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Polyformaldehyde dimethyl ether preparation method

A technology of polyoxymethylene dimethyl ether and silica sol, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as catalyst corrosion, eliminate the influence of diffusion, smooth channels, and large effective surface area Effect

Active Publication Date: 2015-06-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] CN101182367A and CN101962318A disclose the method for preparing polyoxymethylene dimethyl ether by using acidic ionic liquid as a catalyst and using methanol and paraformaldehyde as raw materials, but there is also the problem of serious corrosion of the catalyst
[0008] CN101665414A discloses a method for preparing polyoxymethylene dimethyl ether using acidic ionic liquid as a catalyst and using methylal and paraformaldehyde as raw materials, which also has the problem of serious corrosion of the catalyst
[0009] In summary, the catalysts used in the prior art have the disadvantage of being corrosive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 7.4 grams of silica sol (SiO 2 weight content 40%), then add sodium metaaluminate, 40% aqueous sodium hydroxide solution, so that the molar ratio is: 6 Na 2 O: Al 2 o 3 : 80 SiO 2 , and add water to mix, knead and extrude. After that, it was dried at 100° C. for 1 hour, and then pelletized. A mixture of 2 grams of tetrapropylammonium bromide and 10 grams of distilled water was added in advance in the reaction kettle, a stainless steel mesh was placed above the mixture, the formed molecular sieve was placed on the stainless steel mesh, and the reaction kettle was sealed. The reactor was subjected to gas-solid phase treatment at 150°C for 4 days. After the product was taken out, it was washed with water, dried at 120°C for 10 hours, and then baked at 550°C for 5 hours to remove the template agent. For the XRD characterization results of the sample, see figure 1 . Afterwards, the obtained material was exchanged three times with 10% by weight ammonium nitrate a...

Embodiment 2

[0030] Weigh 7.4 grams of silica sol (SiO 2 weight content 40%), then add sodium metaaluminate, 40% aqueous sodium hydroxide solution, so that the molar ratio is: 8 Na 2 O: Al 2 o 3 : 100 SiO 2 , and add water to mix, knead and extrude. Thereafter, it was dried at 120° C. for 1 hour, and then pelletized. Add a mixture of 2 grams of tetrapropylammonium hydroxide and 10 grams of distilled water in advance in the reaction kettle, place a stainless steel mesh above the mixture, place the formed molecular sieve on the stainless steel mesh, and seal the reaction kettle. The reactor was subjected to gas-solid phase treatment at 170°C for 3 days. After the product was taken out, it was washed with water, dried at 120°C for 10 hours, and then baked at 550°C for 5 hours to remove the template. Afterwards, the obtained material was exchanged three times with 10% by weight ammonium nitrate aqueous solution at 80°C, washed twice with water, dried at 120°C for 10 hours, and calcined a...

Embodiment 3

[0033] Weigh 7.4 grams of silica sol (SiO 2 weight content 40%), then add sodium metaaluminate, 40% aqueous sodium hydroxide solution, so that the molar ratio is: 3.5 Na 2 O: Al 2 o 3 : 60 SiO 2 , and add water to mix, knead and extrude. After that, it was dried at 120° C. for 2 hours and cut into pellets. A mixture of 6 g of ethylenediamine and 10 g of distilled water was preliminarily added to the reaction kettle, a stainless steel mesh was placed above the mixture, the formed molecular sieve was placed on the stainless steel mesh, and the reaction kettle was sealed. The reactor was subjected to gas-solid phase treatment at 180°C for 2 days. After the product was taken out, it was washed with water, dried at 120°C for 10 hours, and then baked at 550°C for 5 hours to remove the template. Afterwards, the obtained material was exchanged three times with 10% by weight ammonium nitrate aqueous solution at 80°C, washed twice with water, dried at 120°C for 10 hours, and calci...

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Abstract

The present invention relates to a polyformaldehyde dimethyl ether preparation method, wherein the problem that the catalyst has corrosion in the prior art is mainly solved with the present invention. The technical scheme comprises that: methanol or dimethyl ether, and formaldehyde or trioxymethylene are adopted as raw materials, a molar ratio of the methanol or the dimethyl ether to the formaldehyde or the trioxymethylene is 1:0.1-10, and the reaction raw materials contact a catalyst at a reaction temperature of 50-200 DEG C under a reaction pressure of 0.1-10 MPa to produce polyformaldehyde dimethyl ether, wherein the catalyst is at least the one selected from a binder-free ZSM-5 molecular sieve and a binder-free ZSM-11 molecular sieve. With the technical scheme, the problem in the prior is well solved, and the method can be used for industrial production of polyformaldehyde dimethyl ether.

Description

technical field [0001] The invention relates to a method for preparing polyoxymethylene dimethyl ether. Background technique [0002] Polyoxymethylene dimethyl ether (Chinese name can also be polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ether Ether, polyoxymethylene dimethyl ether, etc.), that is, polyoxymethylene dimethyl ethers (PODE), which is a general term for a class of substances, and its molecular structure is CH 3 O(CH 2 O) n CH 3 , with higher cetane number (cetane number, CN. When n=3~8, CN>76) and oxygen content (42~49%). When the value of n is 3 to 8, its physical and chemical properties and combustion performance are very close to those of diesel, and it can be used as a diesel additive. The amount added to diesel...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/30C07C41/50C07C41/56
Inventor 何欣袁志庆滕加伟陈康成陶伟川
Owner CHINA PETROLEUM & CHEM CORP
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