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A method and device system for producing 1,2-hexanediol

A technology of hexanediol, -II is applied in the field of hydrolysis reaction to prepare 1,2-hexanediol, which can solve the problems of low product yield and the like, and achieve the effects of simple process technology, improving conversion rate, and breaking the limit of hydrolysis balance.

Active Publication Date: 2021-08-31
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the product after alkaline hydrolysis needs to undergo unit operations such as neutralization, extraction, drying, and rectification to obtain the product, resulting in low product yield and high-salt wastewater containing sodium formate

Method used

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  • A method and device system for producing 1,2-hexanediol
  • A method and device system for producing 1,2-hexanediol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The feed flow rate of 1,2-hexanediol dicarboxylate and water mixed liquid is 1000kg / h, and the feed molar composition: 1.2-hexanediol dicarboxylate:water=1:2. Send the mixed solution into the pre-reactor for pre-reaction, the residence time is 120min, and the pre-reaction temperature is 95°C. The theoretical board numbers of tower section-I, tower section-II and tower section-III are 20, 10 and 10 respectively. The residence time of reactor I and reactor II is 45min, and the temperature of the reactor is controlled to be 110°C. Tower section-I has a top pressure of 15kpa and a reflux ratio of 4. 145kg / h of supplementary water is fed to the bottom of the reactor II, 594.5kg / h of water and formic acid are produced at the top of the tower, and 564.3kg / h of crude 1,2-hexanediol is produced at the bottom of the tower. According to the material balance calculation, the single-pass hydrolysis rate of 1,2-hexanediol dicarboxylate is 99.1%. The crude product can obtain 99.5% ...

Embodiment 2

[0051] The feed flow rate of 1,2-hexanediol dicarboxylate and water mixture is 1000kg / h, 25°C, and the feed molar composition: 1.2-hexanediol dicarboxylate:water=1:4. Send the mixed liquid into the pre-reactor for pre-reaction, the pre-reaction temperature is 95°C, and the residence time is 60min. The number of theoretical boards of Tower Section-I, Tower Section-II and Tower Section-III are 24, 10 and 10 respectively. The residence time of reactor I and reactor II is 60min, and the temperature of the controlled reactor is 100°C. Tower section-I has a top pressure of 20kpa and a reflux ratio of 2. 148kg / h of supplementary water is fed to the bottom of the reactor II, 650.9kg / h of water and formic acid are produced at the top of the tower, and 481.3kg / h of crude 1,2-hexanediol is produced at the bottom of the tower. According to the material balance calculation, the single-pass hydrolysis rate of 1,2-hexanediol dicarboxylate is 99.3%. The crude product can obtain 469kg / h of ...

Embodiment 3

[0053] The feed flow rate of 1,2-hexanediol monoformate and water mixed liquid is 1000kg / h, 25°C, and the feed molar composition: 1.2-hexanediol monoformate: water = 1:2. Send the mixed liquid into the pre-reactor for pre-reaction, the pre-reaction temperature is 95°C, and the residence time is 100min. The number of theoretical boards of Tower Section-I, Tower Section-II and Tower Section-III are 24, 10 and 10 respectively. The residence time of reactor I and reactor II is 50min, and the temperature of the controlled reactor is 105°C. Tower Section-I has a top pressure of 15kpa and a reflux ratio of 3. 198kg / h of supplementary water is fed to the bottom of the reactor II, 540.6kg / h of water and formic acid are produced at the top of the tower, and 649.7kg / h of crude 1,2-hexanediol is produced at the bottom of the tower. According to the material balance calculation, the single-pass hydrolysis rate of 1,2-hexanediol dicarboxylate is 99.1%. The crude product can obtain 99.5% ...

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Abstract

The invention belongs to the technical field of organic synthesis application, in particular to a method and device for producing 1,2-hexanediol. Using 1,2-hexanediol dicarboxylate or 1,2-hexanediol monoformate as raw material, water and 1,2-hexanediol dicarboxylate (or, 2-hexanediol monoformate Formic esters) are mixed in proportion and sent to a pre-reactor equipped with an acidic resin catalyst for partial hydrolysis, and the pre-reaction liquid is then sent to a column device coupled with reaction and rectification to achieve complete hydrolysis. The aqueous solution containing formic acid is extracted from the top of the tower device, and the crude product of 1,2-hexanediol is obtained from the bottom tower kettle. The present invention has mild reaction conditions, simple process, and is easy for industrial continuous production. The single-pass hydrolysis rate of 1,2-hexanediol di(mono)formate is higher than 99%, and 1,2-hexanediol di(mono)formate can be obtained with a purity higher than 99.5% after simple purification. 2‑Hexanediol products.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis application, and specifically relates to a method for preparing 1,2-hexanediol dicarboxylate or 1,2-hexanediol monoformate through hydrolysis reaction. diol method. Background technique [0002] 1,2-hexanediol, also known as DL-1,2-hexanediol or DL-1,2-hexanediol, is a colorless, transparent liquid with a pungent odor, soluble in water, It can also be mixed with various organic compounds in any proportion. 1,2-Hexanediol is widely used in the ink of color inkjet printers and synthetic raw materials in the pharmaceutical industry. Adding 1,2-hexanediol in cosmetics can play antiseptic, sterilizing, moisturizing and other functions, but has no side effects on human health, so it is an important raw material for the synthesis of advanced cosmetics. In addition, 1,2-hexanediol can also be used as an intermediate in organic synthesis for the manufacture of downstream products such as 1,2-h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/20C07C29/09C07C29/80
CPCC07C29/095C07C29/80C07C2531/08C07C31/20
Inventor 黄智贤李明明杨臣王清莲王晓达邱挺王红星
Owner FUZHOU UNIV
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