Method for preparing mercapto polyether

A technology of mercapto polyether and chlorinated polyether, which is applied in the field of preparation of mercapto-terminated polyether, can solve the problems of low utilization rate of sodium hydrosulfide, poor dispersion of sodium hydrosulfide, etc., and achieve reduction of energy consumption, improvement of utilization rate, and reaction The effect of temperature reduction

Inactive Publication Date: 2010-06-02
BEIJING UNIV OF CHEM TECH
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  • Description
  • Claims
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Problems solved by technology

[0011] In order to overcome the problems of poor dispersion of sodium hydrosulfide and low utilization rate of sodium hydrosulfide in the synthesis reaction of mercapto-terminated polyether, the invention provides a method for preparing mercapto-terminated polyether using alcohols as solvents

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  • Method for preparing mercapto polyether
  • Method for preparing mercapto polyether
  • Method for preparing mercapto polyether

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Embodiment 1

[0023] Preparation of mercapto-terminated polyether:

[0024] Raw materials: chlorinated polyether, the number-average molecular mass Mn=1277, and a functionality of 3; sodium hydrosulfide, with a purity of 70%; ethanol as the solvent.

[0025] Add 250g of chlorinated polyether and 46.99g of sodium hydrosulfide into 200ml of ethanol solvent, heat up to 78°C under stirring, and stop the reaction after reacting at this temperature for 2 hours, remove the salt from the reactant, and distill to obtain a transparent, light yellow liquid Polymer terminated mercapto polyether.

[0026] The synthetic product is liquid at room temperature, and it is 13 C NMR characterization, compared with the NMR spectrum of chlorinated polyether, the characteristic peak at 44.0-45.0ppm disappeared, indicating that the C-CI group was reacted; new characteristic peaks appeared at 25.5ppm and 35.2ppm, indicating that There are C-SH and C-Sx-C (X is 1-5) groups generated. The GPC characterization of t...

Embodiment 2

[0029] Preparation of mercapto-terminated polyether:

[0030] Raw materials: chlorinated polyether, the number-average molecular mass Mn=1277, and a functionality of 3; sodium hydrosulfide, with a purity of 70%; and isopropanol as the solvent.

[0031] Add 250g of chlorinated polyether and 46.99g of sodium hydrosulfide into 250ml of isopropanol solvent, raise the temperature to 82°C under stirring, and stop the reaction after reacting at this temperature for 3 hours, desalinate the reactant, and distill to obtain transparent, shallow Yellow liquid polymer mercapto-terminated polyether.

[0032] The synthetic product is liquid at room temperature, and it is 13 C NMR characterization, compared with the NMR spectrum of chlorinated polyether, the characteristic peak at 44.0-45.0ppm disappeared, indicating that the C-CI group was reacted; new characteristic peaks appeared at 25.5ppm and 35.2ppm, indicating that There are C-SH and C-Sx-C (X is 1-5) groups generated. The GPC chara...

Embodiment 3

[0035] Preparation of mercapto-terminated polyether:

[0036] Raw materials: chlorinated polyether, number average relative molecular mass Mn=1277, functionality 3; sodium hydrosulfide, purity 70%; tert-butanol as solvent.

[0037] Add 250g of chlorinated polyether and 46.99g of sodium hydrosulfide into 300ml of tert-butanol solvent, raise the temperature to 82°C under stirring, and stop the reaction after reacting at this temperature for 3.5 hours, desalt the reactant, and distill it to obtain transparent, shallow Yellow liquid polymer mercapto-terminated polyether.

[0038] The synthetic product is liquid at room temperature, and it is 13 C NMR characterization, compared with the NMR spectrum of chlorinated polyether, the characteristic peak at 44.0-45.0ppm disappeared, indicating that the C-CI group was reacted; new characteristic peaks appeared at 25.5ppm and 35.2ppm, indicating that There are C-SH and C-Sx-C (X is 1-5) groups generated. The GPC characterization of the ...

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Abstract

The invention relates to a preparation method of end-mercapto polyether, belonging to adhesive field. The deficits of the present preparation method of end-mercapto polyether: the solubleness of product obtained by reacting polyalkylene diol and epoxy halopropane in sodium hydrosulphide is poor and the availability of sodium hydrosulphide is reduced, therefore the difficulty is added to the post-treatment. The chloride polyether, sodium hydrosulphide and alcohol material are mixed together and react for 2-5 hours at boiling point of alcohol material to 40 degree, wherein the quantity relativeratio of alcohol material and sodium hydrosulphide is 3-18:1, the quantity relative ratio of chloride polyether and sodium hydrosulphide is 1:2-3.5. The availability of the sodium hydrosulphide is greatly increased. In addition, the displacement reaction of chloride polyether and sodium hydrosulphide occurs in alcohol material, the reaction temperature is reduced, so as to reduce the energy consumption.

Description

Technical field: [0001] The invention relates to a method for preparing a mercapto-terminated polyether using alcohols as a solvent, in particular to a method for preparing a mercapto-terminated polyether that significantly improves the dispersibility of sodium hydrosulfide. The mercapto-terminated polyether belongs to the field of adhesives . Background technique: [0002] Mercapto-terminated polyether can be used in sealants containing a small amount of plasticizer. As a curable component, mercapto-terminated polyether will hardly transfer from the sealant to the coating on the surface of the object, thus avoiding the softening of the coating. Mercapto-terminated polyether can also be used as a curing agent for epoxy resin, with fast curing speed and durable cured product. Sealants, coatings and adhesives prepared from mercapto-terminated polyethers have high resistance to oxygen, ozone, organic solvents, oils and fuels. [0003] When a single molecule contains two or mo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/338C08G65/48
Inventor 张军营刘殿君
Owner BEIJING UNIV OF CHEM TECH
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