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Method and system for preparing 3-methyl-2-buten-1-ol through ester exchange

A technology of prenol and prenol acetate, which is applied in the field of rectifying separation and preparation of prenol products, can solve the problems of large amount of waste water, difficult treatment, high energy consumption for separation, avoid corrosion, and easily The effect of separation and recovery and simplified process flow

Active Publication Date: 2014-08-20
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The method described in the above-mentioned patent has disadvantages such as the use of polar organic solvents, high energy consumption for separation, and the large amount of waste water produced is difficult to handle. The development of a solvent-free, three-waste-free, and low-energy-consumption prenol manufacturing process is in line with the development of green chemical industry requirements

Method used

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  • Method and system for preparing 3-methyl-2-buten-1-ol through ester exchange
  • Method and system for preparing 3-methyl-2-buten-1-ol through ester exchange

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Experimental program
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Effect test

Embodiment 1

[0029] at 3m 3 In the transesterification reactor, add prenyl alcohol acetate 1000kg, methanol 1250kg, strong basic anion exchange resin 50kg, react at 50 ℃ for 3h, the conversion ratio of prenyl alcohol acetate after the reaction is 99.7 %, the yield of isopentenol is 99.4%. The obtained transesterification reaction liquid enters the continuous separation and purification process, and the mass fraction of the final product isopentenol can reach 99.85%. The flow rate of each stream is shown in Table 1.

[0030] Table 1

[0031]

[0032]

Embodiment 2

[0034] 5kg KOH solid was dissolved in 100L deionized water, 100kg SiO 2The solution was added to the above solution, and after stirring for 1 h, the water in the system was removed by a rotary evaporator. The obtained solid was vacuum dried at 80° C. for 24 h to obtain a solid base catalyst with a KOH loading of 5 wt %.

[0035] at 3m 3 In the transesterification reactor, add prenol acetate 1600kg, recovered prenol acetate 200kg, methanol 250kg, reclaimed methanol 200kg, KOH / SiO 2 18kg of solid base catalyst was reacted at 80° C. for 1 hour. After the reaction, the conversion rate of prenol acetate was 70.5%, and the yield of prenol was 70.3%. The obtained transesterification reaction solution enters the continuous separation and purification process, and the mass fraction of the final product isoprenol can reach 99.51%. The flow rates of each stream are shown in Table 2.

[0036] Table 2

[0037]

Embodiment 3

[0039] Dissolve 30kg of NaOH solid in 100L of deionized water, add 100kg of MCM-41 molecular sieves to the above solution, and after stirring for 1 hour, remove the water in the system by a rotary evaporator. The obtained solid was vacuum dried at 80° C. for 24 h to obtain a solid base catalyst with a NaOH loading of 30 wt %.

[0040] at 3m 3 In the transesterification reactor, add prenol acetate 1100kg, reclaimed prenol acetate 100kg, methanol 850kg, reclaim methanol 50kg, NaOH / MCM-41 solid base catalyst 36kg, react at 60 ℃ 2h, the conversion rate of prenol acetate was 85% after the reaction, and the yield of prenol was 84.6%. The obtained transesterification reaction solution enters the continuous separation and purification process, and the mass fraction of the final product isoprenol can reach 99.77%. The flow rates of each stream are shown in Table 3.

[0041] table 3

[0042]

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Abstract

The invention relates to a method and a system for preparing 3-methyl-2-buten-1-ol through ester exchange. According to the method, solvent-free heterogeneous catalysis ester exchange reaction is carried out on 3-methyl-2-buten-1-ol acetic acid ester and methyl alcohol used as raw materials under the catalytic action of solid alkali or strongly alkaline anion exchange resin so as to obtain 3-methyl-2-buten-1-ol and methyl acetate, and after purification, the unreacted methyl alcohol and the unreacted 3-methyl-2-buten-1-ol acetic acid ester can be recycled. The method has the characteristics that the catalyst is easy to separate, recycle and reuse, no three wastes (waste gas, industrial wastewater and industrial residue) are generated, the yield of the 3-methyl-2-buten-1-ol product is high, and the like.

Description

technical field [0001] The invention relates to a method for preparing prenol by transesterification, in particular to a method for transesterifying prenol acetate and methanol, followed by distillation and separation to prepare a prenol product. Background technique [0002] Isopentenol, whose scientific name is 3-methyl-2-buten-1-ol, is a widely used chemical intermediate, which can be used to synthesize methyl pyrethinate and its downstream high-efficiency and low-toxicity pesticide pyrethroids Insecticides - permethrin, etc., can also be used in the synthesis of fine chemicals such as fragrances and essences. [0003] There are many ways to prepare isopentenol, such as using isobutylene as raw material, and formaldehyde under the action of solid base catalyst, through Prins condensation reaction to obtain 3-methyl-3-buten-1-ol, and then isomerize to obtain isopentenol. The reaction temperature and pressure of this method are high, and the requirements for equipment are...

Claims

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Application Information

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IPC IPC(8): C07C33/03C07C69/14C07C27/00C07C67/03C07C29/128
CPCC07C29/1285C07C67/03C07C69/14C07C33/03
Inventor 崔咪芬汤吉海曹雅陈献费兆阳乔旭
Owner NANJING UNIV OF TECH
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