阅读说明：本技术 一种反应精馏制备生产硫酰氯的工艺 (Process for preparing sulfuryl chloride by reactive distillation ) 是由 刘辉 刘春江 谢省宾 郭凯 项文雨 魏东旭 韦昌鹏 付娜 李月坤 于 2020-08-31 设计创作，主要内容包括：本发明提出一种反应精馏制备生产硫酰氯的工艺,包括反应精馏塔、再沸器和冷凝器；其特征是反应精馏塔由精馏段、反应段和提馏段组成；反应段装有催化精馏模块,催化剂为活性炭或樟等；反应精馏塔塔底设有再沸器、塔顶设有冷凝器。二氧化硫从反应精馏塔塔反应段的上部进料,氯气从反应精馏塔塔反应段下部进料,产品硫酰氯塔底采出,塔顶为采出过量的氯气,二氧化硫转化率超过93.0％,硫酰氯纯度在99.0％以上。本发明可以实现硫酰氯连续化生产、流程简单、设备投资少、提高了硫酰氯生产工艺的经济效益。(The invention provides a process for preparing sulfuryl chloride by reactive distillation, which comprises a reactive distillation tower, a reboiler and a condenser; it is characterized in that the reaction rectifying tower consists of a rectifying section, a reaction section and a stripping section; the reaction section is provided with a catalytic rectification module, and the catalyst is active carbon or camphor wood and the like; the tower bottom of the reaction rectifying tower is provided with a reboiler, and the tower top is provided with a condenser. Sulfur dioxide is fed from the upper part of the reaction section of the reaction rectifying tower, chlorine is fed from the lower part of the reaction section of the reaction rectifying tower, the product sulfuryl chloride is extracted from the bottom of the tower, the excessive chlorine is extracted from the top of the tower, the conversion rate of the sulfur dioxide is over 93.0 percent, and the purity of the sulfuryl chloride is over 99.0 percent. The invention can realize the continuous production of the sulfuryl chloride, has simple flow and less equipment investment and improves the economic benefit of the sulfuryl chloride production process.)

1. A process for preparing sulfuryl chloride by reactive distillation comprises a reactive distillation tower, which is characterized in that the reactive distillation tower consists of a distillation section, a reaction section and a stripping section; the reaction section is provided with a catalytic rectification module, and the catalyst is active carbon or camphor; the tower bottom of the reaction rectifying tower is provided with a reboiler, and the tower top is provided with a condenser; sulfur dioxide is fed from the upper part of the reaction section of the reaction rectifying tower, chlorine is fed from the lower part of the reaction section of the reaction rectifying tower, the product sulfuryl chloride is extracted from the bottom of the reaction rectifying tower, and the excessive chlorine is extracted from the top of the reaction rectifying tower.

2. The process for preparing sulfuryl chloride by reactive distillation as claimed in claim 1, wherein sulfur dioxide is fed from the upper part of the reaction section of the reactive distillation column, and chlorine gas is fed from the lower part of the reaction section of the reactive distillation column.

3. The process for preparing sulfuryl chloride by reactive distillation according to claim 1, wherein the reactive distillation tower is operated continuously under normal pressure or pressurization, and the temperature of the reaction section is-20 to 60 ℃.

4. The process for preparing sulfuryl chloride by reactive distillation as claimed in claim 1, wherein the top gas phase is condensed by a condenser, and the condensed liquid sulfur dioxide is fed into the reactive distillation column as reflux.

Technical Field

The invention belongs to the field of fine chemical production, and particularly relates to a production process for producing sulfuryl chloride by reactive distillation.

Background

Sulfuryl chloride is mainly used as a chlorinating agent, a sulfonating agent and a chlorosulfonating agent for organic synthesis, such as the chlorination of aromatic compounds, the chlorination of carboxylic acids and the chlorination of other various organic and inorganic compounds; also can be used for preparing medicinal products, dyes, surfactants, etc. Therefore, the application market and the development prospect are very wide. One of the production methods is a chlorination method, and the reaction formula is as follows:

the domestic preparation method mainly comprises three methods: (1) reacting gasified sulfur dioxide with chlorine in the presence of an active carbon catalyst, and condensing generated sulfuryl chloride to obtain a sulfuryl chloride finished product; (2) active carbon or camphor is used as a catalyst to make sulfur dioxide and chlorine react directly to prepare sulfuryl chloride; (3) the trifluorotrichloroethane (CFC-113a or R113a) and sulfur trioxide are reacted through fixed bed catalysis. In any of the preparation methods, a fixed bed type reactor is basically adopted, and after the reaction is finished, the product needs to be purified and separated by rectification, so that the investment is large and the occupied area is large.

Disclosure of Invention

The invention aims to provide a process for preparing sulfuryl chloride by reactive distillation, which has the advantages of continuous operation, simple process flow, high product yield and stable quality.

The invention utilizes the reactive distillation technology to separate the generated product out of the reaction system while the chemical reaction is carried out, thereby promoting the reaction. Therefore, the process can effectively improve the yield of the product and reduce the cost of subsequent separation.

The invention adopts active carbon or camphor wood and the like as the catalyst, and has the advantages of less equipment investment, simple process flow, high economic benefit and the like.

The invention is realized by adopting the following technical scheme: a process for preparing sulfuryl chloride by reactive distillation comprises the following steps: a reactive distillation column, a reboiler and a condenser; it is characterized in that the reaction rectifying tower consists of a rectifying section, a reaction section and a stripping section; the reaction section is provided with a catalytic rectification module, and the catalyst is active carbon or camphor wood and the like; the tower bottom of the reaction rectifying tower is provided with a reboiler, and the tower top is provided with a condenser. Sulfur dioxide is fed from the upper part of the reaction section of the reaction rectifying tower, chlorine is fed from the lower part of the reaction section of the reaction rectifying tower, the product sulfuryl chloride is extracted from the bottom of the reaction rectifying tower, and the excessive chlorine is extracted from the top of the reaction rectifying tower.

Sulfur dioxide, also known as sulfurous anhydride, has the chemical formula of SO₂64.06 molecular weight, colorless gas, strong pungent odor, melting point-75.5 deg.C, boiling point-10 deg.C, and relative density of 2.26kg/m³. Chlorine gas of the formula Cl₂The molecular weight is 71, the toxic gas is yellow green at normal temperature and normal pressure, has strong pungent smell, the melting point is-101 ℃, the boiling point is-34 ℃, and the relative density is 3.21kg/m³. Sulfuryl chloride is also known as "dichlorosulfur dioxide". Chemical formula SO₂Cl₂Molecular weight 134.97, colorless liquid. Has strong pungent smell. Melting point-54.1 deg.C, boiling point 69.1 deg.C, relative density 1.667kg/m³。

The invention provides a process for preparing sulfuryl chloride by reactive distillation, which comprises the following steps:

(1) the reaction rectifying tower consists of a rectifying section, a reaction section and a stripping section, the reaction rectifying section is provided with a catalytic rectifying module, and the catalyst is active carbon or camphor and the like;

(2) feeding sulfur dioxide from the upper part of the reaction section of the reaction rectifying tower, and feeding chlorine from the lower part of the reaction section of the reaction rectifying tower;

(3) the reaction rectifying tower is operated continuously under normal pressure or pressurization, and the temperature of a reaction section is-20-60 ℃;

(4) condensing the top gas phase by a condenser, feeding the condensed liquid sulfur dioxide into a reaction rectifying tower as reflux, and extracting or recycling chlorine;

(5) the product sulfuryl chloride is extracted from the bottom of the tower.

The invention has the advantages that:

the invention organically couples the reaction process and the rectification separation process together, and separates the generated product out of the reaction system while the chemical reaction is carried out, thereby promoting the reaction, realizing that the conversion rate of sulfur dioxide exceeds 93.0 percent and the purity of sulfuryl chloride is more than 99.0 percent. The invention realizes continuous operation, simple flow, less equipment investment and no waste water, and improves the economic benefit of the sulfuryl chloride production process.

Drawings

FIG. 1: flow chart of the device

R1-reaction rectifying tower, E1-reaction rectifying tower reboiler, E2-reaction rectifying condenser, 1-sulfur dioxide, 2-chlorine, 3-reaction rectifying tower gas phase, 4-reaction rectifying tower reflux liquid phase and 5-sulfuryl chloride.

Detailed Description

The invention is described in further detail below with reference to the accompanying drawings:

as shown in fig. 1:

a process for preparing sulfuryl chloride by reactive distillation comprises the following steps: a reaction rectifying tower R1, a reaction rectifying tower reboiler E1 and a reaction rectifying condenser E2. The device is characterized in that a reaction rectifying tower (R1) consists of a rectifying section, a reaction section and a stripping section, wherein the reaction rectifying section is provided with a catalytic rectifying module, and a catalyst is active carbon or camphor and the like; sulfur dioxide (1) is fed from the upper part of the reaction section of the reaction rectifying tower (R1), and chlorine (2) is fed from the lower part of the reaction section of the reaction rectifying tower (R1); the reaction rectifying tower (R1) is continuously operated under normal pressure or pressurization, and the temperature of a reaction section is-20-60 ℃; condensing a gas phase (3) at the top of the reactive distillation tower (R1) by a condenser, taking the condensed liquid-phase sulfur dioxide as reflux to enter the reactive distillation tower, and extracting or recycling chlorine (4); the sulfuryl chloride (5) in the liquid phase at the bottom of the tower is taken out as a product.

The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples. It will be appreciated by those skilled in the art that the present invention encompasses all alternatives, modifications and equivalents as may be included within the scope of the claims.