Catalyst for synthesizing ethylenimine as well as preparation method and application thereof

一种乙撑亚胺、催化剂的技术，应用在催化剂活化/制备、化学仪器和方法、非均相催化剂化学元素等方向，能够解决催化剂活性和选择性低、乙撑亚胺选择性降低、副产物增多等问题，达到使用寿命长、改善扩散效果、降低反应温度的效果

Active Publication Date: 2014-05-28
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In the prior art, the intramolecular dehydration reaction of amino alcohol is carried out at a relatively low temperature (~370°C), the catalyst activity and selectivity are low, and the reaction temperature is high, generally requiring a temperature higher than 400°C to proceed quickly, but Deamination and intermolecular condensation reactions are prone to occur, resulting in an increase in by-products, resulting in a decrease in the selectivity of ethyleneimine. Generally, the weight selectivity is lower than 65%, and the service life is short

Method used

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  • Catalyst for synthesizing ethylenimine as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] In terms of SiO as an oxide 2 :TiO 2 :P 2 o 5 The weight ratio is a stoichiometric configuration of 5:80:15.

[0041] Mix 10g of white carbon black, 160g of titanium dioxide, and 55.7g of diammonium hydrogen phosphate, then add silica sol, the amount of silica sol added is 20% of the mass of titanium dioxide, knead, extrude, dry at 120°C for 6h, and Roast in a furnace at 350°C for 6 hours, then program the temperature at 1°C / min to 650°C for 6 hours to prepare a composite oxide composed of titanium, silicon, and phosphorus.

[0042] Put the composite oxide composed of titanium, silicon and phosphorus into the tubular reactor after cooling, raise the temperature to 150°C, and then use the volume ratio of HF:N 2 =1:5 mixture was fluorinated for 2h to obtain a catalyst carrier. The specific surface area of ​​the carrier was determined by low temperature nitrogen adsorption method to be 42m 2 / g, pore volume 0.22mL / g, average pore diameter 5.6nm.

[0043]According to...

Embodiment 2

[0046] The preparation process in embodiment 2 is basically the same as in embodiment 1, the difference is that according to SiO 2 :TiO 2 :P 2 o 5 The weight ratio is a 10:80:10 stoichiometric configuration. The specific surface area of ​​the catalyst carrier was determined by low temperature nitrogen adsorption method to be 43.2m 2 / g, pore volume 0.21mL / g, average pore diameter 5.8nm.

[0047] According to metal ions as 5.3% load of the carrier mass, the molar ratio of magnesium ions, iron ions, and cesium ions is 8:1:0.1, configure a soluble metal salt solution, impregnate the obtained catalyst carrier for 8 hours, take it out and dry it at 350°C The catalyst was obtained by roasting under nitrogen atmosphere.

[0048] Fill the above catalyst into the reactor with a loading volume of 30mL and heat it to a reaction temperature of 380°C. Nitrogen is used as a protective gas. The gas volume ratio of nitrogen to monoethanolamine is 16. The total space velocity of the gas b...

Embodiment 3

[0050] The preparation process in embodiment 2 is basically the same as in embodiment 1, the difference is that according to SiO 2 :TiO 2 :P 2 o 5 The weight ratio is a 15:80:5 stoichiometric configuration. The specific surface area of ​​the catalyst carrier was determined by low-temperature nitrogen adsorption method to be 46.8m 2 / g, pore volume 0.25mL / g, average pore diameter 6.1nm.

[0051] According to the 0.5% load of metal ions on the mass of the carrier, the molar ratio of magnesium ions, iron ions, and cesium ions is 1:1:0.1, configure a soluble metal salt solution, impregnate the obtained catalyst carrier for 8 hours, take it out and dry it. The catalyst was obtained by roasting in air.

[0052] Fill the above catalyst into the reactor with a loading volume of 30mL, heat it to a reaction temperature of 380°C, use nitrogen as a protective gas, the gas volume ratio of nitrogen to monoethanolamine is 16, and the total gas space velocity in standard state: 3200h -1...

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Abstract

The invention relates to a catalyst for synthesizing ethylenimine as well as a preparation method and application thereof. The related catalyst comprises a carrier and metal ions loaded on the carrier; the carrier is a composite oxide comprising titanium, silicon and phosphorus elements; the metal ions are magnesium ions, iron ions and cesium ions; the molar ratio of the magnesium ions to the iron ions to the cesium ions is (1-10):1:0.1; the mass of all metal ions is 0.5-10 percent of that of the carrier. The related preparation method comprises the step of roasting a catalyst precursor at the temperature of 350-650 DEG C, so that the catalyst is obtained; the catalyst precursor is the mixture of the carrier, soluble salt of magnesium, soluble salt of iron and soluble salt of cesium. The invention also provides the application of the catalyst to synthesis the ethylenimine by using amino alcohol as the raw material. Compared with a common catalyst which has the requirement on the temperature of over 400 DEG C, the catalyst disclosed by the invention obviously reduces the reaction temperature. The prepared catalyst can catalyze the intramolecular dehydration reaction of the amino alcohol and has relatively excellent selectivity.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a catalyst for synthesizing ethyleneimine, a preparation method and an application. Background technique [0002] Ethyleneimine, also known as aziridine, is an important fine chemical product, which has a wide range of uses in the fields of medicine, pesticides, high-energy fuels, and bonding agents. [0003] The initial industrial production method of ethyleneimine is a liquid phase method, using monoethanolamine as a raw material, using concentrated sulfuric acid as a dehydrating agent, the reaction needs to add concentrated alkali, the cost is high and useless inorganic salt by-products are produced, causing serious problems environmental pollution. [0004] US4301036 discloses a catalyst composed of tungsten oxide and silicon oxide, and its application in the synthesis of ethyleneimine. [0005] US4488591 discloses a method for synthesizing ethyleneimi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185C07D203/02C07D203/08
CPCB01J37/04B01J37/082B01J37/26B01J37/28B01J21/063B01J21/08B01J23/78B01J37/0009B01J37/0217B01J27/1853B01J2523/00C07D203/08B01J37/0018B01J35/613B01J35/633B01J35/647B01J2523/15B01J2523/22B01J2523/41B01J2523/47B01J2523/51B01J2523/842B01J35/19B01J27/182B01J37/088
Inventor 杨建明吕剑梅苏宁余秦伟惠丰李亚妮赵锋伟王为强王伟
Owner XIAN MODERN CHEM RES INST
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