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Preparation method of polyoxy methylene dimethyl ether

A technology of polyoxymethylene dimethyl ether and dimethyl ether, which is applied in the field of preparation of polyoxymethylene dimethyl ether, can solve problems such as catalyst corrosion, achieve improved activity and stability, and high crystallinity Internal diffusion rate, reducing the effect of depth reactions

Active Publication Date: 2014-01-29
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 dimethyl ether is provided

Method used

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  • Preparation method of polyoxy methylene dimethyl ether
  • Preparation method of polyoxy methylene dimethyl ether
  • Preparation method of polyoxy methylene dimethyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Mix 40% silica sol, sodium metaaluminate, tetrabutylammonium bromide, sodium chloride, sodium hydroxide and water, stir for 20 minutes, put into a reaction kettle, and crystallize at 170°C for 1 day. The crystallized product was quenched, filtered, and washed with water until the pH value was 8, and dried at 120°C for 12 hours to obtain the original powder of ZSM-11 molecular sieve. The XRD spectrum is shown in figure 1 , SEM photo see figure 2 , the grain diameter is 0.5 microns. The molar ratio of each raw material in the reaction mixture is: SiO 2 / Al 2 o 3 =149.3,H 2 O / SiO 2 =32.8, NaCl / SiO 2 =0.6, NaOH / SiO 2 =0.08, TBABr / SiO 2 =0.12.

[0028] The synthesized ZSM-11 molecular sieve raw powder was treated with 0.3 mol / L nitric acid at 80°C for 4 hours for 3 consecutive times to obtain HZSM-11.

[0029] Mix HZSM-11 with boehmite, Tianqing powder, and 0.3 mol / liter nitric acid, and the weight ratio of each raw material is ZSM-11 / Al 2 o 3 / Tianqing powder = ...

Embodiment 2

[0033] Mix 40% silica sol, sodium metaaluminate, tetrabutylammonium bromide, sodium chloride, sodium hydroxide and water, stir for 20 minutes, put into a reaction kettle, and crystallize at 170°C for 1 day. The crystallized product was quenched, filtered, washed with water until the pH value was 8, and dried at 120°C for 12 hours to obtain ZSM-11 molecular sieve raw powder with a grain diameter of 0.5 microns. The molar ratio of each raw material in the reaction mixture is: SiO 2 / Al 2 o 3 =149.3,H 2 O / SiO 2 =32.8, NaCl / SiO 2 =0.6, NaOH / SiO 2 =0.08, TBABr / SiO 2 =0.12.

[0034] The synthesized ZSM-11 molecular sieve raw powder was treated with 0.3 mol / L hydrochloric acid at 80°C for 4 hours for 3 consecutive times to obtain HZSM-11.

[0035] Mix HZSM-11 with boehmite, Tianqing powder, and 0.3 mol / liter nitric acid, and the weight ratio of each raw material is HZSM-11 / Al 2 o 3 / Tianqing powder = 1:1:0.1, extruded into strips, dried at 120°C for 12 hours, roasted at 55...

Embodiment 3

[0039] According to the steps and conditions of [Example 2], only SiO in the synthetic formula 2 / Al 2 o 3 =52, tetrabutylammonium hydroxide was used as template agent, crystallized at 120° C. for 8 days, and the crystal grain diameter of the synthesized ZSM-11 molecular sieve raw powder was 1 micron. Exchange with 1.0 mol / L citric acid at 80°C for 10 hours. Get a catalyst.

[0040] The performance evaluation of the catalyst was carried out on a 300ml autoclave reaction device. Add 1.2 grams of catalyst, 50 grams of methanol, 50 grams of dimethyl ether, and 100 grams of paraformaldehyde in the autoclave, and react for 5 hours at 100 ° C and a pressure of 1 MPa by filling nitrogen, and filter and separate the catalyst and the reaction product. Chromatographic analysis, the composition of the obtained mixture is shown in Table 1.

[0041]

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Abstract

The invention relates to a preparation method of polyoxy methylene dimethyl ether, which mainly solves the problem of corrosiveness of the catalyst in the prior art. The method comprises the following step: contacting raw materials methanol or dimethyl ether and formaldehyde or trioxymethylene in a mol ratio of 1:(0.1-10) with a catalyst to react at the reaction temperature of 50-200 DEG C under the reaction pressure of 0.1-10 MPa to generate the polyoxy methylene dimethyl ether. The catalyst comprises the following components in parts by weight: a) 40-95 parts of ZSM-11 molecular sieve of which the silicon / aluminum (SiO2 / Al2O3) mol ratio is 20-300 and the crystal grain diameter is at most 5 micrometers, and b) 5-60 parts of adhesive. The ZSM-11 molecular sieve is subjected to acid washing at least once. The technical scheme provided by the invention well solves the problem, and can be used for industrial production of the polyoxy methylene dimethyl ether.

Description

technical field [0001] The invention relates to a preparation method of polyoxymethylene dimethyl ether. Background technique [0002] Polyoxymethylene dimethyl ether (Chinese name can also be polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ether, polyoxymethylene acetal, polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ether base 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 can reach 30% (v / v), while maintaining a high ten Hexane number and combustion performance. It can improve the lubricity of diesel,...

Claims

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Application Information

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IPC IPC(8): C07C43/30C07C41/56B01J29/40C08G2/08C08G2/10
CPCB01J29/40B01J2229/14B01J2229/37C07C41/56C07C43/30
Inventor 何欣袁志庆滕加伟
Owner CHINA PETROLEUM & CHEM CORP
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