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A kind of synthetic method of hydroquinone dihydroxyethyl ether

The technology of dihydroxyethyl ether and hydroquinone, which is applied in the field of organic compound synthesis, can solve problems such as complex process, and achieve the effects of high product purity, few by-products, and effective and reasonable synthesis process.

Active Publication Date: 2018-03-20
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The obtained product has transparent appearance, good color, high yield and high purity, but the process is complex and requires decolorization and water removal

Method used

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  • A kind of synthetic method of hydroquinone dihydroxyethyl ether
  • A kind of synthetic method of hydroquinone dihydroxyethyl ether
  • A kind of synthetic method of hydroquinone dihydroxyethyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 550g of hydroquinone, 1.0g of 1,1'-bis(diphenylphosphino)ferrocene, and 440g of ethylene glycol di-n-butyl ether into the reaction kettle, vacuumize with a vacuum pump, and replace the inside of the reaction kettle with nitrogen After replacing the air three times, under the protection of nitrogen, the temperature was raised to 110°C, and the temperature was kept for 3-4 hours, and the material in the kettle was completely dissolved. When the hydroquinone is completely melted, vacuumize at this temperature for 20 minutes to remove the low-boiling substances in the kettle, then continue to add 440g of ethylene oxide, and complete the addition within 3 hours, and control the reaction temperature at 125-130°C. The pressure of the reaction kettle is -0.05-0.4Mpa. After adding, keep warm for 7 hours to continue the reaction; after the reaction is completed, cool down to 80°C, vacuum degass to remove unreacted ethylene oxide, and gradually heat up the mother liquor to 125°...

Embodiment 2

[0037]Add 434 g of ethylene glycol di-n-butyl ether recovered in Example 1 together with 550 g of hydroquinone and 1.0 g of 1,1'-bis(diphenylphosphino)ferrocene into the reaction kettle, and vacuumize with a vacuum pump. Use nitrogen to replace the air in the reactor. After three replacements, under the protection of nitrogen, raise the temperature to 110° C., keep the temperature for 3-4 hours, and the materials in the reactor are completely dissolved. When the hydroquinone is completely melted, vacuumize at this temperature for 20 minutes to remove the low-boiling substances in the kettle, then continue to add 440g of ethylene oxide, and complete the addition within 3 hours, and control the reaction temperature at 125-130°C. The pressure of the reaction kettle is -0.05-0.4Mpa. After adding, keep warm for 7 hours to continue the reaction; after the reaction is completed, cool down to 80°C, vacuum degass to remove unreacted ethylene oxide, and gradually heat up the mother liquo...

Embodiment 3

[0040] Add 550g of hydroquinone, 0.5g of 1,1'-bis(diphenylphosphino)ferrocene, and 330g of diethylene glycol diethyl ether into the reactor, vacuumize with a vacuum pump, and replace the nitrogen in the reactor with nitrogen. After the air is replaced three times, under the protection of nitrogen, the temperature is raised to 100 ° C, and the temperature is kept for 3-4 hours, and the material in the kettle is completely dissolved. When the hydroquinone is completely melted, vacuumize at this temperature for 20 minutes to remove the low-boiling substances in the kettle, then continue to add 484g of ethylene oxide, and complete the addition within 4 hours, and control the reaction temperature at 130-135°C. The pressure of the reaction kettle is -0.05-0.4Mpa. After adding, keep warm for 5 hours to continue the reaction; after the reaction is completed, cool down to 80°C, vacuum degass to remove unreacted ethylene oxide, and gradually heat up the mother liquor to 115°C and distill...

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Abstract

The invention relates to a method for synthesizing hydroquinone dihydroxyl diethyl ether and belongs to the technical field of synthesis of organic compounds. The method comprises the steps: carrying out synthesis by taking hydroquinone and epoxyethane as raw materials, adding hydroquinone, a ferrocene catalyst and an ether solvent into a reactor, carrying out vacuumizing, heating the reactor until hydroquinone is completely dissolved in the ether solvent under nitrogen protection, then, adding a chain extender into the reactor, heating the reactor to a polymerization reaction temperature, and carrying out hydroquinone dihydroxyl diethyl ether synthesis under polymerization reaction pressure; and after the reaction ends, carrying out cooling, and subjecting crystallizing mother liquor to normal-pressure or reduced-pressure rectification, so as to separate out the ether solvent. The hydroquinone dihydroxyl diethyl ether is synthesized by the method, the problems in the conventional technologies that the preparation process is complicated and the quality of product is poor are solved, and the obtained product is reasonable in distribution, light in color and luster and low in byproduct content.

Description

technical field [0001] The invention relates to a method for synthesizing hydroquinone bishydroxyethyl ether, which belongs to the technical field of organic compound synthesis. Background technique [0002] Hydroquinone bishydroxyethyl ether, referred to as HQEE, also known as hydroquinone bishydroxyethyl ether, is a new type of low-toxic chain extender for polyurethane elastomers. It is a diol containing an aromatic ring and a linear symmetrical structure, and can be widely used in polyurethane elastomers. It has good compatibility with MDI (diphenylmethane diisocyanate), which can significantly improve the tensile strength, hardness and resilience of products. HQEE / MDI is a series of polyurethane (PU) elastomers juxtaposed with MOCA / TDI (diaminodichlorodiphenylmethane / toluene diisocyanate). The PU used in this product is generally used in fields with high requirements for product physical properties. Such as: oil well seals, forklift tires, hydraulic cylinder seals, con...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/23C07C41/03
CPCC07C41/03C07C43/23
Inventor 金一丰颜吉校马定连金洪财
Owner ZHEJIANG HUANGMA TECH
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