Preparation method for enabling 3-methyl-2-butene-1-alcohol to be synthesized into 3-methylcrotonaldehyde catalyst

A prenyl aldehyde catalyst and alcohol synthesis technology, which is applied in the direction of catalyst activation/preparation, carbon-based compound preparation, organic compound preparation, etc., can solve the problem of high catalyst cost and achieve the effect of low cost and long life

Active Publication Date: 2019-10-25
CHINA CATALYST HLDG CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the traditional prenyl aldehyde synthesis method, TEM-PO and its derivatives are used as the main catalyst, and nitrate and nitrite are auxiliary agents to oxidize prenyl alcohol by oxygen in an organic solvent to prenyl aldehyde. , the cost of the catalyst in this method is extremely high; BASF in Germany uses a catalyst bed composed of copper-silver crystal particles of different sizes as a catalyst to oxidize 3-methyl-3-butene-1-ol in air and then rearrange isopentyl alkenal, and continuously optimize this process; however, the carbon deposition formed by the reaction has a certain impact on the catalyst, and the problem needs to be solved by continuous sintering

Method used

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  • Preparation method for enabling 3-methyl-2-butene-1-alcohol to be synthesized into 3-methylcrotonaldehyde catalyst
  • Preparation method for enabling 3-methyl-2-butene-1-alcohol to be synthesized into 3-methylcrotonaldehyde catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Take 500g of deionized water and put it into a four-necked reaction flask; raise the temperature to 60°C, and stir at a constant temperature; add 500g of 20% silica sol and 294.7g of 20% copper nitrate aqueous solution dropwise; add dropwise at a constant speed, and control the dropwise addition within 2 hours; Keep the temperature at 60°C and let it stand for aging for 6 hours; start stirring, control the temperature of the kettle at 60°C, add 245g of 5% ammonium heptamolybdate aqueous solution into the reaction bottle dropwise, and control the drop for one hour; then add 181g of 1% telluric acid aqueous solution dropwise Add it into the reaction bottle, control the dripping for 1 hour; keep the temperature at 60°C, let stand for aging for 2 hours; filter, wash the filter cake with deionized water until PH = 7; dry the filter cake at 120°C, and roast at 550°C for 6 hours; after roasting The catalyst is compressed into a 5*5mm cylinder and is ready for use. Take 50 g of...

Embodiment 2

[0027] Take 500g of deionized water and put it into a four-necked reaction flask; raise the temperature to 60°C, and stir at a constant temperature; add 500g of 20% silica sol and 333g of 20% copper nitrate aqueous solution; 60°C, stand for aging for 6 hours; start stirring, control the temperature of the kettle at 60°C, add 222g of 4.5% ammonium heptamolybdate aqueous solution dropwise into the reaction bottle, and control the dripping for one hour; then add 100g of 1% telluric acid aqueous solution Add it dropwise into the reaction bottle, and control the dripping for 1 hour; keep the temperature at 60°C, let it stand for aging for 2 hours; filter, wash the filter cake with deionized water until PH=7; dry the filter cake at 120°C, and roast at 550°C for 6 hours; roast The final catalyst was compressed into a 5*5mm cylinder for use. Take 50 g of the formed catalyst and fill it into the middle of the fixed-bed reactor, control the temperature at 230° C. and the hydrogen flow r...

Embodiment 3

[0030] Take 500g of deionized water and put it into a four-necked reaction flask; raise the temperature to 60°C, and stir at a constant temperature; add 500g of 20% silica sol and 294.7g of 20% copper nitrate aqueous solution dropwise; add dropwise at a constant speed, and control the dropwise addition within 2 hours; Keep the temperature at 60°C and let it stand for aging for 6 hours; start stirring, control the temperature of the kettle at 60°C, add 300g of 5% ammonium heptamolybdate aqueous solution into the reaction bottle dropwise, and control the dripping for one hour; then add 200g of 1% telluric acid aqueous solution dropwise Add it into the reaction bottle, control the dripping for 1 hour; keep the temperature at 60°C, let stand for aging for 2 hours; filter, wash the filter cake with deionized water until PH = 7; dry the filter cake at 120°C, and roast at 550°C for 6 hours; after roasting The catalyst is compressed into a 5*5mm cylinder and is ready for use. Take 50 ...

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Abstract

The invention discloses a preparation method for enabling 3-methyl-2-butene-1-alcohol to be synthesized into a 3-methylcrotonaldehyde catalyst. The preparation method for enabling 3-methyl-2-butene-1-alcohol to be synthesized into the 3-methylcrotonaldehyde catalyst comprises the steps that firstly a certain proportion of a copper-silicon carrier is prepared by a gel method, and then active component molybdenum and ruthenium are loaded by a certain ratio by a dipping method, and the mixture is dried, calcined and shaped to obtain the catalyst. The catalyst is charged to a fixed bed reactor foractivation. Feeding and reaction are carried out, it is verified that the catalyst has a conversion rate of up to 80% and selectivity of up to 99% for the synthesis of 3-methyl-2-butene-1-alcohol into 3-methylcrotonaldehyde, the catalyst can be used for reaction without air and oxygen, the catalyst is long in service life and low in cost, and continuous production and environmental protection areachieved.

Description

technical field [0001] The invention belongs to a synthesis method of organic compounds, and relates to a preparation method of a catalyst for synthesizing prenyl aldehyde from 3-methyl-2-buten-1-ol Background technique [0002] Prenaldehyde is an important chemical raw material, mainly used as an intermediate of medicine, and also used to prepare daily necessities and flavors, and it is also an important intermediate for the synthesis of citral. Citral is a raw material for synthesizing ionone, methyl ionone, and damascenone; as an organic raw material, it can be reduced to citronellol, nerol, and geraniol; it can also be converted into citronellol. It is used in the manufacture of vitamins A and E in the pharmaceutical industry, and is also the raw material of phytol. With the continuous expansion of applications, the market demand for prenaldehyde continues to expand. In the traditional prenyl aldehyde synthesis method, TEM-PO and its derivatives are used as the main ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J27/057B01J37/02B01J37/03C07C45/00C07C47/21
CPCB01J23/72B01J27/0576B01J37/036B01J37/0201C07C45/002C07C47/21
Inventor 王庆吉王蕊王炳春王贤彬李进
Owner CHINA CATALYST HLDG CO LTD
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