Preparation method of polyether diol

A technology of polyether diol and polyether monool, which is applied in the field of preparation of polyether diol, and achieves the effects of cheap and easy-to-obtain raw materials, high yield, and mild reaction conditions

Active Publication Date: 2013-07-10
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there is no public report about the mature process route for the preparation of this type of compound

Method used

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  • Preparation method of polyether diol
  • Preparation method of polyether diol
  • Preparation method of polyether diol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Preparation of compound (3)

[0038] Add 268g of trimethylolpropane, 928g of acetone and 9.16g of ferric sulfate into a three-necked flask, raise the temperature to 56°C, and keep the reaction for 7 hours to obtain a yellow reaction solution. Add potassium acetate aqueous solution to the reaction solution to adjust the pH value to approximately equal to 7, and then collect the yellow filtrate by filtration; use dichloromethane to perform liquid-liquid extraction on the filtrate, collect the dichloromethane phase, dry it over anhydrous sodium sulfate, and filter it at 45°C Distillation under reduced pressure (vacuum degree: 0.098 MPa) gave 320 g of a light yellow transparent liquid with a yield of 92.0%. Such as figure 1 and 2 As shown, the product was determined to be 2,2-dimethyl-1,3-dioxane-5-ethyl-5-methanol by GC and NMR analysis.

[0039]The gas phase analysis conditions are: Shimadzu 2010 gas chromatograph (FID detector), chromatographic column type DB-5, c...

Embodiment 2

[0054] (1) Preparation of compound (3)

[0055] Add 268g of trimethylolpropane, 696g of acetone and 2.15g of strong acidic resin into a three-necked flask, raise the temperature to 56°C, and keep the reaction for 7h. The reaction solution was filtered to obtain a colorless transparent solution, which was distilled under reduced pressure at 45°C (vacuum degree: 0.098MPa) to obtain 311g of a light yellow transparent liquid, namely the compound 2,2-dimethyl-1,3-dioxane-5- Ethyl-5-methanol, the yield is 89.5%, and the product purity is 99.3%.

[0056] The product structure is:

[0057]

[0058] (2) Preparation of polyether monoalcohol (4)

[0059] Accurately weigh 1063g of ethylene oxide and put it into a storage tank, put 87g of compound (3) and 5.75g of KOH into a 2L reaction kettle, replace the air with nitrogen three times, then heat up to 95°C for vacuum dehydration for 1h (vacuum degree is 0.098 MPa), then start to add ethylene oxide, keep the temperature in the kettle...

Embodiment 3

[0067] (1) Preparation of compound (3)

[0068] Add 268g of trimethylolpropane, 464g of acetone and 6.7g of acid clay into a three-necked flask, raise the temperature to 45°C, and keep the temperature for 5h. The reaction solution was filtered to obtain a colorless and transparent solution, which was distilled under reduced pressure at 45°C (vacuum degree of 0.098MPa) to obtain 295g of a light yellow transparent liquid, namely the compound 2,2-dimethyl-1,3-dioxane-5- Ethyl-5-methanol, the yield is 84.7%, and the product purity is 99.6%.

[0069] The product structure is:

[0070]

[0071] (2) Preparation of polyether monoalcohol polyether monoalcohol (4)

[0072] Accurately weigh 1663g ethylene oxide and put it into the storage tank, and 87g compound (3) and 8.75gBa(OH) 2 Put it into a 2L reaction kettle, replace the air with nitrogen three times, then heat up to 95°C for vacuum dehydration for 1h (vacuum degree is 0.098MPa), then start adding ethylene oxide, keep the te...

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Abstract

The invention relates to a preparation method of a polyether diol. The polyether diol has a structure shown in the formula 1. The preparation method can design products having different molecular weights according to demands. The preparation method comprises the following steps that trimethylolpropane and an aldehyde or a ketone undergo an aldolization (ketalation) reaction to produce a compound (3); ethylene oxide is polymerized into a polyether monoalcohol in the presence of the compound (3) as an initiator; the polyether monoalcohol and dimethyl sulfate or dimethyl carbonate or a haloalkane undergo a Williamson reaction to produce a methyl-terminated polyether product; and the methyl-terminated polyether product undergoes a ring-opening reaction to produce polyether diol. The preparation method has the advantages of simple processes, high efficiency, low raw material cost, wide raw material sources and good industrialization prospect.

Description

Technical field: [0001] The invention relates to a preparation method of polyether diol, which belongs to polyether diol nonionic reactive surface active agent and is mainly used for water-based polyurethane emulsion. Background technique: [0002] Emulsifiers are surface active substances that can make two immiscible liquids form a stable solution dispersion system under certain conditions. It is one of the main components in the preparation of water-based polyurethane coatings. Although its dosage is small, it plays a decisive role in the process of forming water-based polyurethane emulsion. Traditional emulsion polymerization uses anionic surfactants and nonionic surfactants as emulsifiers. Anionic surfactants include sulfonates (alkyl sulfonates, alkylbenzene sulfonates, succinate sulfonates, etc.) , sulfate esters (fatty alcohol sulfate, fatty alcohol ether sulfate, etc.), carboxylates, phosphates, etc.; nonionic surfactants include polyoxyethylene ether type (fatty al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/327C08G65/334C08G65/32C08G65/16C08G18/48B01F17/42A61K8/86C09K23/42
Inventor 刘瑞阳陈海波叶天郭可银鞠昌迅黄长荣李晶隋宝华丁建生华卫琦
Owner WANHUA CHEM GRP CO LTD
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