Preparation method preparation method of low-molecular-weight polyether polyol for polyetheramine

A low-molecular-weight polyether and polyether polyol technology, which is used in the preparation of ethers, the preparation of ethers from alkylene oxide, and organic chemistry, can solve the problems of unstable product quality, wide molecular weight distribution, and low amine end capping rate. Strong bending resistance, improved amine value, good mutual solubility

Active Publication Date: 2016-12-21
SHANDONG INOV NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And the low-molecular-weight polyether polyol that traditional technique synthesizes, from GPC spectrogram (see figure 1 ) can be seen that the molecular weight distribution is wide, and there are multiple miscellaneous peaks. Using such polyether polyols to prepare polyetheramines has low amine end-capping rate, large activity deviation, and unstable product quality.

Method used

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  • Preparation method preparation method of low-molecular-weight polyether polyol for polyetheramine
  • Preparation method preparation method of low-molecular-weight polyether polyol for polyetheramine
  • Preparation method preparation method of low-molecular-weight polyether polyol for polyetheramine

Examples

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Effect test

Embodiment 1

[0027] Add 270g of 2-methyl-1,3-propanediol and 2.4g of sodium hydroxide into a 2.5L autoclave at room temperature, evacuate to -0.09MPa and replace with nitrogen three times, start stirring and raise the temperature to 80°C. Under the vacuum degree of -0.09MPa, 150g of epoxides were continuously added dropwise, including 30g of propylene oxide and 120g of ethylene oxide. The pressure in the reaction kettle is ≤0.4MPa, the reaction temperature is 80-95°C, and the aging reaction is continued for 1 hour after the feeding is completed to obtain the intermediate polyether polyol. Heat up to 100°C, then continuously add 180g of propylene oxide dropwise, continue to react for a period of time, control the reaction temperature at 100-120°C, and the reaction pressure is ≤0.4MPa, wait until the pressure is stable and does not change for 30 minutes, then vacuumize the pressure ≤- Under 0.09MPa, the unreacted propylene oxide monomer is removed, and the polymerization reaction is complete...

Embodiment 2

[0029] Add 360g of 2-methyl-1,3-propanediol and 8.32g of potassium hydroxide into a 2.5L autoclave at room temperature, evacuate to -0.09MPa and replace with nitrogen three times, start stirring and raise the temperature to 80°C. Under the vacuum degree of -0.09MPa, 860g of epoxides were continuously added dropwise, including 420g of propylene oxide and 420g of ethylene oxide. The pressure in the reaction kettle is ≤0.4MPa, the reaction temperature is 80-95°C, and the aging reaction is continued for 1 hour after the feeding is completed to obtain the intermediate polyether polyol. Heat up to 100°C, then continuously drop 860g of propylene oxide, continue to react for a period of time, the reaction temperature is controlled at 100-120°C, the reaction pressure is ≤0.4MPa, wait until the pressure is stable and does not change for 30 minutes, and the vacuum pressure is ≤- Under 0.09MPa, the unreacted propylene oxide monomer is removed, and the polymerization reaction is completed....

Embodiment 3

[0031] Add 180g of 2-methyl-1,3-propanediol and 8g of potassium hydroxide into a 2.5L autoclave at room temperature, evacuate to -0.09MPa and replace with nitrogen three times, start stirring and raise the temperature to 80°C. Under the vacuum degree of -0.09MPa, 1229g of epoxide was added dropwise continuously, all of which were propylene oxide. The pressure in the reaction kettle is ≤0.4MPa, the reaction temperature is 80-95°C, and the aging reaction is continued for 1 hour after the feeding is completed to obtain the intermediate polyether polyol. Heat up to 100°C, then continuously drop 600g of propylene oxide, and continue to react for a period of time, the reaction temperature is controlled at 100-120°C, the reaction pressure is ≤0.4MPa, wait until the pressure is stable and does not change for 30 minutes, and the vacuum pressure is ≤- Under 0.09MPa, the unreacted propylene oxide monomer is removed, and the polymerization reaction is completed. Cool down to below 90°C, ...

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Abstract

The invention belongs to the technical field of polyether polyol synthesis and specifically relates to a preparation method of low-molecular-weight polyether polyol for polyetheramine. According to the preparation method, 2-methyl-1,3-propylene glycol, which is used as a starting agent, reacts with epoxide in the presence of an alkali metal catalyst at low temperature; and then, the reaction product is end-capped with epoxypropane at high temperature so as to obtain low-molecular-weight polyether polyol for polyetheramine. During the polymerization, 2-methyl-1,3-propylene glycol is used as the starting agent. Due to structural regularity and symmetry of 2-methyl-1,3-propylene glycol, activities at two ends are identical. During polymerization between 2-methyl-1,3-propylene glycol and the epoxide, polyether structure is more regular. During amino-capping, activities at two ends are consistent. The product has characteristics of amorphism, strong weatherability, tension resistance, strong bending resistance and the like. By the structure, polyetheramine can be endowed with characteristics of low melting point, low viscosity and good intersolubility with auxiliaries.

Description

technical field [0001] The invention belongs to the technical field of polyether polyol synthesis, and in particular relates to a preparation method of low molecular weight polyether polyol for polyether amine. Background technique [0002] Polyether amine is a kind of polymer whose main chain is polyether polyol structure and the terminal active functional group is amine group. Polyetheramines are obtained by amination of polyether polyols of polyethylene glycol, polypropylene glycol or ethylene glycol / propylene glycol copolymers at high temperature and pressure. Polyetheramine can be used as a high-performance curing agent for epoxy resins to produce high-strength, high-toughness composite materials; it has low viscosity, and can reduce the amount of solvents and lower the system when applied to epoxy floors or anti-corrosion coatings. Viscosity; as a key component of polyurea materials, there are many application examples in the waterproofing system of concrete structure...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/03C07C43/11
CPCC07C41/03C07C43/11
Inventor 王玉孙兆任李剑锋周玉波杨凯
Owner SHANDONG INOV NEW MATERIALS CO LTD
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