi-continuous dispersion polymerization process. The method adopts a copolymer of poly(methyl) methacrylate containing dithiocarboxylic ester group is a stabilizer, vinyl monomer, the polyether polyol and an initiator are mixed to prepare monomer feed liquid; the polyether polyol, the stabilizer and the initiator are mixed and stirred in a reactor provided with a stirrer; the reactor is heated to the reaction temperature, and the monomerfeed liquid is continuously and uniformly added to the reactor under stirring; after the monomer feed liquid is added, the initiator is additionally added, and the reaction temperature is maintained to continue the reaction; and after a reaction product is vacuumed to remove residual monomers, a product POP is obtained by cooling and discharging. The method can produce a stable POP product with high solid content and low viscosity, and the polymerization process and the product POP have good stability and reproducibility; and the production process is easy to control and the operation window is wide.

Description

technical field [0001] The invention belongs to the technical field of preparation of polymer polyether polyols, and in particular relates to a method for preparing polymer polyether polyols by a semi-continuous dispersion polymerization process. Background technique [0002] Polyether polyol is a polyether with multiple terminal hydroxyl functional groups. It mainly uses a compound containing multiple active hydrogens as an initiator to trigger propylene oxide (PO) or ethylene oxide (EO) in the presence of a catalyst. It is prepared by ring-opening polymerization and is an important polyurethane raw material. Polyether polyols include homopolyethers of propylene oxide and copolyethers of propylene oxide and ethylene oxide. According to the method of adding ethylene oxide, the copolyether can be a random copolyether, and the chain end of the polyether polyol is mainly composed of secondary hydroxyl groups; it can also be a block copolyether, and the EO block is mainly distr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/06C08F212/08C08F220/44C08F2/38C08F220/14
CPCC08F2/38C08F283/06C08F283/065C08F212/08C08F220/44C08F220/14
Inventor 郭睿威朱玉杰
Owner TIANJIN UNIV