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Process for preparing paraformaldehyde with methanol as raw material

A paraformaldehyde and preparation process technology, applied in the direction of organic chemistry, can solve the problems of difficult recycling, heavy recycling system load, and many by-products, and achieve the effects of improving atomic utilization, increasing manufacturing costs, and reducing intermediate products

Active Publication Date: 2021-06-01
CHINA CHEM TECH RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional paraformaldehyde synthesis process mainly has the following problems: the sulfuric acid catalyst severely corrodes the equipment, the product is difficult to separate from the catalyst, and the product separation is complicated; the continuous production stability of the formaldehyde synthesis and formaldehyde concentration unit is poor, it is difficult to run at full load, and the energy consumption is high; The conversion rate of the paraformaldehyde monomer reaction system is low, the load of the recovery system is large, the extraction effect is poor, the steam consumption is large, and the impurity content exceeds the standard
The current process generally adopts the method of crystallization or extraction to carry out preliminary separation of the synthetic product, plus the refining of rectification, but it is still unable to obtain paraformaldehyde with ultra-purity or close to 100% purity. At the same time, the extraction process introduces new solvents, resulting in The separation system is more complicated, resulting in energy consumption and dilute aldehyde recovery difficulties, and often requires a separate dilute aldehyde recovery unit for recovery
[0016] Second, in the existing and above-mentioned paraformaldehyde preparation process, there are difficulties of large amount of dilute aldehyde and high recovery energy consumption. For example, every ton of paraformaldehyde produced will produce about 4 tons of 15% dilute formaldehyde , producing 1 ton of paraformaldehyde consumes 7-8 tons of steam, and the steam used for dilute aldehyde recovery accounts for more than 70%
[0026] Therefore, in the synthesis process of paraformaldehyde, there are by-products such as methanol, formic acid and methyl formate, especially methanol and formaldehyde are very easy to form hemiacetal, and the separation is difficult. However, if methanol is not separated, it will cause methanol to accumulate in the system. Reduced production rate of paraformaldehyde
[0027] Fourth, when using the rectification method to recover dilute aldehyde, the continuous heating of the formaldehyde solution causes the disproportionation reaction (Cannizzaro) of formaldehyde to generate methanol and formic acid, and formic acid is extremely corrosive, causing corrosion of equipment, making The rectification tower for recovering dilute aldehyde cannot be used for a long time
[0028] In summary, the above-mentioned patented technologies are only optimized and improved from the aspects of catalyst, separation process and preparation process, and still cannot solve the long-term constraints on the production of dilute aldehyde, which have a large amount of dilute aldehyde recovery, many by-products, difficult recycling, high energy consumption, and equipment Key issues such as high material requirements

Method used

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  • Process for preparing paraformaldehyde with methanol as raw material
  • Process for preparing paraformaldehyde with methanol as raw material
  • Process for preparing paraformaldehyde with methanol as raw material

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Embodiment 1

[0075] A process for preparing paraformaldehyde using methanol as a raw material, using methanol and methanol and methylal produced in the recovery section as raw materials to prepare concentrated formaldehyde with a concentration of more than 50%; the concentrated formaldehyde is synthesized under the catalysis of solid acid and acid, The formaldehyde aqueous solution containing paraformaldehyde is purified by rectification and membrane coupling process, and impurities such as methanol, methyl formate, formaldehyde, water, and formaldehyde polymers are separated to obtain pure paraformaldehyde.

[0076] The dilute aldehyde mixture and by-product impurities in the production process are converted into methylal through reactive distillation, and recycled to the reactor in the high-concentration formaldehyde production section, and part of the water generated in the recovery section is recycled to the formaldehyde absorption unit.

[0077] Described technique specifically compris...

Embodiment 2

[0103] The preparation process is performed by the following: formaldehyde reactor R0101 and formaldehyde absorption tower T0101; paraformaldehyde synthesis reactor R0201, paraformaldehyde concentration tower T0201 and dealcoholization reaction rectification tower R0202; membrane dehydration unit M0301, light removal tower T0301 And weight removal tower T0302; dilute aldehyde recovery reaction distillation tower R0401 and paraformaldehyde recovery distillation tower R0402.

[0104] In the formaldehyde reactor R0101, methanol and methylal mixture (methanol 2 and recycle stream 16) are evaporated, mixed with air (material 1) with a mass flow rate of 1825Kg / h, under the action of iron molybdenum oxidation catalyst, at 280 ℃, formaldehyde is generated under normal pressure, and the permeate stream 7 absorbs formaldehyde in the formaldehyde absorption tower T0101 to obtain a concentrated formaldehyde aqueous solution stream 3 with a formaldehyde concentration of 56.98%.

[0105] In...

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Abstract

The present invention discloses a process for preparing paraformaldehyde by using methanol as a raw material, and preparing concentrated formaldehyde with a concentration of more than 50% through methanol and methanol and methylal produced by the catalytic conversion of the recycling section as raw materials; the concentrated formaldehyde is synthesized under the catalysis of solid acid Paraformaldehyde, the formaldehyde aqueous solution containing paraformaldehyde is purified by rectification and membrane coupling process, and impurities are separated to obtain pure paraformaldehyde. The disclosed process reduces the production of dilute aldehyde, reduces the energy consumption of separation, reduces the impurity content of paraformaldehyde, and circulates dilute aldehyde and by-products through catalytic conversion, improves the utilization rate of raw materials, and can realize the production of paraformaldehyde Long-term stable operation.

Description

technical field [0001] The invention provides a process for preparing paraformaldehyde by using methanol as a raw material, which belongs to the field of chemical production process. Background technique [0002] Polyoxymethylene (POM), also known as acetal resin and polyoxymethylene, is a thermoplastic engineering plastic with excellent comprehensive properties. It is one of the five major engineering plastics. "Super Steel" or "Sai Steel". The main key monomer for the production of polyoxymethylene is trioxane (TOX), a stable form of anhydrous formaldehyde polymer. Preparation of fine chemicals. [0003] The traditional synthesis method of paraformaldehyde is to use 50-65% concentrated formaldehyde as raw material to synthesize paraformaldehyde under the action of sulfuric acid catalyst. This reaction is a fast reversible reaction, but the reaction equilibrium constant is small, the conversion rate of formaldehyde is low, and only the paraformaldehyde whose equilibrium ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D323/06
CPCC07D323/06
Inventor 雷骞张小明陈洪林邓兆敬雷蔚鑫李克景
Owner CHINA CHEM TECH RES INST
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