Process of preparing dipentaerythritol and/or tripentaerythritol

A technology of dipentaerythritol and tripentaerythritol, which is applied in chemical instruments and methods, preparation of carboxylate, preparation of organic compounds, etc., can solve the problems of inability to meet quality and quantity requirements, difficulty of dipentaerythritol, high energy consumption, etc., and achieve simple separation Ease of operation, high product purity and high yield

Inactive Publication Date: 2007-08-08
PUYANG YONGAN CHEM IND
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  • Abstract
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AI Technical Summary

Problems solved by technology

The by-products of dipentaerythritol (Di-Pentae) and tripentaerythritol (Tri-Pentae) are mainly obtained by separating the mixture generated during the production of pentaerythritol (Pentae), but due to polydipentaerythritol, polytripentaerythritol and acetals The existence of impurities such as lead to the separation of high-purity dipentaerythritol (Di-Pentae) and tripentaerythritol (Tri-Pentae) is very difficult, and the energy consumption is too high, the yield also only has less than 5%, and the purity is relatively low, only 50% -70% and 30-40%, unable to meet the increasing quality and quantity demand for dipentaerythritol (Di-Pentae) and tripentaerythritol (Tri-Pentae)

Method used

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  • Process of preparing dipentaerythritol and/or tripentaerythritol
  • Process of preparing dipentaerythritol and/or tripentaerythritol
  • Process of preparing dipentaerythritol and/or tripentaerythritol

Examples

Experimental program
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Embodiment 1

[0039] Step 1: Take 10 mol of formaldehyde with a concentration (mass concentration) of 18%, 1 mol of acetaldehyde with a concentration of 50%, and 1.2 mol of a calcium hydroxide solution with a concentration of 5% and add them to an atmospheric chemical reaction kettle with a stirrer Stirring is carried out, the temperature is controlled at 15°C, and the reaction time is controlled at 4 hours. Firstly, pentaerythritol (Pentae) is generated through condensation and Toulon reaction, and the main component of pentaerythritol (Pentae) is di-pentaerythritol (Di-Pentae) through etherification and disproportionation reactions. And the condensation liquid of tripentaerythritol (Tri-Pentae), generate simultaneously by-product and impurity mainly be the acetals of pentaerythritol (Pentae), calcium formate, methyl alcohol.

[0040] Step 2: Rectification adopts double towers to remove methanol, formaldehyde and part of water. The dealcoholization tower uses a packed tower equivalent to 1...

Embodiment 2

[0047] Step 1: get concentration (mass concentration) to be 2.5mol of formaldehyde of 25%, get the concentration of acetaldehyde 1mol of 90%, get concentration of calcium hydroxide (Ca(OH) 2 ) solution 1.2mol, formaldehyde and acetaldehyde as the bottom water, the calcium hydroxide solution is added in batches into a reactor with a pressure of 0.1mpa for stirring, the temperature is controlled at 40 ° C, and the reaction time is controlled at In 90 minutes, at first, pentaerythritol (Pentae) was generated through condensation and Toulon reaction, and pentaerythritol (Pentae) was generated through etherification and disproportionation reactions into condensation liquids whose main components were dipentaerythritol (Di-Pentae) and tripentaerythritol (Tri-Pentae). The by-products and impurities are mainly pentaerythritol (Pentae) acetals, calcium formate, and methanol.

[0048] Step 2: Rectification: Use double towers to remove methanol, formaldehyde and part of water: use a pack...

Embodiment 3

[0055] Get concentration (mass concentration) to be 37% formaldehyde 6.5mol, get concentration to be 99% acetaldehyde 1.2mol, get concentration to be 40% calcium hydroxide solution 1.2mol, formaldehyde and acetaldehyde make bottom water, calcium hydroxide The feeding method of adding the solution in batches is added to a 0.1mpa pressure reactor with a stirrer for stirring, the temperature is controlled at 70°C, and the reaction time is controlled at 30 minutes. First, pentaerythritol (Pentae) is generated through condensation and Toulon reaction. Pentaerythritol (Pentae) undergoes etherification and disproportionation reactions to generate a condensation liquid whose main components are dipentaerythritol (Di-Pentae) and tripentaerythritol (Tri-Pentae). Calcium, Methanol.

[0056] Step 2: Rectification: Use double towers to remove methanol, formaldehyde and part of water. The dealcoholization tower uses a packed tower equivalent to 10 trays, and the temperature is controlled a...

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Abstract

The invention discloses a manufacturing technique of dipentaerythritol and/or tripentaerythritol, which comprises the following steps: 1. condensing acetaldehyde, formaldehyde and calcium hydroxide solution with molar rate at 2.0-15.2:1:0.3-1.9 under 15-70 deg.c for 0.5-4h; 2. removing aldehyde in the condensing reacting liquid; 3. evaporating condensing reacting liquid; dehydrating; 4. crystallizing calcium formate; centrifuging; drying; 5. controlling the temperature at 80-150 deg.c; blending with active charcoal for 0.1-10h to make the mother liquid of Di-Pentae, Tri-Pentae and Pentae; 6. transmitting upper suspension in the mother liquid into 30-80 order screen to separate; entering into the processing procedure of dipentaerythritol and tripentaerythritol; centrifuging to hydrate for lower crystal liquid; washing to obtain the semiproduct of pentaerythritol.

Description

technical field [0001] The present invention relates to the production technology of dipentaerythritol and / or tripentaerythritol, especially by formaldehyde and acetaldehyde in alkaline calcium hydroxide (Ca(OH) 2 ) solution to prepare high-purity dipentaerythritol and / or tripentaerythritol production process. Background technique [0002] Di-Pentaerythritol (Di-Pentaerythrito1) is a solid tetrahydric alcohol, its structural formula is as follows:. [0003] [0004] (Dipentaerythritol) [0005] High-purity dipentaerythritol (DTMP) is mainly used in light curing agents, coatings, resins and special inks, as well as PVC stabilizers and synthetic greases. With the rapid development of coating resins, inks and PVC stabilizers, the demand in the international market continues to increase. At present, the supply of dipentaerythritol products is in short supply, and the market prospect is very broad. [0006] Tripentaerythritol (Tri-Pentaerythrito1) is a solid hexahydric alco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/01C07C43/10C07C29/38C07C31/24C07C51/41C07C53/06
Inventor 王永军
Owner PUYANG YONGAN CHEM IND
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