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Method for preparing polyoxymethylene dimethylethers from methanol and formaldehyde

A polymethoxydimethyl ether and methanol technology, which can be used in chemical instruments and methods, preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, etc., and can solve problems such as unsatisfactory selectivity

Active Publication Date: 2015-07-15
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, when referring to making PODE by the reaction of methanol and formaldehyde, the catalyst used is an acidic catalyst, which leads to products (especially PODE n＞2 ) selectivity is not ideal, therefore, there is still room for improvement in the prior art

Method used

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  • Method for preparing polyoxymethylene dimethylethers from methanol and formaldehyde
  • Method for preparing polyoxymethylene dimethylethers from methanol and formaldehyde
  • Method for preparing polyoxymethylene dimethylethers from methanol and formaldehyde

Examples

Experimental program
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Effect test

preparation example Construction

[0010] (1) Carrier (γ-Al 2 o 3 ) preparation:

[0011] Prepare aluminum sulfate in water at 60°C to 70°C to make an aqueous solution with a relative density of 1.21 to 1.23, and at the same time prepare Na with a mass percentage of 20%. 2 CO 3 aqueous solution;

[0012] Under the condition of 50 ℃ ~ 60 ℃, the aluminum sulfate aqueous solution with a relative density of 1.21 ~ 1.23 and 20% by mass percent of Na 2 CO 3 The aqueous solution is mixed, there is precipitation, filter, and the filter cake is washed with distilled water at a temperature of 50 ° C to 60 ° C until the washing liquid does not contain SO 4 2- ions (can pass Ba 2+ detection);

[0013] Put the washed filter cake in ammonia water with a temperature of 50°C-60°C and a pH value of 9.0-11.0, let it stand for at least 4 hours (curing), filter, and use distilled water at a temperature of 50°C-60°C again for the filter cake Wash until the specific resistance of the washing liquid is greater than 200 Ω / cm,...

Embodiment 1

[0023] Carrier (γ-Al 2 o 3 ) preparation:

[0024] Prepare aluminum sulfate in water at 60°C to 70°C to make an aqueous solution with a relative density of 1.21 to 1.23, and at the same time prepare Na with a mass percentage of 20%. 2 CO 3 aqueous solution;

[0025] Under the condition of 50 ℃ ~ 60 ℃, the aluminum sulfate aqueous solution with a relative density of 1.21 ~ 1.23 and 20% by mass percent of Na 2 CO 3 The aqueous solution is mixed, there is precipitation, filter, and the filter cake is washed with distilled water at a temperature of 50 ° C to 60 ° C until the washing liquid does not contain SO 4 2- ions (can pass Ba 2+ detection);

[0026] Put the washed filter cake in ammonia water with a temperature of 50°C-60°C and a pH value of 9.0-11.0, let it stand for at least 4 hours (curing), filter, and use distilled water at a temperature of 50°C-60°C again for the filter cake Washing until the specific resistance of the washing liquid is greater than 200Ω / cm, t...

Embodiment 2

[0028] Take by weighing 5 grams of carrier (γ-Al 2 o 3 ), it was impregnated into 20 (mass)% ammonium molybdate solution, impregnated at a constant temperature of 60°C for 6h, then dried at 120°C for 12h, and then roasted for 6h in an air atmosphere and at 400°C to obtain the target catalyst (abbreviated It is catalyst A): wherein the content of metal molybdenum and / or its oxide is 8 (mass)%, and the balance is carrier (γ-Al 2 o 3 ).

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Abstract

The invention relates to a method for preparing polyoxymethylene dimethylethers (with a molecular formula of CH3O(CH2O)Xch3, 3<=x<=4) form methanol and formaldehyde, comprising the following steps that: in exist of a catalyst, methanol is reacted with formaldehyde formaldehyde to obtain the polyoxymethylene dimethylethers. The method is characterized in that: the catalyst is a supported catalyst, wherein an active component of the supported catalyst comprises: metallic molybdenum and / or its oxide, metallic iron and / or its oxide, and / or metallic niobium and / or its oxide, and a carrier of the supported catalyst is gamma-Al2O3; and, the supported catalyst, with a total weight being 100%, contains 0.1-35% by weight of metallic molybdenum and / or its oxide, 0-10% by weight of metallic iron and / or its oxide, 0-15% by weight of metallic niobium and / or its oxide, and the balance being the carrier. By the method, the selectivity of polyoxymethylene dimethylethers can be raised 10-30%.

Description

technical field [0001] The invention relates to a method for preparing polyoxymethylene dimethyl ethers (Polyoxymethylene Dimethyl Ethers, PODE for short), in particular to a method for preparing polyoxymethylene dimethyl ethers by reacting methanol and formaldehyde. Background technique [0002] Polyoxymethylene dimethyl ether (PODE) is an oil additive with an average cetane number (CN) value of 76 and a high oxygen content. PODE can increase the calorific value of diesel and reduce exhaust emissions. Therefore, the preparation of PODE has attracted the attention of scientists. [0003] So far, a variety of methods for preparing PODE have been reported (such as US 2008 / 0221368A1, US. Pat. No. 6,166,266, US. Pat. No. 6,160,174 and US. Pat. No. 6,265,528 B1, etc.). In the prior art, when referring to making PODE by the reaction of methanol and formaldehyde, the catalyst used is an acidic catalyst, which leads to products (especially PODE n＞2 ) selectivity is not ideal, the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/30C07C41/56B01J23/887B01J23/28B01J23/881
CPCB01J23/002B01J23/28B01J23/881B01J23/8877B01J2523/00C07C41/56C07C43/30B01J2523/68B01J2523/842B01J2523/56B01J2523/31
Inventor 刘殿华房鼎业罗万明刘宏伟王军峰李铖张荣赵光施敏浩
Owner EAST CHINA UNIV OF SCI & TECH
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