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A kind of method of gas-phase hydrogenation of dimethyl adipate to produce 1,6-hexanediol

A technology of dimethyl adipate and hexanediol, applied in chemical instruments and methods, preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of reducing reaction temperature and reaction pressure, There are many side reactions and high reaction temperature, so as to achieve the effect of reducing acid value and chromaticity, stable product quality and low reaction temperature

Active Publication Date: 2019-12-03
WEIFANG YUANLI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) The reaction conditions are relatively high and the reaction pressure is high;
[0006] (2) low conversion rate; low yield;
[0008] (4) High temperature and high energy consumption;
[0009] (5) Long reaction time;
[0010] (6) The content of 1,6-hexanediol produced is low, the product quality is unstable, and the acid value and chroma are not good;
[0011] (7) Many side effects
[0012] The reaction temperature for the preparation of 1,6-hexanediol in the prior art is high, the energy consumption is high, the reaction pressure is high, the requirements for the reaction equipment are high, and the production cost is high. The prior art has always wanted to reduce the reaction temperature and reaction pressure , but the reaction temperature and reaction pressure are reduced at the same time, the quality of the prepared 1,6-hexanediol is not good, the acid value of the product is higher, and the color is darker, which cannot meet the downstream application of 1,6-hexanediol

Method used

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  • A kind of method of gas-phase hydrogenation of dimethyl adipate to produce 1,6-hexanediol
  • A kind of method of gas-phase hydrogenation of dimethyl adipate to produce 1,6-hexanediol

Examples

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Effect test

Embodiment 1

[0050] Embodiment 1 A kind of method of gas-phase hydrogenation of dimethyl adipate to produce 1,6-hexanediol

[0051] Include the following steps:

[0052] (1) Preparation of catalyst

[0053] Include the following steps:

[0054] mix

[0055] Prepare an ethanol solution with an Au content of 0.02wt% chloroauric acid; prepare an ethanol solution with a Pt content of 0.01wt% chloroplatinic acid, mix the ethanol solution of chloroauric acid with the ethanol solution of chloroplatinic acid in a mass ratio of 4:1 Mixed solution A is obtained, so that the mass ratio of gold: platinum is 8:1;

[0056] Add protectant and reducer

[0057] Then add polyvinylpyrrolidone (PVP) with a concentration of 1wt% in the above mixed solution A as a protective agent, and then add a concentration of 0.1wt% paraformaldehyde, wherein the mass ratio of Au: polyvinylpyrrolidone: paraformaldehyde is 1: 1:0.7, stirred at a speed of 500 rpm for 15 minutes, and the reaction temperature was 25°C, to obt...

Embodiment 2

[0069] Embodiment 2 A kind of method of gas-phase hydrogenation of dimethyl adipate to produce 1,6-hexanediol

[0070] Include the following steps:

[0071] (1) Preparation of catalyst

[0072] The catalyst was prepared by the preparation method of Example 1.

[0073] (2) Activation of the catalyst

[0074] Add the catalyst to a 100-liter vibrating mill, the addition amount is 17% (volume ratio), adjust the vibration frequency to 3700rmp, fill the vibrating mill with 42L of grinding media with a diameter of 2 mm and a length of 12 mm, vibrate for 8 minutes, and take out the catalyst Afterwards, heat up to 120°C and dry for 4.5h under nitrogen, and activate in the mixed flow of nitrogen and hydrogen (the volume flow ratio of nitrogen and hydrogen is 2:3), first at 110°C, pressure 1.2MPa, activate for 2.7h, and then Raise the temperature to 160°C at a rate of 2.5°C / min, and activate for 7 hours at 160°C and a pressure of 4MPa.

[0075] (3) Vaporization of dimethyl adipate

...

Embodiment 3

[0081] Embodiment 3 A kind of method of gas-phase hydrogenation of dimethyl adipate to produce 1,6-hexanediol

[0082] Include the following steps:

[0083] (1) Preparation of catalyst

[0084] The catalyst was prepared by the preparation method of Example 1.

[0085] (2) Activation of the catalyst

[0086] Add the catalyst to a 100-liter vibrating mill, the addition amount is 18% (volume ratio), adjust the vibration frequency to 4000rmp, fill the vibrating mill with 43L of grinding media with a diameter of 2 mm and a length of 12 mm, vibrate for 10 minutes, and take out the catalyst Afterwards, heat up to 130°C and dry for 5 hours under nitrogen, activate in a mixed flow of nitrogen and hydrogen (the volume flow ratio of nitrogen and hydrogen is 2:3), first activate at 120°C and pressure 1.5MPa for 2 hours, and then activate with 2 The temperature was raised to 170°C at a rate of °C / min, and activated for 8 hours at 170°C and a pressure of 6 MPa.

[0087] (3) Vaporization...

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Abstract

The invention provides a method for producing 1,6-hexanediol by virtue of gas hydrogenation of dimethyl adipate. The method comprises the steps of preparing a catalyst, activating the catalyst, vaporizing dimethyl adipate, and performing the hydrogenation reaction. The method is low in reaction pressure, and the hydrogenation reaction pressure is 2.5 to 5 MPa; a conversation rate is 99.5 to 99.99 percent; a yield is 99 to 99.5 percent; the content of the generated 1,6-hexanediol is high, and the product quality is stable; and a coarse product can reach the following indexes: an acid value is less than or equal to 0.06mgKOH / g, a color number is less than or equal to No. 11, a water content is less than or equal to 0.1 percent, and a content of hexanediol is greater than or equal to 99.2 percent; and a final product can reach the following indexes: the acid value is less than or equal to 0.03 mgKOH / g, the color number is less than or equal to No. 8, the water content is less than or equal to 0.05 percent, and the content of hexanediol is greater than or equal to 99.8 percent.

Description

technical field [0001] The invention relates to a method for preparing 1,6-hexanediol by hydrogenation of dimethyl adipate, in particular to a method for producing 1,6-hexanediol by gas-phase hydrogenation of dimethyl adipate, belonging to the chemical industry The field of synthetic technology. Background technique [0002] 1,6-hexanediol is an important chemical intermediate with a wide range of uses, mainly used in the production of saturated / unsaturated polyester resins, oil-free alkyd resins, polyester polyols and esters used in synthetic lubricants, Polyurethane foam and elastomer plasticizers, additives for advanced lubricants and other fine chemicals. 1,6-Hexanediol is an excellent solvent for the selective separation of aromatics and cycloalkyl hydrocarbons. 1,6-hexanediol derivatives are widely used in the fields of automobile, textile, medicine, paint, pesticide, plastic and petroleum. At present, a few companies such as BASF Corporation, GFS Chemical Corporati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/149C07C31/20B01J23/52
CPCB01J23/52C07C29/149C07C31/20
Inventor 刘修华秦国栋王坤杨德虎张玉菡
Owner WEIFANG YUANLI CHEM