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Method for preparing ethylene glycol ether

A glycol ether and aliphatic alcohol technology, applied in the field of glycol ether preparation, can solve the problems of low selectivity of glycol ether, no catalyst stability, high molar ratio of alcohol/ethylene oxide, etc., to achieve High selectivity, excellent reaction performance, and low alcohol-to-alkane ratio

Active Publication Date: 2008-06-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The technical problem to be solved by the present invention is that there is low selectivity of the target product glycol ether in the prior art, the alcohol / ethylene oxide molar ratio (alcohol / alkane ratio) is high and does not involve the problem of catalyst stability, and a new The preparation method of glycol ether, the method has the advantages of high glycol ether selectivity, low alcohol-to-alkane ratio and good catalyst stability

Method used

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  • Method for preparing ethylene glycol ether
  • Method for preparing ethylene glycol ether
  • Method for preparing ethylene glycol ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 100 g of ZSM-5 zeolite (SiO 2 / Al 2 o 3 Molar ratio 60, ammonium type) add 65 milliliters of 10% (weight) dilute nitric acid, fully knead in the kneader, form agglomerate material, extrude molding, dry at 150 ℃ for 2 hours, 800 ℃ roast for 4 hours, obtain Strip carrier. The niobium oxalate solution was impregnated on the prepared ZSM-5 carrier, and dried at 120°C for 2 hours; then the ammonium metavanadate was dissolved in 5% (weight) hydrogen peroxide, impregnated on the catalyst again, and dried at 120°C for 2 hours; Finally, lanthanum trichloride aqueous solution was impregnated on the catalyst, dried at 120°C for 2 hours, and calcined in air at 400°C for 4 hours to obtain catalyst A, whose composition is shown in Table 1.

Embodiment 2

[0034] Fully mix 67.6 grams of aluminum hydroxide, 40 grams of silicon dioxide, and 4 grams of cyclodextrin, then add 60 milliliters of 4% (weight) dilute nitric acid, fully knead in a kneader to form a lump material, and extrude , dried at 150°C for 2 hours, and calcined at 1400°C for 4 hours to obtain a strip-shaped carrier. Use a certain concentration of ammonium molybdate solution of 125 mmol / ml to impregnate the above-mentioned carrier at room temperature, the volume ratio of impregnated liquid to solid is 2:1, impregnate for 2 hours, filter the solution, and dry in vacuum at 120°C for 2 hours; then use a certain 15% niobium ammonium complex solution (NH 4 [NbO(C 2 o 4 )2 (H 2 O) 2 ]·(H 2 O) n ) continue to impregnate the above-mentioned treated carrier at room temperature, the volume ratio of impregnation liquid to solid is 2:1, the impregnation time is 2 hours, the solution is filtered off, and vacuum-dried at 120°C for 2 hours, so impregnation is carried out thre...

Embodiment 3

[0036] Fully mix 113 grams of aluminum hydroxide powder, 5 grams of graphite, and 5 grams of squash powder, then add 60 milliliters of 4% (weight) dilute nitric acid, fully knead in a kneader to form a lump material, and extrude , dried at room temperature for 24 hours, dried at 150°C for 2 hours, and calcined at 1200°C for 4 hours to obtain strip-shaped α-Al 2 o 3 carrier. Impregnating α-Al with a mixed solution of magnesium nitrate and aluminum nitrate 2 o 3 Carrier, dried at 150°C for 2 hours, and calcined again at 1200°C for 4 hours to obtain MgAl 2 o 4 / α-Al 2 o 3 carrier. Immerse the carrier with a neodymium chloride aqueous solution with a concentration of 39.88 mg / ml at room temperature for 2 hours, the liquid-solid volume ratio is 2.5:1, filter the solution, and dry it in vacuum at 120° C. for 2 hours to obtain the carrier 1; Carrier 1 was continuously impregnated in vacuum with a liquid-to-solid volume ratio of 2.0:1, the solution was filtered off, and vacuum...

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Abstract

The invention relates to a glycol ether preparation method, mainly solving the problems of the original technique that the target product, glycol ether, has low selectivity, high alcohol / epoxy ethane ratio (alcohol / alkyl ratio) and no concern on catalyst stability. The invention uses epoxy ethane and lower fatty alcohol as raw materials, adopts niobium oxide as a main activated component, and chooses at least one of elements or compounds of V, Mo, Sn, Pb, La, Pr, Nd as auxiliary agent to form catalyst, so as to prepare glycol ether under the reaction temperature of 100 to 300 DEG C, reaction pressure of 0.1 to 3.0MPa, alcohol / alkyl ratio of 1-5: 1, and reaction time of 30 minutes to 8.0 hours. The technical proposal can well solve the problem and can be used for the industrial production of the glycol ether.

Description

technical field [0001] The invention relates to a method for preparing glycol ethers, in particular to a method for preparing glycol ethers by reacting ethylene oxide with low-carbon fatty alcohols. Background technique [0002] Glycol ether series products have both ether bonds and different alkyl groups in their molecules, so they can dissolve small organic molecules, macromolecules, synthetic or natural polymer substances, and can also be soluble in water or water to varying degrees. The compounds are soluble in each other, so they are widely used as solvents, antifreeze agents, brake fluids, cleaning agents, chemical intermediates, etc. [0003] Glycol ether series products are mainly etherified by ethylene oxide (EO) and low-carbon fatty alcohols to obtain corresponding glycol ethers and a small amount of diethylene glycol ether and triethylene glycol ether. The synthesis principle is as follows: [0004] [0005] When there is no catalyst, it can be carried out at ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/03C07C43/10B01J29/48B01J23/28B01J21/16
Inventor 李应成何文军费泰康何立
Owner CHINA PETROLEUM & CHEM CORP
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