Isomerization synthesis of 3-methyl-2-buten-1-ol using water-containing methyl butenol

A water-containing methyl butenol and isopentenol technology, applied in the field of chemical engineering, can solve the problems of low selectivity, increased separation process, low selectivity, etc., and achieve the effect of high reactivity and selectivity

Active Publication Date: 2016-09-28
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this reaction system introduces more other components, which increases the subsequent separation process and brings about the problem of solvent loss.
In addition, from the results reported by the patent, the reaction rate is very slow, and the conversion rate of reaction 4-15h is only 22%
When Rajender Reddy Leleti et al. used methanesulfonic acid as a catalyst, the reaction rate was slow and the selectivity was not high. In...

Method used

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  • Isomerization synthesis of 3-methyl-2-buten-1-ol using water-containing methyl butenol
  • Isomerization synthesis of 3-methyl-2-buten-1-ol using water-containing methyl butenol
  • Isomerization synthesis of 3-methyl-2-buten-1-ol using water-containing methyl butenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-9

[0019] Embodiment 1-9: Isomerization experiments under different water contents

[0020] Add about 150g of methylbutenol raw material into a 250mL high-pressure stirred tank, and add a certain amount of water to prepare reaction raw materials with different water contents, and then add about 2.0g of ammonium metavanadate. After replacing with nitrogen for several times, the temperature was raised to 160°C, and samples were taken after 60 minutes of reaction. The samples were analyzed by gas chromatography and calculated as shown in Table 1.

[0021] Table 1 Results of isomerization reaction at different water contents

[0022] Example

[0023] Note: Comparative Example 8* uses the ester synthesized from vanadium pentoxide and n-hexanol as the catalyst, and 9* uses the ester synthesized from vanadium pentoxide and isoamyl alcohol as the catalyst. The results show that when esters are used as catalysts, a small amount of water will obviously reduce the selectivity of ...

Embodiment 10-13

[0024] Embodiment 10-13: Isomerization experiments under different catalyst concentrations

[0025] Add about 150g of methylbutenol raw material and 4g of water into a 250mL high-pressure stirred tank to prepare a reaction material with a water content of 2.6%, and then add a certain amount of ammonium metavanadate. After replacing with nitrogen for several times, the temperature was raised to 160°C, and samples were taken after 60 minutes of reaction. The samples were analyzed by gas chromatography and calculated as shown in Table 2.

[0026] Table 2 Experimental results of different catalyst concentrations

[0027] Example

Embodiment 14

[0028] Embodiment 14: Catalyst circulation experiment

[0029] Add about 600g of methylbutenol raw material into a 1000mL high-pressure stirred tank, and then add 15g of water and 15g of ammonium metavanadate. After replacing with nitrogen for several times, the temperature was raised to 160°C, and the reaction was stopped after 60 minutes and samples were taken for analysis. After cooling, the reaction liquid is filtered to obtain the catalyst for use, and the filtrate is rectified to obtain the product isopentenol and unreacted methyl butenol. Add unreacted methylbutenol to 600g and then add it into the reaction kettle to continue the reaction for 60min. The analysis results of the reaction solution circulated four times were calculated and obtained as shown in Table 3. The analytical results of product isopentenol are shown in Table 4.

[0030] Table 3 Results of isomerization cycle experiments

[0031]

[0032] Table 4 Analysis results of product isopentenol composi...

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Abstract

The invention belongs to the field of chemical engineering and particularly relates to isomerization synthesis of 3-methyl-2-buten-1-ol using methyl butenol in a water-containing condition. In the invention, the methyl butenol is adopted as a raw material for isomerization synthesis of 3-methyl-2-buten-1-ol; in the reaction materials, the water content is 0.5-6.5%; the catalyst is vanadium oxide or vanadium-containing metal salt; the catalyst concentration is 0.1-5.0%, the reaction temperature is 120-190 DEG C, and the reaction time is 20-180min; the purity of the obtained 3-methyl-2-buten-1-ol product is higher than or equal to 98%; and the 3-methyl-2-buten-1-ol selectivity in the reaction process can be controlled at 95% or above. The invention has the following advantages: the adopted catalyst does not need to be prepared in advance and is relatively cheap; the raw material methyl butenol can be adopted for isomerization synthesis of 3-methyl-2-buten-1-ol in a water-containing condition; and the reaction activity and selectivity are relatively high.

Description

technical field [0001] The invention belongs to the field of chemical engineering, in particular to the isomerization of water-containing methyl butenol to synthesize isopentenol. Background technique [0002] Isopentenol is an important spice, pharmaceutical and pesticide intermediate, mainly used to produce citral, isophytol, DV permethrin, etc., and also used to synthesize the third generation cement water reducer, polycarboxylate water reducer Raw material TPEG. According to the different sources of raw materials, there are mainly three routes for the formation of prenyl alcohol: the condensation of isobutylene and formaldehyde, the method of acetylene acetone and the hydration of isoprene. [0003] Using acetylene acetone as a raw material to obtain methyl butynol through alkynylation, and then half-hydrogenating to generate methyl butenol, and then isomerizing to obtain isopentenol. In this process route, the alkynylated product methyl butynol and water form an azeot...

Claims

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Application Information

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IPC IPC(8): C07C33/03C07C29/56
CPCC07C29/56C07C33/03
Inventor 陶川东谭平华赖崇伟陈群文王小莉李杰灵余维新刘旋
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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