CN105859513A - Production method for chloromethane - Google Patents
Production method for chloromethane Download PDFInfo
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- CN105859513A CN105859513A CN201610342717.3A CN201610342717A CN105859513A CN 105859513 A CN105859513 A CN 105859513A CN 201610342717 A CN201610342717 A CN 201610342717A CN 105859513 A CN105859513 A CN 105859513A
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- chloromethanes
- chloromethane
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- production method
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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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/16—Preparation of halogenated hydrocarbons by replacement by halogens of hydroxyl groups
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a production method for chloromethane, and relates to the field of raw chemical material production. The production method includes the following steps that 1, methyl alcohol and ammonium chloride are heated in a reaction vessel with an aluminum oxide catalyst to generate a mixture of chloromethane, ammonia and water; 2, the mixture generated in the step 1 is sent to a chilling device and chilled and separated to sequentially enter an acid pickling tower and a sulfuric acid drying system, and is compressed to prepare crude chloromethane; 3, the crude chloromethane obtained in the step 2 is sent to a refining tower, heavy components are separated from the tower bottom, light components are evaporated to a tower top, separation between the chloromethane and methane is achieved accordingly, and the high-purity chloromethane is obtained; the molar ratio of the ammonium chloride to the methyl alcohol is (1.1-1.5):1. The production method for the chloromethane is free of pollution in environment, a single tower distillation mode is adopted, separation between the chloromethane and methane is achieved in the same refining tower, the high-purity chloromethane is obtained, the content of the chloromethane is increased while the investment of a device is not largely increased, and the economic benefits are increased.
Description
Technical field
The present invention relates to industrial chemicals production field, be specifically related to the production method of a kind of chloromethanes.
Background technology
Along with the development of organosilicon industry and continually developing of chloromethanes downstream product, the demand to chloromethanes commodity amount
Increasing, but present stage most chloromethanes process units is intended only as corollary apparatus and produces, the difficult quality of chloromethanes
Reaching market demands, present stage synthesis chloromethanes all uses gas and solid phase catalytic and liquid catalytic, raw at gas and solid phase catalytic
In production. art, there are two kinds of production methods: a kind of is through the thick chloromethanes of catalytic reaction after Quench, successively through washing, alkali cleaning, sulfur
The dried compression of acid prepares chloromethanes, and CN1686981 discloses a kind of chloromethanes preparation method, and it is former with methanol and hydrogen chloride
Material, in the presence of active catalyst, at 260 ~ 320 DEG C, under the conditions of 0.2 ~ 0.6 Mpa, gas phase reaction generates chloromethanes and water, goes out anti-
Answering device pyroreaction gas after dilute hydrochloric acid Quench, after separation, (condensed fluid is that dilute hydrochloric acid is for reaction gas to the condensation of dampness condensed device
Quench), sulphuric acid is dried, compression condensation prepares chloromethanes, and CN1515528 discloses liquid catalytic pressurization and produces the work of chloromethanes
Skill, after hydrogen chloride and methanol being proportioned, equipped with in the tank reactor of catalyst, closes under uniform temperature and pressure
Become chloromethanes, and use acid/washing, alkali cleaning to remove unreacted methanol and hydrogen chloride, and use concentrated sulphuric acid washing removing remnants
Moisture content and reaction by-product dimethyl ether；Methyl chloride gas purified, dried obtains highly purified liquid by compression, condensation
Body chloromethanes product, this production method waste water, salkali waste discharge capacity are big, pollute height, and the chloromethanes content of production is low, typically exists
Between 97% ~ 99%, it is impossible to meet high-end market needs.
Summary of the invention
Instant invention overcomes above-mentioned shortcoming, and the production method of a kind of chloromethanes is provided.
It is an object of the invention to provide the production method of a kind of chloromethanes, comprise the following steps:
1) methanol and ammonium chloride add the mixing being thermally generated chloromethanes, ammonia and water in equipped with the reactor of aluminium oxide catalyst
Thing；2) mixture generated in step 1) is sent into chiller, after Quench separates, successively enter pickling tower and sulphuric acid is dried and is
System, prepares thick chloromethanes after compression；3) by step 2) in the thick chloromethanes that obtains send into treating column, isolate heavy constituent at the bottom of tower,
Light component is evaporated to tower top, thus realizes chloromethanes and separate with ammonia, obtains highly purified chloromethanes；State ammonium chloride and methanol
Mol ratio be 1.1 ~ 1.5:1.
Preferably, in described step 1), the reaction temperature of reactor is 210 ~ 280 DEG C.
Preferably, in described step 1), the reaction pressure of reactor is 0.20 ~ 0.35 Mpa.
Preferably, described step 3) in thick chloromethanes when entering chloromethanes treating column, tower top pressure is 0.50 Mpa, at the bottom of tower
Pressure is 0.60 Mpa.
Preferably, described step 3) in thick chloromethanes when entering chloromethanes treating column, tower top temperature 40 DEG C, column bottom temperature 60
℃。
The invention has the beneficial effects as follows: the production method of the chloromethanes of the present invention, environmentally safe, have employed single column essence
The mode evaporated, realizes chloromethanes in same rectifying column and separates with methane, obtains highly purified chloromethanes, does not rolls up
While equipment investment, improve the content of chloromethanes, increase economic benefit.
Detailed description of the invention
The production method of chloromethanes comprises the following steps:
1) methanol and ammonium chloride add the mixing being thermally generated chloromethanes, ammonia and water in equipped with the reactor of aluminium oxide catalyst
Thing；
2) mixture generated in step 1) is sent into chiller, after Quench separates, successively enter pickling tower and sulphuric acid is dried and is
System, prepares thick chloromethanes after compression；
3) by step 2) in the thick chloromethanes that obtains send into treating column, isolate heavy constituent at the bottom of tower, light component is evaporated to tower top, from
And realize chloromethanes and separate with ammonia, obtain highly purified chloromethanes；Ammonium chloride is 1.1 ~ 1.5:1 with the mol ratio of methanol；
In step 1), the reaction temperature of reactor is 210 ~ 280 DEG C；In step 1), the reaction pressure of reactor is 0.20 ~ 0.35 Mpa；
Step 3) in thick chloromethanes when entering chloromethanes treating column, tower top pressure is 0.50 Mpa, and tower bottom pressure is 0.60 Mpa；Step
3) when in, thick chloromethanes enters chloromethanes treating column, tower top temperature 40 DEG C, column bottom temperature 60 DEG C.
The ultimate principle of the present invention and principal character and advantages of the present invention, the technology of the industry have more than been shown and described
Personnel, it should be appreciated that the present invention is not restricted to the described embodiments, simply illustrating this described in above-described embodiment and description
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, and these become
Change and improvement both fall within scope of the claimed invention, claimed scope by appending claims and
Equivalent defines.
Claims (5)
- The production method of a kind of chloromethanes the most as claimed in claim 1, it is characterised in that comprise the following steps:1) methanol and ammonium chloride add the mixing being thermally generated chloromethanes, ammonia and water in equipped with the reactor of aluminium oxide catalyst Thing；2) mixture generated in step 1) is sent into chiller, after Quench separates, successively enter pickling tower and sulphuric acid is dried and is System, prepares thick chloromethanes after compression；3) by step 2) in the thick chloromethanes that obtains send into treating column, isolate heavy constituent at the bottom of tower, Light component is evaporated to tower top, thus realizes chloromethanes and separate with ammonia, obtains highly purified chloromethanes；State ammonium chloride and methanol Mol ratio be 1.1 ~ 1.5:1.
- The production method of a kind of chloromethanes the most according to claim 1, it is characterised in that reactor in described step 1) Reaction temperature is 210 ~ 280 DEG C.
- The production method of a kind of chloromethanes the most according to claim 1, it is characterised in that reactor in described step 1) Reaction pressure is 0.20 ~ 0.35 Mpa.
- The production method of a kind of chloromethanes the most according to claim 1, it is characterised in that described step 3) in thick chloromethanes When entering chloromethanes treating column, tower top pressure is 0.50 Mpa, and tower bottom pressure is 0.60 Mpa.
- The production method of a kind of chloromethanes the most according to claim 1, it is characterised in that described step 3) in thick chloromethanes When entering chloromethanes treating column, tower top temperature 40 DEG C, column bottom temperature 60 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610342717.3A CN105859513A (en) | 2016-05-23 | 2016-05-23 | Production method for chloromethane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610342717.3A CN105859513A (en) | 2016-05-23 | 2016-05-23 | Production method for chloromethane |
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| Publication Number | Publication Date |
|---|---|
| CN105859513A true CN105859513A (en) | 2016-08-17 |
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| CN201610342717.3A Pending CN105859513A (en) | 2016-05-23 | 2016-05-23 | Production method for chloromethane |
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Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2755316A (en) * | 1951-12-29 | 1956-07-17 | Olin Mathieson | Reaction of organic compounds with ammonium chloride |
| US2755311A (en) * | 1951-12-29 | 1956-07-17 | Olin Mathieson | Production of organic chlorides by reaction of organic compound with ammonium chloride |
| US3315441A (en) * | 1965-07-15 | 1967-04-25 | Du Pont | Process for separating ammonia from methyl chloride |
| JPS57130930A (en) * | 1981-02-05 | 1982-08-13 | Mitsubishi Gas Chem Co Inc | Preparation of methyl chloride and methylamine |
| JPS58194823A (en) * | 1982-05-10 | 1983-11-12 | Mitsubishi Gas Chem Co Inc | Preparation of methyl chloride and ammonia |
| CN1069720A (en) * | 1991-08-22 | 1993-03-10 | 陶氏化学公司 | The method of hydrohalogenation of hydrocarbons and catalyzer |
| CN1686981A (en) * | 2005-04-21 | 2005-10-26 | 江苏梅兰化工股份有限公司 | Preparation method of methane chloride |
| CN1686983A (en) * | 2005-04-21 | 2005-10-26 | 江苏梅兰化工股份有限公司 | Method fo rproducing high pure methane chloride |
| CN101134708A (en) * | 2007-10-12 | 2008-03-05 | 山东东岳氟硅材料有限公司 | Production technique of high-purity methane chloride |
| CN101574657A (en) * | 2009-06-18 | 2009-11-11 | 河北科技大学 | Catalyst for preparing chloromethane and ammonia gas and preparation method thereof |
| CN102234217A (en) * | 2010-04-23 | 2011-11-09 | 天津市泰源工业气体有限公司 | Technology for producing methyl chloride by ammonium chloride method |
| CN202113843U (en) * | 2011-06-22 | 2012-01-18 | 河北科技大学 | Device for preparing chloromethane and ammonia |
| CN102408301A (en) * | 2011-11-30 | 2012-04-11 | 河北科技大学 | Method for preparing methyl chloride and ammonia by using ammonium chloride and methanol |
| CN203159238U (en) * | 2013-03-26 | 2013-08-28 | 北京烨晶科技有限公司 | Equipment for jointly producing ammonium sulfate, hydrogen chloride and methane chloride |
-
2016
- 2016-05-23 CN CN201610342717.3A patent/CN105859513A/en active Pending
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2755316A (en) * | 1951-12-29 | 1956-07-17 | Olin Mathieson | Reaction of organic compounds with ammonium chloride |
| US2755311A (en) * | 1951-12-29 | 1956-07-17 | Olin Mathieson | Production of organic chlorides by reaction of organic compound with ammonium chloride |
| US3315441A (en) * | 1965-07-15 | 1967-04-25 | Du Pont | Process for separating ammonia from methyl chloride |
| JPS57130930A (en) * | 1981-02-05 | 1982-08-13 | Mitsubishi Gas Chem Co Inc | Preparation of methyl chloride and methylamine |
| JPS58194823A (en) * | 1982-05-10 | 1983-11-12 | Mitsubishi Gas Chem Co Inc | Preparation of methyl chloride and ammonia |
| CN1069720A (en) * | 1991-08-22 | 1993-03-10 | 陶氏化学公司 | The method of hydrohalogenation of hydrocarbons and catalyzer |
| CN1686981A (en) * | 2005-04-21 | 2005-10-26 | 江苏梅兰化工股份有限公司 | Preparation method of methane chloride |
| CN1686983A (en) * | 2005-04-21 | 2005-10-26 | 江苏梅兰化工股份有限公司 | Method fo rproducing high pure methane chloride |
| CN101134708A (en) * | 2007-10-12 | 2008-03-05 | 山东东岳氟硅材料有限公司 | Production technique of high-purity methane chloride |
| CN101574657A (en) * | 2009-06-18 | 2009-11-11 | 河北科技大学 | Catalyst for preparing chloromethane and ammonia gas and preparation method thereof |
| CN102234217A (en) * | 2010-04-23 | 2011-11-09 | 天津市泰源工业气体有限公司 | Technology for producing methyl chloride by ammonium chloride method |
| CN202113843U (en) * | 2011-06-22 | 2012-01-18 | 河北科技大学 | Device for preparing chloromethane and ammonia |
| CN102408301A (en) * | 2011-11-30 | 2012-04-11 | 河北科技大学 | Method for preparing methyl chloride and ammonia by using ammonium chloride and methanol |
| CN203159238U (en) * | 2013-03-26 | 2013-08-28 | 北京烨晶科技有限公司 | Equipment for jointly producing ammonium sulfate, hydrogen chloride and methane chloride |
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Application publication date: 20160817 |