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Production technology of bi-tribydroxy methyl propane and/or trihydroxy methyl propane methylal

A technology of trimethylolpropane formal and ditrimethylolpropane, which is applied in the field of producing high-purity ditrimethylolpropane and trimethylolpropane formal, can solve low, only 80- 90%, high energy consumption, and yield less than 2%, to achieve the effect of simple separation, low energy consumption, and high yield

Inactive Publication Date: 2008-07-09
朗盛(溧阳)多元醇有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The by-product of ditrimethylolpropane (DTMP) is mainly obtained by separating the mixture formed by the reaction in the production process of trimethylolpropane (TMP), but because tripolytrimethylolpropane (TTMP) and acetal substances The existence of impurities makes it very difficult to separate and obtain high-purity ditrimethylolpropane (DTMP), and the energy consumption is too high, the yield is only less than 2%, and the purity is relatively low, only 80-90%, which cannot meet the increasing Growing demand for ditrimethylolpropane (DTMP) and trimethylolpropane formal (CTF)

Method used

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  • Production technology of bi-tribydroxy methyl propane and/or trihydroxy methyl propane methylal
  • Production technology of bi-tribydroxy methyl propane and/or trihydroxy methyl propane methylal
  • Production technology of bi-tribydroxy methyl propane and/or trihydroxy methyl propane methylal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Step 1: Take 15 mol of formaldehyde with a mass percentage concentration of 10%, 1 mol of n-butyraldehyde with a mass percentage concentration of 85%, and 0.8 mol of NaOH solution with a mass percentage concentration of 55% and add it to an atmospheric chemical reaction kettle with a stirrer The temperature is controlled at 35°C, and the reaction time is controlled at 7 hours. First, trimethylolpropane is generated through Toulon reaction and Connizzaro reaction, and then trimethylolpropane is converted into the main component through etherification and disproportionation. It is the condensation liquid of ditrimethylolpropane and trimethylolpropane methylal, and simultaneously generates by-products and impurities such as trimeric trimethylolpropane and acetal substances, sodium formate, light fractions, Bis-TMP, etc.

[0042] Step 2: Evaporation and dehydration. A two-effect evaporation process is used to remove water from the condensation liquid obtained in step 1, the...

Embodiment 3

[0047] Step 1: get 9 mol of formaldehyde with a mass percentage concentration of 50%, 1 mol of n-butyraldehyde with a mass percentage concentration of 85%, 0.5 mol of potassium hydroxide (KOH) solution with a mass percentage concentration of 85%, formaldehyde, potassium hydroxide The solution is used as the bottom water, and the feeding method of n-butyraldehyde is continuously added into a 0.4mpa pressure reactor with a stirrer for stirring. The temperature is controlled at 20°C, and the reaction time is controlled at 5 hours. The Zara reaction produces trimethylolpropane, and then trimethylolpropane undergoes etherification and disproportionation reactions to generate a condensation liquid whose main components are ditrimethylolpropane and trimethylolpropane formal, while generating by-products and impurities Such as trimeric trimethylolpropane and acetal substances, potassium formate, light fractions, Bis-TMP, etc.

[0048] Step 2: Evaporation and dehydration. A 4-effect e...

Embodiment 4

[0053] Step 1: getting mass percentage concentration is 70% formaldehyde 6mol, getting mass percentage concentration is 50% n-butyraldehyde 1mol, getting mass percentage concentration is 10% sodium carbonate (Na 2 CO 3 ) solution 1.8mol, sodium carbonate solution, n-butyraldehyde as bottom water, formaldehyde is added in batches into a reactor with a pressure of 0.3mpa for stirring, the temperature is controlled at 50°C, and the reaction time is controlled at 3 Hours, first through the Toulon reaction and Connizzaro reaction to generate trimethylolpropane, and then trimethylolpropane undergoes etherification and disproportionation reactions to generate ditrimethylolpropane and trimethylolpropane as the main components Aldehyde condensation liquid, while generating by-products and impurities such as trimeric trimethylolpropane and acetals, sodium formate, light fractions, Bis-TMP, etc.

[0054] Step 2: Evaporation and dehydration. A 5-effect evaporation process is used to rem...

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Abstract

The present invention discloses ditrimethylolpropane and / or trimethylolpropane methylal producing process. Butyl aldehyde, formaldehyde and alkaline water solution are added into reactor to produce Turonian reaction, Connizaros reaction, etherification and disproportionation so as to produce condensated liquid containing ditrimethylolpropane, trimethylolpropane methylal and trimethylolpropane mainly. The condensated liquid is then evaporated to eliminate water, extracted, rectified and purified to obtain the target product. The production process of the present invention has low power consumption, high yield, and simple and feasible separation.

Description

Technical field [0001] The present invention relates to the production process of ditrimethylolpropane and trimethylolpropane formal, especially the high-yield production of high-purity ditrimethylolpropane through the reaction of formaldehyde and n-butyraldehyde in an alkaline solvent And the production process of trimethylolpropane methylal. Background technique [0002] Ditrimethylolpropane (DTMP) is a solid tetraol with the following structural formula. Trimethylolpropane formal (CTF) is a liquid monocyclic monohydric alcohol, and its structural formula is as follows. High-purity ditrimethylolpropane (DTMP) and high-purity trimethylolpropane formal (CTF) are mainly used in light curing agents, coatings, resins and special inks, as well as PVC stabilizers and synthetic greases. [0003] [0004] Ditrimethylolpropane [0005] [0006] Trimethylolpropane formal [0007] Generally, in the process of preparing trimethylolpropane (TMP) from formaldehyde and n-butyral...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/13C07C41/09C07D319/06
Inventor 王强刘武平
Owner 朗盛(溧阳)多元醇有限公司