Preparation method of polyoxymethylene dimethyl ether (DMMn)

The technology of polymethoxydimethyl ether and polyoxymethylene is applied in the field of preparation of polymethoxydimethyl ether (DMMn, generally n=3-8), which can solve problems such as unfavorable industrialization, blockage of transmission pipelines, influence and the like, To achieve the effect of good catalytic effect, low cost and high yield

Pending Publication Date: 2021-03-30
SHANDONG CHENXIN NEW ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Other conventional methods for preparing anhydrous gaseous formaldehyde also include: 1. Depolymerize paraformaldehyde by heating to prepare gaseous formaldehyde, but the bound water of paraformaldehyde itself is only about 4%, which greatly affects the yield and intermediate rate of DMMn synthesis. The further recycling of the product not only makes the preparation of solid polyoxymethylene more cumbersome, but also the further feeding and transportation are not conducive to large-scale and continuous large-scale production, and there are great safety hazards
2. Under the action of an acidic catalyst, paraformaldehyde is heated and decomposed and gasified. In this way, there will be paraformaldehyde that is too late to decompose and gasify with gaseous formaldehyde, which is easy to cause pipeline blockage, and the cost of paraformaldehyde is high, which is not conducive to Realize industrialization

Method used

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  • Preparation method of polyoxymethylene dimethyl ether (DMMn)
  • Preparation method of polyoxymethylene dimethyl ether (DMMn)
  • Preparation method of polyoxymethylene dimethyl ether (DMMn)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1: After mixing 400g of formaldehyde aqueous solution (37%) and 60g of ethylene glycol, vacuumize and heat to remove moisture to obtain 193.2g of anhydrous flowing polyoxymethylene, and then gradually heat the anhydrous flowing polyoxymethylene to 160 ℃, formaldehyde is gradually gasified to form gaseous formaldehyde, and then dry anhydrous gaseous formaldehyde is passed into a mixture of 10g catalyst and 280g methylal, and a catalytic reaction occurs at a certain temperature. After the reaction reaches equilibrium, the catalyst is filtered out to obtain Reaction equilibrium liquid 356.7g, residual ethylene glycol 91.7g (a total loss of 24.8g), and then the reaction equilibrium liquid 356.7g were subjected to normal pressure and vacuum distillation respectively, and 250.8g of low boilers, 15.5g of macromolecules and DMMn finished product were separated 72.4g (loss of 18.0g), DMMn finished product is then subjected to vacuum distillation to obtain each single comp...

Embodiment 2

[0028] Example 2: After mixing 400g of formaldehyde aqueous solution (37%) and 91g of ethylene glycol recovered from the previous batch, vacuumize and heat to remove moisture, and obtain 222.5g of anhydrous mobile polyoxymethylene, and then anhydrous mobile polyoxymethylene After gradually heating to 160°C, the formaldehyde is gradually gasified to form gaseous formaldehyde, and then the dry anhydrous gaseous formaldehyde is passed into a mixture of 10g catalyst and 280g methylal, and a catalytic reaction occurs at a certain temperature. After the reaction reaches equilibrium, The catalyst was filtered out to obtain 384.7g of reaction equilibrium liquid and 93.5g of residual ethylene glycol (a total loss of 24.3g), and then 384.7g of reaction equilibrium liquid were subjected to normal pressure and reduced pressure distillation respectively, and 264.0g of low boilers and macromolecular 22.9g and DMMn finished product 77.3g (loss 20.5g), the DMMn finished product is subjected to...

Embodiment 3

[0029] Example 3: After mixing 400g of formaldehyde aqueous solution (37%) and 93.5g of ethylene glycol recovered from the previous batch, vacuumize and heat to remove moisture to obtain 226.7g of anhydrous mobile polyoxymethylene, anhydrous mobile polyoxymethylene After gradually heating to 160°C, the formaldehyde is gradually gasified to form gaseous formaldehyde, and then the dry and anhydrous gaseous formaldehyde is passed into a room containing 10g of catalyst, 264.0g of recovered low boiling matter, 22.9g of macromolecules and 196g of methylal. In the mixture, a catalytic reaction occurs at a certain temperature. After the reaction reaches equilibrium, the catalyst is filtered out to obtain 593.6 g of reaction equilibrium liquid and 90.0 g of residual ethylene glycol (a total loss of 26 g). and vacuum distillation to separate out 397.3g of low boilers, 35.5g of macromolecules and 128.8g of finished DMMn (loss of 32.0g). The finished DMMn is then subjected to vacuum distil...

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Abstract

The invention belongs to the technical field of energy and chemical industry, and provides a preparation method of a fuel additive and an environment-friendly solvent polyoxymethylene dimethyl ether (DMMNn, generally n=3-8), which comprises the following steps: mixing a formaldehyde water solution and polyol according to a certain proportion, and conducting heating and dehydrating under vacuum conditions to obtain flowing polyoxymethylene with lower moisture content in one step; heating and gasifying flowing polyformaldehyde with the lower moisture content to obtain purer gaseous formaldehyde,mixing the obtained gaseous formaldehyde with methylal, mechanically used last-batch low-boiling-point substances, macromolecules and the like in the presence of a catalyst, carrying out catalytic reaction at a certain temperature, filtering out the catalyst after the reaction is balanced, purifying the synthetic liquid, respectively carrying out atmospheric pressure and reduced pressure distillation, conducting separating to obtain a low-boiling-point substance, macromolecules and a DMMn finished product, and carrying out reduced pressure distillation on the DMMn finished product to obtain each single component; and after the formaldehyde is gasified, returning the residual polyhydric alcohol for application of next-batch concentrating of formaldehyde to prepare the flowing polyformaldehyde with lower moisture content.

Description

technical field [0001] The invention belongs to the technical field of energy and chemical engineering, in particular, a preparation method of polymethoxydimethyl ether (DMMn, generally n=3-8) is designed. Background technique [0002] Polyoxymethylene dimethyl ether, also known as paraformaldehyde dimethyl ether, English name: Polyoxymethylene dimethylethers, referred to as PODE or DMMn, is a kind of low molecular weight with dimethoxymethane as the matrix and methyleneoxy as the main chain. Acetal polymer, its general formula is expressed as: CH3O(CH2O)nCH3. Among them, polyoxymethylene dimethyl ether with a degree of polymerization of 3-8, referred to as DMM3-8, is used to clean diesel blending components. Its physical properties are similar to diesel oil, and it is not necessary to modify the vehicle engine fuel supply system when blending it into diesel oil. . Its cetane number is as high as 76, its oxygen content is 47%~50%, and it has no sulfur and no aromatics. Ble...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/56C07C41/58C07C43/30C07C41/50C07C45/51C07C47/04
CPCC07C41/56C07C41/58C07C41/50C07C45/513
Inventor 蔡依进王兴路蔡依超郑吉振孙华李文强陈海龙徐胜凯张月凤
Owner SHANDONG CHENXIN NEW ENERGY
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