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Method for synthesizing polyether amine

A technology for polyether amine and polyether polyol, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxy compounds, etc., can solve the problems of reducing the conversion rate of polyether, inconvenient product separation, polluting the environment, etc. Lower activation energy, easier control of synthesis reaction conditions, and fewer by-products

Pending Publication Date: 2020-02-18
ZHEJIANG LYUKEAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, they all have the disadvantages that the added reagents are toxic, pollute the environment and are not easy to purchase, especially the side reactions are more, and the by-products are more, which reduces the conversion rate of polyether, and needs to be added in the post-treatment process. A large amount of acid or alkali is neutralized to generate a large amount of inorganic salts. In view of the compatibility of the target product polyetheramine and inorganic salts, it will inevitably bring inconvenience to the separation of the products.

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  • Method for synthesizing polyether amine
  • Method for synthesizing polyether amine
  • Method for synthesizing polyether amine

Examples

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Embodiment 1

[0042]

[0043] A method for synthesizing polyetheramine, specifically comprising the following steps:

[0044] S1. Preparation of ethylene glycol polyoxyethylene (10) ether: pump 1 mol of ethylene glycol with a mass of 62 g into the glass-lined reactor, and pump in an aqueous solution containing 4.0 g of KOH. After the pumping is complete, close the vacuum valve. replace N 2 Three times, vacuum degree ≥ -0.098MPa, displacement pressure ≥ 0.02MPa. replace N 2 After completion, slowly raise the temperature, control the temperature at 105±2°C, and dehydrate for 1.0h. After the dehydration is completed, raise the temperature to above 120°C and try to add 10mol of 440g EO, control the reaction temperature to 145-150°C, and the pressure to be ≤0.30Mpa. After the reaction is completed, the temperature is lowered to 100° C. for degassing, and the material is discharged to obtain the crude product of ethylene glycol polyoxyethylene (10) ether.

[0045] S2. Preparation of polyet...

Embodiment 2

[0049] The preparation method of this example is the same as that of Example 1, the difference from Example 1 is that the amount of EO added is different, and the amount of each added reagent also changes with the change of EO, see Table 1 for details.

[0050] Table 1 Amino-terminated glycol polyoxyethylene ethers of different specifications

[0051]

[0052] It can be seen from Table 1 that when the molar ratio of the initiator ethylene glycol to EO is in the range of 1:3-1:20, the conversion rate of the prepared polyetheramine is greater than 96%. properties are greater than 97%, and with the increase of molecular weight, the conversion rate and primary amine selectivity gradually decrease, therefore, the method of the present invention is more suitable for the synthesis of small molecular weight polyetheramine products.

Embodiment 3

[0054] A method for synthesizing polyetheramine, specifically comprising the following steps:

[0055]

[0056] S1. Preparation of propylene glycol polyoxypropylene (10) ether: pump 1 mol of 76 g of 1,2-propylene glycol into the glass-lined reactor, and pump in an aqueous solution containing 5.3 g of NaOH. After the pumping is complete, close the vacuum valve. replace N 2 Three times, vacuum degree ≥ -0.098MPa, displacement pressure ≥ 0.02MPa. replace N 2 After completion, slowly raise the temperature, control the temperature at 105±2°C, and dehydrate for 1.0h. After the dehydration is completed, raise the temperature to above 120°C and try to add 10mol of PO with a mass of 580g, control the reaction temperature at 145-150°C, and the pressure ≤0.30Mpa. After the reaction is completed, the temperature is lowered to 100° C. for degassing, and the material is discharged to obtain the crude product of propylene glycol polyoxypropylene (10) ether.

[0057] S2. Preparation of...

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Abstract

The invention discloses a method for synthesizing polyether amine, and belongs to the technical field of organic polymer synthesis. The method for synthesizing polyether amine comprises the followingsteps: adding alkylene oxide to polyfunctional alcohol which is used as an initiator, and carrying out a polymerization reaction under the action of a catalyst to synthesize polyether polyol; adding an esterifying agent, and carrying out an esterification reaction on the terminal hydroxyl group of the polyether polyol and the esterifying agent to obtain an ester; and carrying out an amination reaction on the obtained ester and an aminating agent to obtain the polyether amine. The synthesis method has the advantages of mild reaction conditions, few byproducts, short reaction period, conveniencein post-treatment, high conversion rate of the obtained polyether amine and high selectivity of the primary amine, and the obtained polyether amine has the advantages of high activity and wide application range.

Description

technical field [0001] The invention relates to the technical field of organic polymer synthesis, in particular to a method for synthesizing polyetheramine. Background technique [0002] Polyetheramine (PEA), also known as Amine-Terminated Polyethers, is a class of compounds with a polyoxyalkylene structure as the main chain and terminal amine groups as active functional groups. Since the amine hydrogen at the end of polyetheramine has stronger reactivity than the hydroxyl hydrogen at the end of polyether, it can react with a variety of compounds, which greatly broadens the application range of polyetheramine in the industrial field. According to the number of substituted hydrogen atoms in the amine group, polyetheramine can be divided into primary amine polyetheramine and secondary amine polyetheramine. Common polyetheramines in industry are polyethylene oxide diamine, poly Primary amine polyether amines such as propylene oxide diamine, polyethylene oxide / polypropylene oxi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/325C08G65/333C07C227/08C07C229/30C07C213/00C07C217/08C07C213/02
CPCC08G65/3255C08G65/33306C07C227/08C07C213/00C07C213/02C08G2650/04C07C229/30C07C217/08
Inventor 赵世聪余江王胜利向松柏金凌熠
Owner ZHEJIANG LYUKEAN CHEM
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