阅读说明：本技术 一种二环戊基醚的生产方法 (Production method of dicyclopentyl ether ) 是由 石康明 于 2019-08-28 设计创作，主要内容包括：本发明公开一种二环戊基醚的生产方法,具体包括将环戊醇通过由催化剂强酸性阳离子交换树脂构成的固定床进行脱水反应的步骤,其中：环戊醇的体积液时空速控制为0.5～2.0hr<Sup>-1</Sup>,系统压力控制为0.1～1.0MPa,进料温度控制为60～130℃,催化剂磺酸基阳离子交换树脂的质量交换容量为3～5.5mmol/g。本发明的二环戊基醚的生产方法,通过磺酸基阳离子交换树脂催化剂催化环戊醇脱水来生产二环戊基醚,二环戊基醚的转化率高,且工艺简单,工艺环保,易于工业化大生产和工业化推广应用。(The invention discloses a production method of dicyclopentyl ether, which specifically comprises the step of carrying out dehydration reaction on cyclopentanol through a fixed bed formed by a catalyst, namely a strong-acid cation exchange resin, wherein: the volume liquid hourly space velocity of cyclopentanol is controlled to be 0.5-2.0 hr ‑1 The system pressure is controlled to be 0.1-1.0 MPa, the feeding temperature is controlled to be 60-130 ℃, and the mass exchange capacity of the sulfonic cation exchange resin catalyst is 3-5.5 mmol/g. The production method of dicyclopentyl ether of the invention produces dicyclopentyl ether by catalyzing cyclopentanol to dehydrate through sulfonic cation exchange resin catalyst, the conversion rate of dicyclopentyl ether is high, and the process is simple, environment-friendly, and easy for industrial mass production and industrial popularization and application.)

1. A production method of dicyclopentyl ether is characterized by specifically comprising the step of carrying out dehydration reaction on cyclopentanol through a fixed bed consisting of a catalyst, namely a strong-acid cation exchange resin, wherein:

the volume liquid hourly space velocity of cyclopentanol is controlled to be 0.5-2.0 hr^-1The system pressure is controlled to be 0.1-1.0 MPa, the feeding temperature is controlled to be 60-130 ℃, and the mass exchange capacity of the sulfonic cation exchange resin catalyst is 3-5.5 mmol/g.

2. The method for producing dicyclopentyl ether of claim 1, wherein the mass exchange capacity of the sulfonic acid group cation exchange resin is 3.5 to 4.5 mmol/g.

3. The method for producing dicyclopentyl ether according to claim 1, wherein the sulfonic acid group cation exchange resin is a spherical sulfonic acid group cation exchange resin having a particle diameter of 0.40 to 1.25 mm.

4. The method for producing dicyclopentyl ether of claim 1, wherein the liquid hourly space velocity is controlled to be 0.8 to 1.5hr^-1。

5. The method for producing dicyclopentyl ether according to claim 1, wherein the system pressure is controlled to be 0.2 to 0.6 MPa.

6. The method for producing dicyclopentyl ether according to claim 1, wherein the feed temperature is controlled to 80 to 100 ℃.

Technical Field

The invention belongs to the technical field of chemical synthesis, and particularly relates to a production method of dicyclopentyl ether.

Background

Dicyclopentyl ether is a novel hydrophobic ether solvent, is a more environment-friendly solvent, can be used for replacing tetrahydrofuran, methyl tetrahydrofuran, cyclopentyl methyl ether, methyl tert-butyl ether, dioxane and the like as reaction solvents, and is used for reactions such as Grignard reaction, coupling amination reaction, metal reduction and the like. Compared with the solvents, the dicyclopentyl ether has the characteristics of easy recovery and refining and environmental protection, has better dissolving performance for various reagents, and is a reaction solvent with good prospect.

Disclosure of Invention

The invention aims to provide a production method of dicyclopentyl ether, which produces dicyclopentyl ether by intermolecular dehydration reaction of cyclopentanol on a sulfonic cation exchange resin catalyst and has the characteristics of simple process, environmental protection and easy industrial operation.

In order to achieve the purpose, the invention adopts the following technical scheme:

a production method of dicyclopentyl ether specifically comprises a step of carrying out dehydration reaction on cyclopentanol through a fixed bed composed of a catalyst sulfonic cation exchange resin, wherein:

the volume liquid hourly space velocity of cyclopentanol is controlled to be 0.5-2.0 hr^-1The system pressure is controlled to be 0.1-1.0 MPa, the feeding temperature is controlled to be 60-130 ℃, and the mass exchange capacity of the sulfonic cation exchange resin catalyst is 3-5.5 mmol/g.

Preferably, the mass exchange capacity of the sulfonic cation exchange resin is 3.5-4.5 mmol/g.

Preferably, the sulfonic acid group cation exchange resin is spherical sulfonic acid group cation exchange resin with the particle size of 0.40-1.25 mm.

Preferably, the hourly space velocity of the liquid is controlled to be 0.8-1.5 hr^-1。

Preferably, the system pressure is controlled to be 0.2-0.6 MPa.

Preferably, the feeding temperature is controlled to be 80-100 ℃.

Preferably, the volume liquid hourly space velocity of cyclopentanol is controlled to be 0.8-1.5 hr^-1Controlling the system pressure to be 0.2-0.6 MPa, controlling the feeding temperature to be 80-100 ℃, and controlling the mass exchange capacity of the sulfonic cation exchange resin catalyst to be 3.5-4.5 mmol/g; the sulfonic cation exchange resin is spherical sulfonic cation exchange resin with the particle size of 0.40-1.25 mm.

It should be noted that the inventors found that the dehydration of cyclopentanol as the starting material is most temperature sensitiveWhen the temperature exceeds 150 ℃, intramolecular dehydration of cyclopentanol occurs to produce dicyclopentanyl ether and intramolecular dehydration occurs to produce cyclopentene, and higher temperature results in-SO on the surface of the sulfonic acid-based cation exchange resin₃The functional group falls off to shorten the service life of the catalyst, so the reaction is carried out at a lower temperature range of 60-130 ℃, and the total yield of the reaction can be improved by recycling unreacted cyclopentanol though the conversion per pass of the cyclopentanol is lower.

More preferably, spherical sulfonic cation exchange resin with the particle diameter of 0.40-1.25 mm is used as the catalyst, and the mass exchange capacity of the catalyst is 4.5 mmol/g. The hourly space velocity of the liquid is controlled to be 1.5hr^-1The system pressure is controlled to be 0.6MPa, the feeding temperature is controlled to be 100 ℃, and the conversion rate of dicyclopentyl ether reaches 98.9 percent.

Compared with the prior art, the invention has the following beneficial technical effects:

(1) the invention produces the dicyclopentyl ether product by catalyzing the cyclopentanol to dehydrate through the sulfonic cation exchange resin, and has the characteristics of simple process, low operation cost, environmental protection and easy industrial operation.

(2) The method has mild reaction conditions, and the selectivity of the dicyclopentyl ether is more than or equal to 97.5 percent and can reach 98.9 percent at most.

Detailed Description

The present invention will be further described with reference to the following examples. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention.

The invention is further described below by way of specific embodiments in which the volumetric liquid hourly space velocity is defined as: