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Production process and device of high-purity methylal

A production process, methylal technology, applied in the field of high-purity methylal synthesis process and equipment, can solve the problems of affecting the quality of methylal products, increasing the difficulty of wastewater treatment, equipment investment and equipment occupying a large area, etc., to achieve The effect of product quality improvement, easy handling, and small investment in equipment

Active Publication Date: 2020-06-05
四川纬邦亿科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. It is still necessary to set up a pre-reactor, and the equipment investment and equipment occupy a large area; 2. The purity of the methylal obtained, although in this patent document, The purity data is not disclosed, however, the inventor of the present application used the method to prepare methylal during the test process, and the obtained methylal had a purity of 98.21% and a methanol content of 1.73%, and there is still room for further improvement in its purity In addition, the methylal of gained, its moisture content is 0.06%, and its moisture content is higher, influences the quality of methylal product, in addition, formaldehyde content 3.3% in the waste water at the bottom of the reaction distillation tower, methanol content 0.19%, Increased the difficulty of wastewater treatment

Method used

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  • Production process and device of high-purity methylal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] see figure 1 , a high-purity methylal production device, comprising a formaldehyde tank 1, a methanol tank 2, a raw material mixer 3 and a reactive distillation tower 5, a first pump 91 is set between the formaldehyde tank 1 and the raw material mixer 3, and the methanol tank 2 A second pump 92 is set between the raw material mixer 3, and a shell-and-tube heat exchanger 4 is set between the raw material mixer 3 and the reactive distillation tower 5, and the heat exchanger 4 is connected to the middle of the reactive distillation tower 5 , the lower part of the reactive distillation tower 5 is provided with a catalyst layer 51, and the top of the reactive distillation tower 5 is connected to the first condenser 71, the first reflux tank 81 and the pressurized rectification tower 6 in sequence, and also includes a second reflux tank 82, a fourth pump 94 is arranged between the first reflux tank 81 and the pressurized rectification tower 6, the fourth pump 94 is connected ...

Embodiment 2

[0038] (1) The methanol and formaldehyde solutions are respectively pumped into the raw material mixer 3 through the first pump 91 and the second pump 92 for mixing, then pass through the shell-and-tube heat exchanger 4, and then enter the reactive distillation tower 5 for reaction, wherein the raw material methanol The concentration is 99.5%, the formaldehyde concentration is 31.2%, the top temperature of the reactive distillation column is 36.5°C, the bottom temperature is 99.4°C, and the reflux ratio is 1.8 times the minimum reflux ratio. After the reaction, an azeotropic mixture of methylal and methanol is obtained. The composition of the azeotropic mixture is: 88.93% of methylal, 11.03% of methanol, and 0.04% of water; the composition of waste water at the bottom of the reactive distillation tower is: no methanol, 0.04% of formaldehyde; the catalyst layer 51 in the reactive distillation tower 5 It is a strongly acidic cation exchange resin, and the strong acidic cation exc...

Embodiment 3

[0041] (1) The methanol and formaldehyde solutions are respectively pumped into the raw material mixer 3 through the first pump 91 and the second pump 92 for mixing, then pass through the shell-and-tube heat exchanger 4, and then enter the reactive distillation tower 5 for reaction, wherein the raw material methanol The concentration is 99.5%, the formaldehyde concentration is 56.5%, the top temperature of the reactive distillation column is 43.5°C, the bottom temperature is 99.4°C, and the reflux ratio is 1.6 times the minimum reflux ratio. After the reaction, an azeotropic mixture of methylal and methanol is obtained. The composition of the azeotropic mixture is: methylal 91.82%, methanol 8.16%, water 0.02%; the waste water at the bottom of the reactive distillation tower is composed of: no methanol and 0.02% formaldehyde; the catalyst layer 51 in the reactive distillation tower 5 It is a strongly acidic cation exchange resin, and the strong acidic cation exchange resin is mo...

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Abstract

The invention discloses a production process of high-purity methylal, which belongs to the technical field of methylal production, and comprises the following steps: mixing methanol and a formaldehydesolution, feeding the mixed solution in a reactive distillation tower for a reaction to obtain an azeotropic mixture of methylal and methanol, wherein a catalyst in the reactive distillation tower isstrongly acidic cation exchange resin, and the resin is modularly mounted in the reactive distillation tower, separating the azeotropic mixture by a pressurized distillation tower, condensing a separated product at the bottom of the pressurized distillation tower to obtain a product, wherein a mixture of methylal and methanol is obtained at the top of the pressurized distillation tower, and feeding one part of the mixture into a catalyst layer at the lower part of the reactive distillation tower for a reaction. According to the process, the double towers of the reactive distillation tower andthe pressurized distillation tower are adopted, the quality of the obtained product is high, the purity of the product methylal is greater than 99.9%, the moisture content is less than 0.03%, the quality of the product is obviously improved, wastewater is easy to treat, the production energy consumption is reduced, and the equipment investment is small.

Description

technical field [0001] The invention relates to the technical field of methylal production, in particular to a synthesis process and device for high-purity methylal. Background technique [0002] Methylal is obtained by condensation reaction of methanol and formaldehyde solution as raw materials, and then purified by rectification. It is widely used in cosmetics, pharmaceuticals, industrial automotive supplies, insecticides, leather polishes, cleaning agents, and rubber industries. , paints, inks and other products. [0003] For the production process of methylal, there have been many reports in the prior art. Because the methylal obtained after the reaction of methanol and formaldehyde contains impurities such as methanol and formaldehyde, the existing methods generally adopt the addition of various alcohols and their derivatives for extraction, rectification and purification. Although these methods can greatly improve the formaldehyde The purity of acetal, for example, c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/56C07C41/58C07C43/30
CPCC07C41/56C07C41/58C07C43/30Y02P20/10
Inventor 田永宏蔡昌庚
Owner 四川纬邦亿科技有限公司
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