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Process of synthesizing trihydroxy methyl propane acetal

A technology of trimethylolpropane and formal, which is applied in the direction of organic chemistry, can solve problems such as unfavorable product yield, poor reaction effect, and reduced economy, and achieve process simplification, increase production efficiency, and reduce energy consumption Effect

Inactive Publication Date: 2009-08-19
CNPC JILIN CHEM GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the heavier condensate recovered by this method will continue to react with formaldehyde under the reaction conditions to form a condensation product with a higher boiling point that is not easy to be reprocessed. During the recovery process, the reaction effect will gradually become worse, which is unfavorable for the synthesis of CTF. The progress of the process will adversely affect the product yield and reduce the economics of the method

Method used

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  • Process of synthesizing trihydroxy methyl propane acetal
  • Process of synthesizing trihydroxy methyl propane acetal
  • Process of synthesizing trihydroxy methyl propane acetal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 201g of trimethylolpropane and 48g of paraformaldehyde into the reaction distillation device, then pass in nitrogen gas by bubbling and dispersing at the bottom and raise the temperature to 125°C, add 2g of sodium bisulfate, and carry out the aldehyde reaction under normal pressure. Water is discharged from the reaction system from the top of the tower. When no reaction water is discharged from the top of the tower, it is reacted for 3 hours at an absolute pressure of 2.67KPa and a reaction temperature of 145°C. Evaporated and dried. Based on the added amount of trimethylolpropane, the CTF yield is 96.4%.

Embodiment 2

[0032] According to the same procedure of embodiment 1, except adding 0.02g sodium bisulfate, all the other conditions remain unchanged. Based on the added amount of trimethylolpropane, the CTF yield is 91.5%.

Embodiment 3

[0034] According to the same procedure of embodiment 1, except adding 8g sodium bisulfate, all the other conditions remain unchanged. Based on the added amount of trimethylolpropane, the CTF yield is 94.1%.

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Abstract

The invention discloses a method for synthesizing trimethylolpropane monocyclic formal by acetal reaction of trimethylolpropane and paraformaldehyde (solid formaldehyde, paraformaldehyde) with a low degree of polymerization in the presence of an acidic catalyst. Firstly, add trimethylolpropane and paraformaldehyde into the reaction distillation device, carry out atmospheric compression aldehyde reaction at a reaction temperature of 90-145°C and under the action of an acidic catalyst, until no reaction water is discharged from the top of the tower, and then in the reaction The acid hydrolysis reaction is carried out at a temperature of 125-185° C. and negative pressure, and at the same time, the trimethylolpropane monocyclic formal is distilled from the top of the tower and dried to obtain a trimethylolpropane monocyclic formal product. The process route of the method is simple, the reaction temperature is controllable, the conversion rate and selectivity of reactants are high, the product yield is high, and industrial production is easy.

Description

technical field [0001] The invention relates to a method for synthesizing trimethylolpropane monocyclic formal, in particular to a method for preparing trimethylolpropane monocyclic formal with trimethylolpropane and paraformaldehyde as raw materials in the presence of an acidic catalyst . Background technique [0002] The chemical name of trimethylolpropane monocyclic formal (hereinafter referred to as CTF) is 5-ethyl-5-hydroxymethyl-1,3-dioxane, which is a colorless liquid monocyclic with a pungent odor. Cyclic alcohols. As a high value-added deep-processing product of trimethylolpropane, it can be used to produce ester compounds such as monocyclic acetal acrylate and monocyclic acetal methacrylate. These ester compounds are mainly used as thinners for UV curable coatings , CTF is also used in the production of acetal copolymers, which can be used as automotive parts, plumbing parts, and everyday products. [0003] On the basis of the traditional production process of t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D319/06
Inventor 刘乃青徐鸿王硕
Owner CNPC JILIN CHEM GROUP CORP
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