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Method for recycling waste liquid from butanol device

A waste liquid and butanol technology, applied in chemical instruments and methods, preparation of organic compounds, separation/purification of hydroxyl compounds, etc., can solve the problem of inability to ensure long-term stable operation of the device, unfavorable recovery of valuable components, and use of catalysts Short service life and other problems, to achieve the effect of ensuring long-term stable operation, realizing gas phase recycling, and prolonging service life

Active Publication Date: 2021-12-03
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method is not suitable for the butanol production unit waste liquid that the present invention proposes, and reason mainly has three points: one, in the butanol waste liquid, ester content is higher, and ester material is under conventional hydrogenation catalyst and catalytic condition It is difficult to convert, and the experimental data of this patent does not reflect the conversion data of esters; second, the hydrogenation conditions in this method are relatively harsh, requiring a hydrogenation temperature above 230°C, and a large amount of aldehydes in the butanol waste liquid are relatively high Condensation and cyclization will occur at high temperature to produce trioxane polymers, which is not only unfavorable for the recovery of valuable components, but also affects the quality of recovered products; third, under the conditions of this scheme, the service life of the catalyst is short and cannot Ensure long-term stable operation of the device

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] [Preparation Example 1] Preparation of Catalyst A

[0046] Add 3kg of deionized water into the reaction kettle, add 11.7g of nano-titanium dioxide with a particle size of 20-30nm, and stir evenly.

[0047] Dissolve 270.2g of anhydrous copper nitrate, 631.2g of aluminum nitrate nonahydrate, and 65.8g of zinc nitrate hexahydrate in 2.5kg of deionized water to form a mixed metal solution; prepare a sufficient amount of 20% sodium carbonate solution in addition; and sodium carbonate solution were heated to 80°C, and were added dropwise to the reactor for co-precipitation reaction. The temperature of the reactor was controlled at 80°C to keep the temperature constant. 6. After 1.5h, the metal mixed solution was added dropwise. Adjust the pH of the system to 9 with the above sodium carbonate solution, and age for 3 hours.

[0048] Then filter, wash and dry the filter cake at 120°C for 24h, and roast at 600°C for 5h, break the roasted filter cake into strips, and cut strips ...

Embodiment 2

[0049] [Preparation Example 2] Preparation of Catalyst B

[0050] Add 3kg of deionized water into the reaction kettle, add 11.7g of nano-titanium dioxide with a particle size of 20-30nm, and stir evenly.

[0051] Dissolve 272.8g of anhydrous copper nitrate, 630.5g of aluminum nitrate nonahydrate, and 133.1g of zinc nitrate hexahydrate in 2.5kg of deionized water to form a mixed metal solution. In addition, a sufficient amount of 20wt% sodium carbonate solution is prepared; both the metal mixed solution and the sodium carbonate solution are heated to 80°C, and are simultaneously added dropwise to the reactor for coprecipitation reaction, and the temperature of the reactor is controlled at 80°C. The dropwise amount of sodium carbonate solution is to maintain the pH of the system at 5-6, and the dropwise addition of the mixed solution is completed within 1.5 hours. Adjust the pH of the system to 9 with the above sodium carbonate solution, and age for 3 hours.

[0052] Then filt...

Embodiment 3

[0053] [Preparation Example 3] Preparation of Catalyst C

[0054] Add 3kg of deionized water into the reaction kettle, add 11.7g of nano-titanium dioxide with a particle size of 20-30nm, and stir evenly.

[0055] 408.6g of anhydrous copper nitrate, 629.6g of aluminum nitrate nonahydrate, and 66.3g of zinc nitrate hexahydrate were dissolved in 2.5kg of deionized water to form a metal mixed solution; in addition, a sufficient amount of 20wt% sodium carbonate solution was prepared, and the metal mixed solution and sodium carbonate solution are heated to 80°C, and are added dropwise into the reactor for co-precipitation reaction. After 1.5h, the dropwise addition of the mixed solution was completed. Adjust the pH of the system to 9 with the above sodium carbonate solution, and age for 3 hours.

[0056] Then filter, wash and dry the filter cake at 120°C for 24 hours, then roast it at 600°C for 5 hours, break the roasted filter cake into strips, and cut them into strip catalysts w...

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Abstract

The invention discloses a method for recycling waste liquid from a butanol device. The method comprises the following steps: a, pretreating the waste liquid from the butanol device through ion exchange resin filled in a fixed bed; b, pressurizing the pretreated waste liquid, fully mixing the pretreated waste liquid with high-pressure hydrogen in a static mixer, and feeding the mixture into a fixed bed reactor for a hydrogenation reaction, wherein the fixed bed reactor is filled with a hydrogenation catalyst; c, after the reaction is finished, removing hydrogen and other light components dissolved in reaction liquid through a high-pressure degassing tank; and d, feeding the degassed reaction liquid to a product refining tower, and carrying out rectifying and separating to obtain butanol. The invention provides the resource recycling method aiming at the specific composition of the waste liquid from the butanol device, and has the advantages of high ester conversion rate, high product selectivity and long catalyst service life.

Description

technical field [0001] The invention relates to a recycling method, in particular to a recycling method for waste liquid from a butanol plant. Background technique [0002] In the existing industrial butanol preparation process, there are mainly two mainstream technologies: homogeneous hydroformylation reaction technology and aqueous hydroformylation reaction technology. Among them, the homogeneous hydroformylation reaction technology has a relatively wider application range. This technology uses a rhodium metal complex as a catalyst to carbonylate synthesis gas and propylene to produce butyraldehyde, which is further hydrogenated to produce butanol. [0003] Heavy components are produced in the above-mentioned carbonylation reaction and butyraldehyde hydrogenation process. For a butanol production plant waste liquid, it can contain 10-15% butyraldehyde, 1-2% butyric acid, and 5-10% butanol , 50-60% of ester impurities, 20-30% of carbon twelve and above substances. At pres...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/80C07C29/76C07C29/90C07C31/12
CPCC07C29/80C07C29/76C07C29/90C07C31/12
Inventor 孔祥明徐艳飞陈俊张郁葱韩金玲赵文强张宏科
Owner WANHUA CHEM GRP CO LTD
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