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Dewatering catalyst and application thereof in preparing morpholine

A technology of catalyst and magnesium oxide, which is applied in the field of fine chemical industry and catalyst technology, can solve the problems of low reaction yield, high production cost and complicated process, so as to improve selectivity and stability, avoid environmental protection problems and high market competition force effect

Inactive Publication Date: 2012-06-13
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantages are: pressure-resistant equipment is required, the process is complicated, the catalyst has low selectivity, short life, high active metal content, etc.
The process is relatively simple, but the reaction yield is low, the production cost is high, and the raw material DEA is expensive
And because this method uses sulfuric acid to react, the used sulfuric acid must be neutralized with alkali, which brings a lot of waste liquid and by-products

Method used

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  • Dewatering catalyst and application thereof in preparing morpholine
  • Dewatering catalyst and application thereof in preparing morpholine
  • Dewatering catalyst and application thereof in preparing morpholine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 0.5299g of zirconium oxychloride (ZrOCl 2 ·8H 2 O, ZrO 2 content 36%) was dissolved in deionized water, and 5.0 g of treated alumina dry rubber powder was immersed in the above solution, while stirring and dropping ammonia water to adjust and maintain pH = 8-10, aged for 2 hours, then filtered and washed until no Chloride ions, and finally dried at 120°C for 12 hours, and calcined at 600°C for 3 hours.

[0025] 0.70g of catalyst was placed in the constant temperature section of the reactor, and both ends were supported by quartz sand. From room temperature to 260°C at a heating rate of 2°C / min. Use a micro metering pump to send 20% diethanolamine solution into the reactor, the solvent is morpholine, and the space velocity of diethanolamine is 0.2h -1 , At the same time through the ammonia gas 6ml / min, every 2 hours to collect a sample, product analysis by gas chromatography. No less than 3 samples were collected, and the average value of 3 parallel samples wa...

Embodiment 2

[0027] Weigh 0.1567g of 96% titanium sulfate (Ti(SO 4 ) 2 ) was dissolved in deionized water, and an equal volume was impregnated onto 3.0 g of treated γ-alumina for 24 hours, then dried at 120°C for 12 hours, and calcined at 600°C for 3 hours.

[0028] 0.52g of catalyst was placed in the constant temperature section of the reactor, and both ends were supported by quartz sand. From room temperature to 260°C at a heating rate of 2°C / min. Use a micro metering pump to send 20% diethanolamine solution into the reactor, the solvent is morpholine, and the space velocity of diethanolamine is 0.3h -1 , At the same time through the ammonia gas 6ml / min, every 2 hours to collect a sample, product analysis by gas chromatography. No less than 3 samples were collected, and the average value of 3 parallel samples was taken as the product composition for calculation.

Embodiment 3

[0030] Weigh 0.1560g of sodium hydroxide (NaOH) and dissolve it in deionized water, impregnate an equal volume on 3.0g of treated γ-alumina for 24h, then dry at 120°C for 12h, and bake at 600°C for 3h.

[0031] 0.52g of catalyst was placed in the constant temperature section of the reactor, and both ends were supported by quartz sand. From room temperature to 260°C at a heating rate of 2°C / min. Use a micro metering pump to send 20% diethanolamine solution into the reactor, the solvent is morpholine, and the space velocity of diethanolamine is 0.2h -1 , At the same time through the ammonia gas 6ml / min, every 2 hours to collect a sample, product analysis by gas chromatography. No less than 3 samples were collected, and the average value of 3 parallel samples was taken as the product composition for calculation.

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Abstract

The invention relates to a novel catalyst for preparing morpholine by virtue of gas-phase catalysis and dewatering of diethanol amine and an application thereof. The catalyst adopts gamma-alumina as a carrier; an active component is one or the combination of some of zirconium oxide, titanium sulfate, sodium hydroxide, potassium hydroxide and magnesium oxide; and the load of the active component accounts for 0.1wt%-30wt% of the catalyst. In the presence of a solvent and ammonia gas, in a fixed bed reactor, the catalyst prepared by the method is higher in dewatering activity; and the diethanol amine is utilized as a raw material, thus the reaction conversion rate and the selectivity are high.

Description

technical field [0001] The invention belongs to the field of catalyst technology and fine chemical industry, in particular, it relates to a dehydration catalyst and its application in the preparation of morpholine Background technique [0002] Morpholine, also known as morpholine or 1,4-oxazidine, is one of the important cyclic amines for industrial use. It is a colorless water-absorbing oily liquid at room temperature, weakly alkaline, hygroscopic and ammoniacal odor. Due to the characteristics of nitrogen and oxygen heterocycles, morpholine occupies an important position in chemical production. It is an intermediate in the manufacture of many fine chemical products and can be used to prepare NOBS (N-oxodiethylene-2-benzothiazole sulfenamide ), OTOS (N-oxodiethylene thiocarbamoyl-N-oxodiethylene sulfenamide) and other rubber vulcanization accelerators and rust inhibitors, preservatives, cleaning agents, descaling agents , analgesics, local anesthetics, fruit preservatives...

Claims

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Application Information

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IPC IPC(8): B01J21/06B01J23/04B01J21/10B01J27/055C07D295/027C07D295/023
Inventor 陈波李明时鲁墨弘朱建军单玉华
Owner CHANGZHOU UNIV
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