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Method for preparing isooctyl alcohol by catalyzing and condensing butanol

A technology of catalytic condensation and n-butanol, which is applied in the preparation of hydroxyl compounds, organic compounds, chemical instruments and methods, etc., can solve the problems of polluted waste water, high catalyst cost, harsh process conditions, etc., and achieve low cost and easy operation The effect of convenience and simple process

Inactive Publication Date: 2012-12-05
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, high pressure and noble metal catalysts are required in the hydroformylation reaction, the process conditions are harsh, and the catalyst cost is high; on the other hand, in the reaction system, olefins and toxic carbon monoxide are required as raw materials, and a large amount of alkali-containing wastewater ( Li Xiangfu et al., CN101353213A(2009))
It can be seen that the process not only relies on petroleum resources, but also has a large amount of polluted wastewater

Method used

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  • Method for preparing isooctyl alcohol by catalyzing and condensing butanol
  • Method for preparing isooctyl alcohol by catalyzing and condensing butanol
  • Method for preparing isooctyl alcohol by catalyzing and condensing butanol

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preparation example Construction

[0031] 1-1. Preparation of carrier hydroxyapatite

[0032] According to the required Ca / P ratio, prepare calcium nitrate and diammonium hydrogen phosphate into 0.1-2.0 mol / L aqueous solution, adjust pH=10-13 with concentrated ammonia water, heat and reflux for 1-2 hours, and precipitate overnight. Granular hydroxyapatite is obtained by suction filtration, shaping, drying, and burning at 500-700°C for 5-6 hours.

[0033] 1-2. Preparation of metal-supported catalyst

[0034] Dissolve nickel nitrate or nickel acetate or palladium chloride in water to make a solution with a concentration of 0.02 to 1.0 mol / L, then weigh 15 grams of the granular hydroxyapatite carrier prepared in the above (1-1) and pour it into the solution In, impregnated at room temperature for 2 to 4 days, evaporated to dryness, and then dried at 130°C.

[0035] 1-3. Addition of cocatalyst

[0036] The addition of the cocatalyst is to make magnesium nitrate, potassium carbonate or potassium fluoride into an ...

Embodiment 1

[0044] Preparation of hydroxyapatite carrier: Weigh 39.5g calcium nitrate and dissolve it in 200mL deionized water, add concentrated ammonia water to adjust pH=11 to obtain calcium nitrate solution;

[0045] Weigh 13.2g of diammonium hydrogen phosphate and dissolve it in 150mL of deionized water, add concentrated ammonia water to adjust the pH=11, then drop the solution into the above calcium nitrate solution, heat to reflux for 1 hour, stop stirring, and let stand overnight;

[0046] washing, filtering, forming, drying at 130°C, and burning at 500°C for 5 hours to obtain granular hydroxyapatite carrier.

[0047] Preparation of the supported catalyst: Weigh 3.06 g of nickel nitrate and dissolve it in 60 mL of water. After it is completely dissolved, add 15 g of granular hydroxyapatite carrier. After soaking for 3 days, the solution is evaporated to dryness, and then dried overnight at 130° C. to obtain the supported catalyst.

[0048] Put 15g of the catalyst into a tubular rea...

Embodiment 2

[0050] Preparation of hydroxyapatite carrier: Weigh 39.5g calcium nitrate and dissolve it in 200mL deionized water, add concentrated ammonia water to adjust pH=13 to obtain calcium nitrate solution;

[0051] Weigh 13.2g of diammonium hydrogen phosphate and dissolve it in 150mL of deionized water, add concentrated ammonia water to adjust the pH=13, then drop the solution into the above calcium nitrate solution, heat to reflux for 1 hour, stop stirring, and let stand overnight;

[0052] washing, filtering, forming, drying at 130°C, and burning at 500°C for 5 hours to obtain granular hydroxyapatite carrier.

[0053] Weigh 3.06g of nickel nitrate and dissolve it in 60mL of water. After completely dissolving, add 15g of granular hydroxyapatite carrier. After soaking for 3 days, the solution is evaporated to dryness, and then dried overnight at 130°C. Then weigh 1.6g of magnesium nitrate and dissolve it in 60mL of water. After completely dissolving, impregnate the above-mentioned dr...

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Abstract

The invention discloses a method for preparing isooctyl alcohol by catalyzing and condensing butanol. In a continuous flowing reaction system, butanol is catalyzed and condensed to prepare isooctyl alcohol through a tubular fixed bed reactor at one step. The catalyst is of a load-type catalyst by adopting hydroxyapatite as a carrier to load active components such as nickel, palladium and the likeand by adding magnesia, potassium carbonate or potassium fluoride as an assistant catalyst. The catalyst is filled into a tubular fixed bed reactor, after being introduced with hydrogen and treated for 3 to 5 hours at the temperature of 350 to 450 DEG C, the temperature is cooled to the reaction temperature, the hydrogen introduction is stopped, butanol of 5 to 15 mL / hr is directly pumped into a preheating section of the reactor to be evaporated and to be condensed by a catalyst layer to prepare the isooctyl alcohol. The method has simple flow process, convenient catalyst preparation and low cost; and moreover, the selectivity of the isooctyl alcohol in the product is more than 73 percent, and the once-through conversion rate of the butanol reaches 52 percent.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a method for preparing isooctyl alcohol by catalytic condensation of n-butanol. Background technique [0002] Isooctyl alcohol (2-ethylhexanol, 2-EH) is an important fine chemical raw material with a wide range of uses and can be used as a raw material for the production of plasticizers (dioctyl phthalate, dioctyl adipate) , can also be used as an additive for diesel oil and lubricating oil, as a solvent in papermaking, paint and textile industries, as a glaze dispersant in the ceramic industry, etc. The production process of isooctyl alcohol mainly includes oxo synthesis method and acetaldehyde condensation method. Hydroformylation reaction (i.e. oxo synthesis) is the mainstream production process for synthesizing isooctyl alcohol, such as using propylene and synthesis gas (carbon monoxide and hydrogen) as raw materials, and synthesizing n-butanol by hydroformylation reacti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/125C07C29/34B01J27/185
Inventor 杜志强叶平平姜玄珍
Owner ZHEJIANG UNIV