CN110862296B - Method for separating reaction product in chloromethane production process - Google Patents
Method for separating reaction product in chloromethane production process Download PDFInfo
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- CN110862296B CN110862296B CN201911069843.6A CN201911069843A CN110862296B CN 110862296 B CN110862296 B CN 110862296B CN 201911069843 A CN201911069843 A CN 201911069843A CN 110862296 B CN110862296 B CN 110862296B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
- C07C17/386—Separation; Purification; Stabilisation; Use of additives by distillation with auxiliary compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a separation method of reaction products in the production process of chloromethane, which adopts an absorption rectification composite tower for treatment; directly feeding the reaction product into the middle part of an absorption rectification composite tower, taking water as an absorbent at the tower top, and stripping methanol and methyl chloride absorbed by the water to the tower top by means of heating and stripping of a reboiler at the tower bottom, so as to obtain a gas containing hydrochloric acid, methyl chloride and water at the tower top; dilute hydrochloric acid without methanol and chloromethane is obtained in the tower bottom. The invention realizes two process processes of absorption and rectification simultaneously in one tower, realizes the complete separation of hydrogen chloride gas, methanol and chloromethane, has simple process, high separation efficiency, low energy consumption, environmental protection and convenient industrial production.
Description
Technical Field
The invention relates to the technical field of reaction product separation, in particular to a method for separating reaction products in a chloromethane production process.
Background
The monochloromethane is commonly called chloromethane, is mainly used for preparing raw material methylchlorosilane monomers in the organosilicon industry, is also used for producing methylcellulose, quaternary ammonium compounds, pesticides, solvents and emulsifiers of organic compounds and the like, can also be used as a medical anesthetic, and is also an intermediate raw material of methane chloride. With the rapid development of the industry of organosilicon and methane chloride in recent years, most domestic organosilicon and methane chloride production enterprises are matched with own methyl chloride devices to meet the production requirements because the methyl chloride is limited in transportation.
The liquid phase catalytic method is a main production method of methane chloride in China, namely methanol gas and hydrogen chloride gas are used as raw materials and react under the action of a liquid catalyst to generate the methane chloride and water, and the reaction equation is as follows: CH (CH)3OH+HCl＝＝CH3Cl+H2In this reaction, the reaction product contains unreacted methanol and a hydrochloric acid solution formed by dissolving hydrogen chloride in water, in addition to methyl chloride and water, which are formed as a result of an excess of hydrogen chloride as a reaction raw material.
The current general separation process after reaction is as follows: the gas after reaction is condensed and then divided into a gas phase and a liquid phase, the separated gas phase is mainly methyl chloride which contains a certain amount of methanol, water and hydrogen chloride, the gas phase is treated in downstream processes such as alkaline washing, water washing and the like, the separated liquid is mainly hydrochloric acid solution which also contains a certain amount of methanol and methyl chloride, and dilute hydrochloric acid solution is obtained after further treatment. In the process, organic matters such as methanol, chloromethane and the like in a gas phase and a liquid phase are not thoroughly separated, the gas phase and the liquid phase need to be respectively treated, the process is complex, and the energy consumption is high. Hydrochloric acid is contained in the two phases, so that subsequent equipment is corroded, and the hydrochloric acid in the gas is neutralized by using alkali liquor, so that the environment-friendly treatment cost is increased, and the waste of hydrogen chloride is caused.
Disclosure of Invention
The invention aims to provide a method for separating reaction products in the production process of methyl chloride, aiming at the technical defects in the prior art.
The technical scheme adopted for realizing the purpose of the invention is as follows:
a separation method of reaction products in the production process of methyl chloride adopts an absorption rectification composite tower for treatment; directly feeding the reaction product into the middle part of an absorption rectification composite tower, taking water as an absorbent at the tower top, and stripping methanol and methyl chloride absorbed by the water to the tower top by means of heating and stripping of a reboiler at the tower bottom, so as to obtain a gas containing hydrochloric acid, methyl chloride and water at the tower top; and obtaining dilute hydrochloric acid without chloromethane at the tower bottom.
Wherein the reaction product is reaction gas from the liquid phase catalytic reactor or a gas-liquid mixture formed after heat exchange.
Preferably, the operating pressure of the absorption and rectification composite tower is as follows: atmospheric pressure-350 kpa, overhead temperature: 84-121 ℃, and the temperature of the tower kettle is 106-; the feeding amount of the absorbent is 15 to 45 percent of the feeding amount of the reaction product according to the mass ratio.
The invention realizes two process processes of absorption and rectification simultaneously in one tower, realizes the complete separation of hydrogen chloride gas, methanol and chloromethane, has simple process, high separation efficiency, low energy consumption, environmental protection and convenient industrial production.
Drawings
FIG. 1 is a process diagram of the process for the separation of reaction products in the production of methyl chloride according to the invention.
In the figure: t101: an absorption rectification composite tower; e101: a reboiler; s1: a reaction product; s2: an absorbent; s3: overhead gas; s4: dilute hydrochloric acid solution
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in fig. 1, in the separation method of reaction products in the methyl chloride production process of the present invention, water is adopted as an absorbent, two process processes of absorption and rectification are simultaneously realized in an absorption rectification composite tower T101, reaction gas from a liquid phase catalytic reactor or a gas-liquid mixture formed after heat exchange, the formed reaction product S1 directly enters the middle part of the absorption rectification composite tower T101, water is adopted as the absorbent S2 at the tower top, methanol and methyl chloride absorbed by water are stripped to the tower top by the tower bottom due to the heating stripping action of a tower bottom reboiler E101, and the tower top which obtains methyl chloride, methanol and water without hydrochloric acid produces S3; the diluted hydrochloric acid S4 without methyl chloride is obtained in the tower bottom.
Operating pressure: atmospheric pressure-350 kpa (absolute), overhead temperature: 84-121 ℃, tower temperature 106-: the feeding amount of the absorbent is 15 to 45 mass% of the feeding amount of the reaction product.
The following examples are given below, taking a 5000 ton/year methyl chloride plant as an example.
Example 1:
950kg/h of reaction product, gas phase feed, composition of reaction gas (mass percent): 23.6% of water, 6.7% of hydrogen chloride, 3.6% of methanol, 66.0% of methyl chloride, 0.1% of dimethyl ether, T101 normal pressure operation, tower top temperature: 84 ℃, 106 ℃ and 143kg/h of absorbent water. The reboiler E101 consumes 105kw, and the obtained tower top S3 consists of the following components in percentage by mass: 2.56% of water, 5.10% of methanol, 92.2% of chloromethane, 0.14% of dimethyl ether and no hydrogen chloride; the tower bottom S3 comprises the following components in percentage by mass: 15.2% dilute hydrochloric acid (methanol and methyl chloride excluded).
Example 2:
950kg/h of reaction product, gas phase feed, composition of reaction gas (mass percent): 22.5% of water, 8.8% of hydrogen chloride, 5.5% of methanol, 63.2% of methyl chloride, 160kpa (absolute) of operating pressure of T101, temperature at the top of the column: 88 ℃, 119 ℃ and 426kg/h of absorbent water. The reboiler E101 consumes 149kw, and the obtained tower top S3 consists of the following components in percentage by mass: 1.0% of water, 7.8% of methanol and 91.2% of chloromethane, and hydrogen chloride is not contained; the tower bottom S3 comprises the following components in percentage by mass: 11.6% diluted hydrochloric acid (methanol 10ppm, methyl chloride free).
Example 3:
gas-liquid two-phase feeding, reaction product 950kg/h, reaction gas composition (mass percent): 22.5% of water, 8.8% of hydrogen chloride, 5.5% of methanol, 63.2.0% of methyl chloride, 350kpa (absolute) of operating pressure of T101, temperature at the top of the column: 121 ℃, 143 ℃ and 426kg/h of absorbent water. The energy consumption of a reboiler E101 is 283kw, and the composition of the obtained tower top S3 (mass percent) is as follows: 6.8% of water, 4.9% of methanol and 88.3% of chloromethane, and hydrogen chloride is not contained; the tower bottom S3 comprises the following components in percentage by mass: 9.6% diluted hydrochloric acid (methanol 15ppm, methyl chloride free).
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (3)
1. A separation method of reaction products in the production process of methyl chloride is characterized in that an absorption rectification composite tower is adopted for treatment; directly feeding the reaction product into the middle part of an absorption rectification composite tower, taking water as an absorbent at the tower top, and stripping methanol and methyl chloride absorbed by the water to the tower top by means of heating and stripping of a reboiler at the tower bottom, so as to obtain a gas containing hydrochloric acid, methyl chloride and water at the tower top; and obtaining dilute hydrochloric acid without chloromethane at the tower bottom.
2. The method for separating reaction products in the production of methyl chloride according to claim 1, wherein the reaction products are reaction gases from a liquid-phase catalytic reactor or gas-liquid mixtures formed by heat exchange.
3. The method for separating reaction products in the production of methyl chloride according to claim 1, wherein the operating pressure of the absorption-rectification composite tower is as follows: atmospheric pressure-350 kpa, overhead temperature: 84-121 ℃, and the temperature of the tower kettle is 106-; the feeding amount of the absorbent is 15 to 45 percent of the feeding amount of the reaction product according to the mass ratio.
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Citations (11)
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|---|---|---|---|---|
| JPH04368344A (en) * | 1991-06-13 | 1992-12-21 | Shin Etsu Chem Co Ltd | Separation and purification of methyl chloride |
| CN104058924A (en) * | 2014-06-25 | 2014-09-24 | 鲁西化工集团股份有限公司硅化工分公司 | Method for preparing chloromethane by utilizing alcohol-containing hydrochloric acid |
| CN104230650A (en) * | 2013-06-21 | 2014-12-24 | 徐家乐 | Process of preparing chloromethane by photo-chlorination process |
| CN104926595A (en) * | 2015-05-15 | 2015-09-23 | 大连理工大学 | Separation process of removing dimethyl ether impurities in chloromethane through water absorption |
| CN108484352A (en) * | 2018-04-09 | 2018-09-04 | 浙江巨化技术中心有限公司 | A kind of method that methanol hydrogen chloride prepares chloromethanes |
| CN109081767A (en) * | 2018-09-30 | 2018-12-25 | 南京佳华工程技术有限公司 | A kind of the synthesis rectification technique and its equipment of monochloro methane |
| CN109206291A (en) * | 2017-07-04 | 2019-01-15 | 天津中福泰克化工科技有限公司 | A kind of separation method of chloromethanes-dimethyl ether |
| CN109232166A (en) * | 2018-11-16 | 2019-01-18 | 四川天科技股份有限公司 | A kind of carbonated hydrogen chloride gas produces monochloro methane Processes and apparatus |
| CN109574790A (en) * | 2019-01-16 | 2019-04-05 | 杭州东日节能技术有限公司 | Chloromethanes is synthesized without by-product hydrochloric acid technique and its equipment |
| CN110026069A (en) * | 2019-04-11 | 2019-07-19 | 天津大学 | A kind of concentrated hydrochloric acid reactive distillation absorbs the technique and system of melamine tail gas |
| CN110204417A (en) * | 2019-06-21 | 2019-09-06 | 江苏明珠硅橡胶材料有限公司 | A kind of method of monochloro methane purification |
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- 2019-11-05 CN CN201911069843.6A patent/CN110862296B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04368344A (en) * | 1991-06-13 | 1992-12-21 | Shin Etsu Chem Co Ltd | Separation and purification of methyl chloride |
| CN104230650A (en) * | 2013-06-21 | 2014-12-24 | 徐家乐 | Process of preparing chloromethane by photo-chlorination process |
| CN104058924A (en) * | 2014-06-25 | 2014-09-24 | 鲁西化工集团股份有限公司硅化工分公司 | Method for preparing chloromethane by utilizing alcohol-containing hydrochloric acid |
| CN104926595A (en) * | 2015-05-15 | 2015-09-23 | 大连理工大学 | Separation process of removing dimethyl ether impurities in chloromethane through water absorption |
| CN109206291A (en) * | 2017-07-04 | 2019-01-15 | 天津中福泰克化工科技有限公司 | A kind of separation method of chloromethanes-dimethyl ether |
| CN108484352A (en) * | 2018-04-09 | 2018-09-04 | 浙江巨化技术中心有限公司 | A kind of method that methanol hydrogen chloride prepares chloromethanes |
| CN109081767A (en) * | 2018-09-30 | 2018-12-25 | 南京佳华工程技术有限公司 | A kind of the synthesis rectification technique and its equipment of monochloro methane |
| CN109232166A (en) * | 2018-11-16 | 2019-01-18 | 四川天科技股份有限公司 | A kind of carbonated hydrogen chloride gas produces monochloro methane Processes and apparatus |
| CN109574790A (en) * | 2019-01-16 | 2019-04-05 | 杭州东日节能技术有限公司 | Chloromethanes is synthesized without by-product hydrochloric acid technique and its equipment |
| CN110026069A (en) * | 2019-04-11 | 2019-07-19 | 天津大学 | A kind of concentrated hydrochloric acid reactive distillation absorbs the technique and system of melamine tail gas |
| CN110204417A (en) * | 2019-06-21 | 2019-09-06 | 江苏明珠硅橡胶材料有限公司 | A kind of method of monochloro methane purification |
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