Preparation method of polymethoxy methylal

A technology of polymethoxymethylal and paraformaldehyde, applied in the preparation of organic compounds, chemical instruments and methods, molecular sieve catalysts, etc., can solve problems such as catalyst corrosion, improve coke capacity, increase utilization, The effect of increasing selectivity

Active Publication Date: 2014-01-29
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] CN101182367A and CN101962318A disclose the use of acidic ionic liquid as a catalyst, the method for preparing polyoxymethylene acetal by methanol and paraformaldehyde as raw materials, there is also the problem of serious corrosion of the catalyst
[0008] CN101665414A discloses

Method used

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  • Preparation method of polymethoxy methylal

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Mix 40% silica sol, sodium metaaluminate, tetrapropylammonium bromide TPABr, sodium chloride, sodium hydroxide and water, stir for 20 minutes, put it into a reaction kettle, and crystallize dynamically at 170°C (200 rpm). 3 days. 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 the original ZSM-5 molecular sieve powder. The molar ratio of each raw material in the reaction mixture is: SiO 2 / Al 2 o 3 =80.0,H 2 O / SiO 2 =50.8, NaCl / SiO 2 =0.68, NaOH / SiO 2 =0.15, TPABr / SiO 2 =0.40. The average grain diameter is 0.5 micron.

[0020] Get 50 grams of ZSM-5 molecular sieves (SiO 2 / Al 2 o 3 =80), put into 250 grams of concentration and be 0.5 mol / liter of sodium hydroxide aqueous solution, under reflux, stir at 80 ℃ of constant temperature for 0.5 hour, filter, wash with distilled water, then use the ammonium nitrate aqueous solution of 10% mass concentration in 80 Exchanged three...

Embodiment 2

[0024] Get 50 grams of grain diameter and be the ZSM-5 molecular sieve (SiO 2 / Al 2 o 3 =40), put 100 grams of concentration into an aqueous sodium hydroxide solution of 1 mol / liter, stir at a constant temperature of 60° C. for 3 hours under reflux, filter, wash with distilled water, exchange with [Example 1] ammonium, dry, roast , molding, to obtain catalyst B.

[0025] The performance evaluation of the catalyst was carried out on a 300ml autoclave reaction device. Add 1.5 grams of catalyst, 80 grams of dimethyl ether, and 100 grams of paraformaldehyde in the autoclave, react for 4 hours at 110 ° C and make the pressure 4 MPa by filling nitrogen, filter and separate the catalyst and the reaction product, and analyze by gas chromatography to obtain The composition of the mixture is shown in Table 1.

[0026]

Embodiment 3

[0028] Get 50 grams of ZSM-5 molecular sieves (SiO 2 / Al 2 o 3 =100), put 500 grams of concentration into the potassium hydroxide aqueous solution of 0.2 mol / liter, stir at a constant temperature of 50° C. for 3.5 hours under reflux, filter, wash with distilled water, exchange with [Example 1] ammonium, dry, roast , molding, to obtain catalyst C.

[0029] 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.

[0030]

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Abstract

The invention relates to a preparation method of polymethoxy methylal, 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 0.1-10MPa to obtain the polymethoxy methylal, wherein the catalyst is a ZSM-5 molecular sieve of which the crystal grain diameter is smaller than or equal to 5 micrometers, the ZSM-5 molecular sieve is treated in a 0.01-2 mol/L alkali solution at 30-100 DEG C for 0.1-10 hours, and the weight ratio of the alkali solution to the molecular sieve is 1-20. The technique scheme provided by the invention well solves the problem, and can be used for industrial production of polymethoxy methylal.

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, 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 can reach 30% (v / v), while maintaining a high ten Hexane number and combustion performance. It can improve t...

Claims

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Application Information

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IPC IPC(8): C07C43/30C07C41/56C08G2/08C08G2/10
CPCB01J29/40B01J2229/14B01J2229/38C07C41/56C07C43/30
Inventor 何欣袁志庆滕加伟
Owner CHINA PETROLEUM & CHEM CORP
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