A method for separating 1,1-dimethylallyl 3-methyl-2-butenyl ether and 3-methyl-2-buten-1-ol
A technology of dimethylallyl and butenyl ether, which is applied in ether separation/purification, ether preparation, organic chemistry, etc. It can solve the problems of affecting product yield, ineffective separation, low purity, etc., and achieves low processing cost , easy separation, simple process effect
Active Publication Date: 2020-12-15
SHAOXING MINGYE CHEM FIBER
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[0004] Wherein 1,1-dimethylallyl 3-methyl-2-butenyl ether and 3-methyl-2-buten-1-alcohol will form a homogeneous azeotrope, and at -90kPa (G), Azeotropic composition (wt%): 1,1-dimethylallyl 3-methyl-2-butenyl ether: about 19%, 3-methyl-2-buten-1-ol: about 81%, The azeotropic temperature is about 82°C, and cannot be effectively separated by ordinary distillation methods
The azeotropic phenomenon causes the purity of the product 3-methyl-2-buten-1-ol to be low, and entrains a large amount of 3-methyl-2-buten-1-ol, which affects the product yield
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[0013] Specific embodiments of the present invention will be described in detail below in conjunction with the accompanying drawings. It should be understood that the specific embodiments described here are only used to illustrate and explain the present invention, and are not intended to limit the present invention.
[0014] Such as figure 1 A kind of 1,1-dimethylallyl 3-methyl-2-butenyl ether and the separation method of 3-methyl-2-butene-1-alcohol comprise following process: Packed extractive distillation column 1 lower half packing 2 places are continuously fed with 1,1-dimethylallyl 3-methyl-2-butenyl ether and 3-methyl-2-buten-1-ol The azeotropic mixture of the extractive distillation column is continuously fed into two (3-methyl-2-butenyl) ethers as the extractant at the packing 3 in the upper part of the extractive distillation column. The extractive distillation column is equipped with BX500 structured packing with a theoretical plate of 4.5-5.5 blocks / m, which has ...
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Abstract
The invention discloses a separating method of 1,1-methylallyl-3-methyl-2-butenyl ether and 3-methyl-2-butene-1-ol. The separating method comprises the following steps: isomerizing 2-methyl-3-butene-2-ol in an acid environment to generate the 3-methyl-2-butene-1-ol; and with a byproduct bis(3-methyl-2-butenyl) ether in the production process as an extracting agent, carrying out extractive distillation to effectively separate an azeotrope of the 1,1-methylallyl-3-methyl-2-butenyl ether and the 3-methyl-2-butene-1-ol and improve the acquisition rate of the 3-methyl-2-butene-1-ol. The separatingmethod has the characteristics of simple process, low energy consumption and low treatment cost; the boiling point of the 1,1-methylallyl-3-methyl-2-butenyl ether discharged from the tower bottom hasgreat disparity with that of the bis(3-methyl-2-butenyl) ether, and the 1,1-methylallyl-3-methyl-2-butenyl ether is easily separated from the bis(3-methyl-2-butenyl) ether by general rectification under vacuum, so that cycle use of the bis(3-methyl-2-butenyl) ether can be realized.
Description
Technical field: [0001] The invention relates to a method for separating 1,1-dimethylallyl 3-methyl-2-butenyl ether and 3-methyl-2-buten-1-ol. Background technique: [0002] 3-Methyl-2-buten-1-ol is mainly used to react with trimethyl orthoacetate to synthesize methyl permethrin, which is the key intermediate for the preparation of pyrethroids, homocis permethrin (DV-chrysanthemum acid or chrysanthemic acid ester) important raw material. In the process route of synthesizing 3-methyl-2-buten-1-ol with isoprene as the main raw material, chlorinated isopentene is first prepared by addition of isoprene and anhydrous hydrogen chloride, and then in alkali The mixture of 3-methyl-2-butene-1-ol and 2-methyl-3-butene-2-ol is obtained by hydrolysis in medium. Patent CN201110306882.0 introduces 2-methyl-3-butene-2- The alcohol is isomerized in an acidic environment to form 3-methyl-2-buten-1-ol. In this process, two kinds of ether by-products are generated simultaneously, i.e. 1,1-d...
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IPC IPC(8): C07C41/34C07C41/42C07C43/15
CPCC07C41/34C07C41/42C07C43/15
Inventor 董金锋王东徐峰徐赛华
Owner SHAOXING MINGYE CHEM FIBER