A kind of heterogeneous catalyst and its preparation method and the method of using the catalyst to prepare 3-methyl-2-buten-1-ol

A heterogeneous catalyst, methyl technology, applied in isomerization preparation, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of many by-products, increased energy consumption, increased by-products, etc., to reduce the impact, improve The effect of stability and selectivity improvement

Active Publication Date: 2015-11-25
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The reaction of 3-methyl-3-buten-1-ol to prepare 3-methyl-2-buten-1-ol is an equilibrium reaction, and it is difficult to make the conversion rate reach 100% under normal circumstances. In the described patent , did not fundamentally solve the problem that the conversion rate of the equilibrium reaction is not high, and the hydrogenation by-product isoamyl alcohol is difficult to separate, and the removal requires a higher cost
[0011] (1) The single conversion rate is not high. The single conversion rate mentioned in the existing patent is at most 60-70%, and the target selectivity is at most 95%. However, too high conversion rate leads to a decrease in the selectivity of the target product, and the by-products increase
[0012] (2) There are many by-products, mainly isoamyl alcohol, isoprene, and water, which makes product separation difficult and increases energy consumption

Method used

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  • A kind of heterogeneous catalyst and its preparation method and the method of using the catalyst to prepare 3-methyl-2-buten-1-ol
  • A kind of heterogeneous catalyst and its preparation method and the method of using the catalyst to prepare 3-methyl-2-buten-1-ol

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Add 0.83g of palladium chloride, 0.03g of germanium chloride, and 0.045g of praseodymium chloride to 500mL of deionized water to prepare an aqueous solution, add 100g of ZSM-5 molecular sieves with a particle size of 2-3mm to the aqueous solution, and stir evenly , and then aged for 12 hours to obtain a catalyst precursor. After the catalyst precursor was dried, it was calcined at 200°C for 2h, and then reduced with hydrogen at 150°C for 2h at a hydrogen flow rate of 50mL / min to obtain 1# catalyst.

Embodiment 2-10

[0041] Using the same preparation steps as in Example 1, 500mL of deionized water, 100g of ZSM-5 molecular sieve carrier, hydrogen reduction temperature of 150°C, and other parameters according to Table 1 were used to prepare 2~10# catalysts respectively.

[0042] Table 1 catalyst preparation parameters

[0043]

[0044] Note: Catalyst composition = component weight / total weight of heterogeneous catalyst * 100%

Embodiment 11

[0048] Mix 100mL of 1# catalyst with 100mL of Φ2mm triangular spiral packing in the reaction section. The theoretical plate number of the reaction section is 30. Each of the rectification section and the stripping section is filled with 150mL of Φ2mm triangular spiral packing. The theoretical plate numbers are respectively 30 pieces. The system pressure is 50mmHg, the reaction temperature is 60°C, isoprenol is fed from the top of the reaction section, and the weight hourly space velocity is 3.0hr -1 , containing 20% ​​hydrogen (volume ratio), hydrogen-nitrogen mixture gas is fed from the bottom of the stripping section, and the volume space velocity of the mixture gas is 200hr -1 , set total reflux at the top of the tower, hydrogen-nitrogen mixture gas and low boilers are discharged from the emptying system, a small amount of water produced by the reaction is separated through the water separator, and the reaction product is continuously extracted from the tower kettle. The r...

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Abstract

The invention provides a heterogeneous catalyst and a preparation method thereof as well as a method for preparing 3-methyl-2-butene-1-ol in the presence of the catalyst. The heterogeneous catalyst comprises a carrier and three components on the carrier, wherein the first component is selected from one or two or several in palladium, gold, platinum, nickel, chromium and molybdenum; the second component is selected from one or two or several in elements of groups IIIA, IVA and VA; the third component is selected from one or two or several in lanthanide elements. The preparation method comprises the step of performing a reactive distillation process on 3-methyl-3-butene-1-ol to prepare the 3-methyl-2-butene-1-ol in the presence of the heterogeneous catalyst. According to the method provided by the invention, the yield and selectivity of the 3-methyl-2-butene-1-ol can be obviously improved, and the stability of the catalyst is improved, so that the production cost is reduced.

Description

Technical field: [0001] The present invention relates to a kind of isomerization of 3-methyl-3-buten-1-ol (prenyl alcohol) to prepare 3-methyl-2-buten-1-ol (prenyl alcohol). The homogeneous catalyst and the preparation method of the catalyst also relate to a method for preparing 3-methyl-2-buten-1-ol by using the heterogeneous catalyst in a reactive distillation process. Background technique: [0002] 3-Methyl-2-buten-1-ol, namely isopentenol, is mainly used in the synthesis of vitamin E, vitamin A, spice products citral, high-efficiency and low-toxicity pesticides such as pyrethroid insecticides and other important precursors body. As people continue to deepen the synthesis process of 3-methyl-2-buten-1-ol, the application range will be further expanded, and the demand will also increase significantly. Therefore, it is of great significance and application value to strengthen the research on the synthesis technology of 3-methyl-2-buten-1-ol. [0003] According to the dif...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/44B01J29/48C07C33/03C07C29/56
CPCY02P20/10
Inventor 周斌张红涛张永振刘英俊张旭李鹏庞计昌黎源
Owner WANHUA CHEM GRP CO LTD
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