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Ethylene glycol catalyst prepared from dimethyl oxalate and preparation method of ethylene glycol catalyst

A dimethyl oxalate and catalyst technology, which is applied in the field of dimethyl oxalate to prepare ethylene glycol catalyst and its preparation, can solve the problems of activity decline, calcium agglomeration, sintering, etc., and achieve improved activity, good selectivity, and high reaction active effect

Inactive Publication Date: 2019-05-21
李磊
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the catalytic reaction of selective hydrogenation of dimethyl oxalate is mainly based on silica-supported calcium-based catalysts. During the reaction process, generally supported calcium-silicon catalysts are prone to calcium agglomeration and sintering, resulting in decreased activity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0022] The preparation method of the catalyst of this embodiment includes the following steps. In step 1, according to the content of iron oxide in the catalyst, ferric nitrate or ferric acetate is prepared into a solution, and a precipitation agent is prepared into a solution. The precipitation agent is ammonia or Ammonium bicarbonate; Step two, add the prepared iron-containing solution, precipitant solution and silica sol into a container with a stirrer at the same time, and stir for co-precipitation; Step three, evaporate the above solution, wash with water, and dry to obtain iron Silicon catalyst precursor; step four, the above-mentioned iron-silicon catalyst precursor is respectively impregnated with calcium nitrate or calcium acetate solution, tungsten nitrate or tungsten acetate solution; step five, the impregnated iron-silicon catalyst precursor is roasted at 200-600℃ After 8 hours, the catalyst is finally formed by a forming machine to obtain the catalyst.

[0023] In st...

Embodiment 1

[0026] Step 1: 22gZn(NO 3 )2·6H 2 O and 22gNH 4 HCO 3 Prepare 500ml solution respectively;

[0027] Step 2: 50g of silica sol with a concentration of 30%, the iron solution and the precipitant solution are added to a container with a stirrer in parallel to stir;

[0028] Step 3: The temperature is raised to 100°C to remove most of the water, and the precipitate is separated out, the precipitate is washed three times with water, and finally dried;

[0029] Step 4: The ZnSi catalyst precursor prepared by the co-precipitation is then immersed in a solution of 4g calcium nitrate and 8g tungsten nitrate;

[0030] Step 5: The catalyst precursor of the impregnating auxiliary agent is calcined at 350° C. for 8 hours, and finally formed by a forming machine to obtain catalyst A.

[0031] The catalyst needs 10% H before use 2 -N 2 Gas reduction, the reduction temperature is 150~400℃. The reduction is divided into three stages, the initial stage is 150~250℃, the heating rate is 25℃ / h, when the te...

Embodiment 2

[0033] Step 1: 23.3gZn(Ac) 2 ·2H 2 O and 50ml concentrated ammonia water are respectively configured into 500ml solution;

[0034] Step two and step three are the same as in embodiment 1;

[0035] Step 4: The ZnSi catalyst precursor prepared by the above co-precipitation is then immersed in a solution of 3g calcium nitrate and 10g iron acetate;

[0036] Step 5: The catalyst precursor of the impregnating aid is calcined at 550° C. for 8 hours, and finally formed by a forming machine to obtain catalyst B.

[0037] The catalyst needs 30% H before use 2 -N 2 Gas reduction, the reduction temperature is 150~400℃. The reduction is divided into three stages, the initial stage is 150~250℃, the heating rate is 20℃ / h, when the temperature rises to 250℃, the constant temperature is 8 hours; the middle stage is 250~300℃, the heating rate is 15℃ / h, when the temperature rises to 300℃ Constant temperature for 8 hours; the final stage is 300-380℃, the heating rate is 10℃ / h, when the temperature rises...

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Abstract

The invention relates to an ethylene glycol catalyst prepared from dimethyl oxalate and a preparation method of the ethylene glycol catalyst. The ethylene glycol catalyst is prepared from ferric oxide, calcium oxide, tungsten oxide and SiO2, wherein the content of the ferric oxide is 20% to 60%, the content of the calcium oxide is 5% to 12%, the content of the tungsten oxide is 5% to 20%, the content of the SiO2 is 8% to 70%, and the content is based on the mass percent of the oxide in one part of the catalyst. The preparation method of the catalyst comprises the following steps: preparing ferric nitrate or ferric acetate and ammonium hydroxide or ammonium hydrogen carbonate into a solution; simultaneously adding the prepared iron-containing solution, a precipitator solution and silica solinto a container with a stirrer, stirring and performing coprecipitation; evaporating the solution to dryness, washing and drying to obtain an iron-silicon catalyst precursor; separately and sequentially dipping the iron-silicon catalyst precursor into a calcium nitrate or calcium acetate solution and a tungsten nitrate or tungsten acetate solution; and roasting the dipped iron-silicon catalyst precursor under 200 to 600 DEG C for 8 hours and finally forming through a forming machine. The ethylene glycol catalyst and the preparation method of the ethylene glycol catalyst involved in the invention have the advantages of reducing catalyst preparation cost; and the catalyst has high activity and good stability.

Description

Technical field [0001] The invention relates to the field of ethylene glycol preparation, in particular to a catalyst for preparing ethylene glycol from dimethyl oxalate and a preparation method thereof. Background technique [0002] Dimethyl oxalate is an important raw material for ethylene glycol from coal. Ethylene glycol is an important chemical raw material. It is mainly used to make polyester polyester and polyester resin. It can produce synthetic resin PET, namely polyethylene terephthalate, fiber grade PET, polyester fiber, bottle flake grade PET is used to make mineral water bottles, etc. It can also produce alkyd resin, glyoxal, etc., and can also be used as an antifreeze, etc., with a wide range of uses. In the past ten years, due to the continuous increase in domestic demand for polyester industry, the dependence on imports has always been as high as 60%, and the domestic production gap is relatively large. my country is rich in coal and less oil. Coal-to-ethylene ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/80B01J23/888C07C29/149C07C31/20
CPCY02P20/52
Inventor 李磊
Owner 李磊
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