Process for producing 1,6-hexanediol and coproducing epsilon-caprolactone

A technology of hexanediol and caprolactone, which is applied in the field of adipate esterification hydrogenation preparation 1, can solve the problems of difficult separation of products and catalysts, high energy consumption for product separation and purification, and a large amount of acidic wastewater, so as to save separation energy consumption, save equipment investment, and shorten the production process

Active Publication Date: 2012-02-15
SHANGHAI WUZHENG ENG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, the esterification reaction adopts a two-step method, through two processes of pre-esterification and continuous esterification, and the loading method of the catalyst in the continuous esterification process brings about a large bed pressure drop and uneven gas-liquid distribution.
Sulfuric acid in the pre-esterification process has a serious

Method used

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  • Process for producing 1,6-hexanediol and coproducing epsilon-caprolactone
  • Process for producing 1,6-hexanediol and coproducing epsilon-caprolactone
  • Process for producing 1,6-hexanediol and coproducing epsilon-caprolactone

Examples

Experimental program
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Effect test

Embodiment 1

[0046] In this example, refer to the attached figure 1 The apparatus and procedures shown set up the various reaction components.

[0047] In the reactive distillation column C (inner diameter 40mm, the pipe of height 4000mm), fill the filler of 50 theoretical plate heights, in the tower, filler particle average loading superacid active center 0.6% (weight ratio), filler particle average size is 5mm×5mm.

[0048] This filler is a self-made filler, first of all (NH4) 2 S 2 o 8 Immerse it on the nano-beta molecular sieve to make catalyst nano-scale powder (particle size is 68-80nm), adopt the mode of spraying or mechanical mixing, preferably mechanical mixing mode, and mix described catalyst nano-scale powder with ceramic mud and binder ( Hydroxypropyl methylcellulose and / or squash powder), dried, and roasted at 550°C for 4 hours, and its size is 3-5mm×3-5mm, preferably 5mm×5mm.

[0049] The adipic acid liquid passes through the first tray at the top of the reactive distill...

Embodiment 2

[0056] Adipic acid and methanol are continuously esterified in a reactive distillation tower, and the process flow is the same as in Example 1. The reaction pressure is normal pressure, the reaction temperature is 100-150°C, and the liquid hourly space velocity is 0.8Kg / Kg.h. The specific results are as follows:

[0057] Table 1

[0058]

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Abstract

The invention provides a process for preparing 1,6-hexanediol and coproducing epsilon-caprolactone through esterification and hydrogenation of adipic acid. The process comprises the following steps of: performing countercurrent contact of pure adipic acid and methanol steam on a catalyst active ingredient-loaded filler in a reaction catalytic distillation tower, and performing esterification reaction; and purifying dimethyl adipate, and performing hydrogenation purification to obtain the 1,6-hexanediol and coproduce epsilon-caprolactone, wherein polymer generated after product separation is subjected to ester exchange reaction to be recycled. The catalyst has high activity and selectivity, the products are high in yield, energy consumption is low, the equipment investment is small, the catalyst is environment-friendly, and the preparation process is simple, economic and practical.

Description

technical field [0001] The invention relates to a process for producing 1,6-hexanediol and co-producing ε-caprolactone, in particular to a process for preparing 1,6-hexanediol and co-producing ε through esterification and hydrogenation of adipic acid - Process of caprolactone. Background technique [0002] 1,6-Hexanediol is an important fine chemical raw material, widely used in polyurethane, polyester, coil coating, light curing, degradable plastics and other fields. [0003] ε-caprolactone is mainly used in the production of modified polyols and caprolactone acrylic monomers, and is also a strong solvent and a non-reactive solvent for storage and transportation. [0004] Patent CN1212681A discloses a method for preparing 1,6-hexanediol and ε-caprolactone from a carboxylic acid mixture containing adipic acid, 6-hydroxyacetic acid and a small amount of 1,4-cyclohexanediol. The carboxylic acid mixture is obtained from an oxidation reaction of cyclohexane with oxygen to prod...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/149C07C29/80C07D313/04
CPCY02P20/10Y02P20/584
Inventor 王保明李玉江王东辉徐长青
Owner SHANGHAI WUZHENG ENG TECH CO LTD
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