Liquid phase hydrogenation method for residual liquids of butanol and octanol

A liquid-phase hydrogenation and raffinate technology, which is applied in the field of catalysis, can solve the problems of complex treatment process and low utilization rate of butanol-octanol raffinate, and achieve the effects of simplifying the process flow, improving the utilization rate and simplifying the preparation process.

Active Publication Date: 2014-02-05
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In order to solve the problems of low utilization rate and complicated treatment process of butanol raffinate in the prior art, the method adopts the combined process of obtaining butanol and octanol by first liquid-phase hydrogenating the butanol raffinate and then rectifying separation, and the raw materials do not need to be pre-processed. The process is simple; the hydrogenation unit uses a catalyst with Ni and Zn as the acti...

Method used

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  • Liquid phase hydrogenation method for residual liquids of butanol and octanol
  • Liquid phase hydrogenation method for residual liquids of butanol and octanol

Examples

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Embodiment 1

[0029] 98.5g of nickel nitrate and 91.3g of zinc nitrate were dissolved in 2L of deionized water, and 60g of SiO 2 Add the powder to the above solution and stir for 15 minutes, then add 1.2mol / L sodium carbonate aqueous solution to the above solution for co-precipitation, the pH value of the mixed solution after precipitation is 7, control the precipitation temperature to about 40°C, stir and age for 1 hour, then filter and Wash until neutral, dry at 120°C for 8 hours, calcinate at 500°C for 3 hours, and then press into tablets to obtain the catalyst precursor. The catalyst precursor was loaded into a 20mL fixed-bed reactor, and the catalyst sample 1 was obtained by reducing it with hydrogen for 2 hours under the conditions of a pressure of 1.0MPa, a temperature of 500°C, and a volume ratio of hydrogen to catalyst of 200:1.

[0030] After mixing the butanol raffinate and hydrogen, it enters the hydrogenation reactor from the top in liquid phase, and the catalyst of the present...

Embodiment 2

[0032] 147.8g of nickel nitrate and 68.5g of zinc nitrate were dissolved in 2L of deionized water, and 55g of SiO 2 Add the powder to the above solution and stir for 15 minutes, then add 1.2 mol / L potassium carbonate aqueous solution to the above solution for co-precipitation, the pH of the mixed solution after precipitation is 8, control the precipitation temperature to about 50°C, stir and age for 2 hours, then filter and Wash until neutral, dry at 110°C for 10 hours, calcinate at 450°C for 4 hours, and then press into tablets to obtain a catalyst precursor. The catalyst precursor was loaded into a 20mL fixed-bed reactor, and the catalyst sample 2 was obtained by hydrogen reduction under the conditions of pressure 2.0MPa, temperature 450°C, hydrogen gas and catalyst volume ratio 300:1.

Embodiment 3

[0034] 197g of nickel nitrate and 45.7g of zinc nitrate were dissolved in 2L of deionized water, and 50g of SiO 2 Add the powder to the above solution and stir for 15 minutes, then add 1.2mol / L ammonium bicarbonate aqueous solution to the above solution for co-precipitation, the pH of the mixed solution after precipitation is 7, control the precipitation temperature to about 60°C, and filter after stirring for 3 hours and washed until neutral, dried at 100°C for 12 hours, calcined at 400°C for 5 hours, and then pressed into tablets to obtain a catalyst precursor. The catalyst precursor was loaded into a 20mL fixed-bed reactor, and was reduced with hydrogen for 4h under the conditions of pressure 3.0MPa, temperature 400°C, and volume ratio of hydrogen to catalyst 400:1 to obtain catalyst sample 3.

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Abstract

The invention discloses a liquid phase hydrogenation method for residual liquids of butanol and octanol. The liquid phase hydrogenation method is characterized by comprising the steps of firstly, carrying out fixed bed liquid catalytic hydrogenation reaction on the residual liquids of butanol and octanol, and then, rectifying and separating to obtain butanol and octanol, wherein a rectifying unit comprises a dehydrating tower, a butanol tower and an octanol tower. A catalyst for the hydrogenation reaction is composed of a carrier and active components, wherein the carrier is one of silicon dioxide and silica sol, the active components include Ni and Zn, Ni accounts for 10-50wt% of the total mass of the catalyst, and Zn accounts for 5-30wt% of the total mass of the catalyst; the catalyst is prepared by using a co-precipitation method. The catalyst used in the method is simple in component and preparation, the residual liquids of butanol and octanol are simple in treatment process and high in utilization ratio, and the purity of a product is high.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a method for liquid-phase hydrogenation of butanol raffinate. technical background [0002] Butanol and octanol (referred to as butanol) are mainly used in the production of plasticizers dioctyl phthalate (DOP) and dibutyl phthalate (DBP). With the development of my country's plastics industry, the market demand for octyl alcohol is increasing year by year, and the production capacity of octyl alcohol in China is also increasing year by year. There is a small amount of discharge from the evaporator, phase separator, and weight removal tower of the reactor of the butanol plant, and the discharged mixed liquid is called the butanol raffinate, which is equivalent to about 10% of the product quality of butanol, and It contains a lot of valuable components, but due to its complex composition, it was mostly used as fuel in the past. The domestic existing devices for rec...

Claims

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Application Information

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IPC IPC(8): C07C31/12C07C31/125C07C29/92B01J23/80
CPCB01J23/80C07C29/92C07C31/12C07C31/125
Inventor 于海斌李孝国孙国方高鹏费亚南赵甲肖寒耿姗李佳舒畅郑修新刘有鹏
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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