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Preparation method of polymethoxy acetal

A technology of polymethoxymethylacetal and trioxymethylene, applied in chemical instruments and methods, preparation of organic compounds, molecular sieve catalysts, etc., can solve problems such as catalyst corrosion, achieve simple separation, high reaction conversion rate and Product yield and low energy consumption

Active Publication Date: 2013-05-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem to be solved by the present invention is that there is a problem that the catalyst is corrosive in the prior art, and a new preparation method of polyoxymethylene acetal is provided

Method used

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  • Preparation method of polymethoxy acetal
  • Preparation method of polymethoxy acetal
  • Preparation method of polymethoxy acetal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] By 1SiO 2 : 0.01Al 2 o 3 : 0.41TEAOH: 0.31 acetylacetone: 31.76H 2 O Weigh each material, dissolve sodium aluminate in distilled water, add tetraethylammonium hydroxide dropwise, stir for 1 hour, then add ethyl orthosilicate dropwise, stir for 1 hour, then add acetylacetone, stir for 1 hour , adjusted to pH = 13.0 with 0.1N sodium hydroxide solution, and continued to stir for 5 hours. The resulting mixture was crystallized under hydrothermal conditions at 170°C for 4 days, washed, filtered and dried. The XRD spectrum of the obtained product is shown in figure 2 In curve 1, the relative intensity of (020), (040), (060) and (080) peaks in the diffraction spectrum is significantly increased, which shows that the synthesized product grows preferentially in the (010) direction (b-axis).

[0025] The synthesized raw ZSM-5 zeolite powder was treated with 0.8 mol / L acetic acid at 70°C for 5 hours for 4 consecutive times, wherein the weight ratio of the acid solution to the...

Embodiment 2

[0028] By 1SiO 2 : 0.01Al 2 o 3 : 0.25TPAOH : 0.05 sodium oxalate : 32.0H 2 O Weigh each material, dissolve sodium aluminate in distilled water, add tetrapropylammonium hydroxide dropwise, stir for 1 hour, then add silica sol dropwise, stir for 1 hour, then add sodium oxalate, stir for 1 hour, use 0.1 N sodium hydroxide solution was used to adjust the pH to 12.0, and stirring was continued for another 5 hours. The resulting mixture was crystallized under hydrothermal conditions at 200°C for 3 days, washed, filtered and dried. XRD spectrum see figure 2 In curve 2, the relative intensity of (020), (040), (060) and (080) peaks in the diffraction spectrum is significantly increased, which shows that the synthesized product grows preferentially in the (010) direction (b-axis). The synthesized raw ZSM-5 zeolite powder was treated with 0.8 mol / L acetic acid at 70°C for 5 hours for 4 consecutive times, wherein the weight ratio of the acid solution to the ZSM-5 zeolite was 9 to obt...

Embodiment 3

[0031] By 1SiO 2 : 0.02Al 2 o 3 : 0.23TEAOH: 0.278-hydroxyquinoline: 44.64H 2 O Weigh each material, dissolve aluminum triethoxide in distilled water, add tetraethylammonium hydroxide dropwise, stir for 1 hour, then add silica sol dropwise, stir for 1 hour, then add 8-hydroxyquinoline, stir for 1 hour , adjust pH=11.0 with 0.1N sodium hydroxide solution, and continue stirring for 5 hours. The resulting mixture was crystallized under hydrothermal conditions at 150°C for 6 days, washed, filtered and dried. XRD spectrum see figure 2 In curve 3, the relative intensity of (020), (040), (060) and (080) peaks in the diffraction spectrum is significantly increased, which shows that the synthesized product grows preferentially in the (010) direction (b-axis). The synthesized raw ZSM-5 zeolite powder was treated with 0.8 mol / L acetic acid at 80°C for 5 hours for 3 consecutive times, wherein the weight ratio of the acid solution to the ZSM-5 zeolite was 8 to obtain HZSM-5.

[0032...

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Abstract

The invention relates to a preparation method of polymethoxy acetal and mainly solves the problem that the existing catalyst is corrosive in the prior art. The method includes: mixing silicon source, aluminum source, template agent R1 and template agent R2 with water, and using inorganic base to adjust reaction mixture pH to 8-14; and subjecting the mixture to hydrothermal crystallization at 100-250 DEG C for 1-10 days; wherein the mole ratio of the reaction mixture is Al2O3 / SiO2=0.003-0.05, R1 / SiO2=0.1-2, H2O / SiO2=10-100, R2 / SiO2=0.05-2, the template agent R1 is one of tetramethyl ammonium hydroxide, tetraethyl ammonium hydroxide, tetrapropyl ammonium hydroxide or tetrabutyl ammonium hydroxide, R2 is one of beta-diketone, beta-diketone salt, oxalic acid, oxalate, catechol or 8-hydroxyquinoline. The problem that the existing catalyst is corrosive is solved. The method is applicable to industrial production of polymethoxy acetal.

Description

technical field [0001] The invention relates to a preparation method of polymethoxy formal. Background technique [0002] Polyoxymethylene dimethyl ether (Chinese name can also be polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ether, etc.), that is, polyoxymethylene dimethyl ethers ( PODE), it is a general term for a class of substances, 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 oil, and it can be used as a diesel oil additive. The amount added to diesel oil can reach 30% (v / v), while maintaining a high ten Hexane number and combustion performance. It can improve the lubricity of diesel, reduce the generation of combustion smoke, improve the combustion status of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/303C07C41/56B01J29/40
Inventor 何欣刘志成高焕新
Owner CHINA PETROLEUM & CHEM CORP