CN107814683A - A kind of production technology of dichloromethane - Google Patents
A kind of production technology of dichloromethane Download PDFInfo
- Publication number
- CN107814683A CN107814683A CN201711093639.9A CN201711093639A CN107814683A CN 107814683 A CN107814683 A CN 107814683A CN 201711093639 A CN201711093639 A CN 201711093639A CN 107814683 A CN107814683 A CN 107814683A
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- CN
- China
- Prior art keywords
- dichloromethane
- production technology
- shell
- chloromethanes
- drying
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- 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
- C07C17/10—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
-
- 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
- C07C17/389—Separation; Purification; Stabilisation; Use of additives by adsorption on solids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00162—Controlling or regulating processes controlling the pressure
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a kind of production technology of dichloromethane, comprise the following steps：1) using chloromethanes and liquid chlorine as raw material, using shell and tube fluidized-bed reactor as consersion unit, using calcium chloride as catalyst, wherein, water under high pressure is passed through in the tubulation of shell and tube fluid bed, technical grade dichloromethane is prepared；2) after taking active fruit shell carbon DV11 drying and dehydratings and cooling down, it is fitted into glass column；3) the technical grade dichloromethane being prepared by step 1) is from top to bottom done into Adsorption processing through glass column, produces chromatographic grade dichloromethane.The simple production process of dichloromethane is reasonable in the present invention, and product qualification rate is high, uses catalyst, side reaction is not produced, improves the rate of recovery of target product, significantly digests my company's chloromethanes resource, by being processed further lifting added value, the core competitive power of glyphosate industry is improved.
Description
Technical field
The present invention relates to chemical products preparing technical field, and in particular to a kind of production technology of dichloromethane.
Background technology
Methane chloride industry is the industry that an application field is wide, technology-intensive degree and intensive capital degree is higher.Dichloro
Methane has good dissolving power, is that conventional industrial solvent poisonings are small, non-flame properties low boiling point solvent, to many resins, stone
Wax and fat all have good solvability, are a kind of widely used industrial solvents.The main production line of dichloromethane
It is the chlorination of methane or chloromethanes.Its production method uses methane or chloromethanes high temperature gas phase thermal chlorination earliest, later development
Photochemical chlorination method, methane process for oxychlorination, chloromethanes low temperature liquid phase free radical trigger chloridising to produce the technology of chloromethane.Mesh
Before to be widely used in industrial be thermal chlorination.Reactor types have internal-circulation type, heat accumulating type, shell and tube and ebullated bed etc. more
Kind pattern.
My company has glyphosate products to have abundant chloromethanes resource, while also has abundant chlorine resource, sweet to carry grass
The synthesized competitiveness of phosphine, also being laid a solid foundation to the macro-goal of new material development for company, now develops dichloromethane
Production technology.
The content of the invention
First purpose of the present invention is to provide a kind of production technology of dichloromethane, comprised the following steps：
1) using chloromethanes and liquid chlorine as raw material, using shell and tube fluidized-bed reactor as consersion unit,
Using calcium chloride as catalyst, reaction equation is as follows：
Main reaction：
CH3Cl+Cl2→CH2Cl2+HCl
Side reaction：
CH2Cl2+Cl2→CHCl3+HCl
CHCl3+Cl2→CCl4+HCl
Wherein, water under high pressure is passed through in the tubulation of shell and tube fluid bed, technical grade dichloromethane is prepared；
2) after taking active fruit shell carbon DV11 drying and dehydratings and cooling down, it is fitted into glass column；
3) the technical grade dichloromethane being prepared by step 1) is from top to bottom done into Adsorption processing through glass column,
Produce chromatographic grade dichloromethane.
Preferably, drying and dehydrating is dehydrated using centrifugation in the step 2).
Preferably, drying is carried out in drying oven in the step 2).
Preferably, drying temperature is 125 DEG C in the step 2).
Preferably, in the step 2) dry after dichloromethane water content control mass percentage content≤
0.01%.
Second object of the present invention is to provide a kind of application of production technology of dichloromethane in terms of agricultural chemicals preparation.
Technique advantages of simple, product qualification rate is high, using catalyst, does not produce side reaction, improves the recovery of target product
Rate, while shell and tube fluidized-bed reactor is used, can almost it be approached with controlling reaction temperature by adjusting steam pressure in tubulation
Constant temperature, the generation of side reaction can be effectively controlled, gained chromatographic grade dichloromethane purity is high, is adapted to scale industrial production
Need.My company's chloromethanes resource is significantly digested, by being processed further lifting added value, the core for improving glyphosate industry is competing
Strive.
Embodiment：
With reference to specific implementation case, the present invention is described in further detail：
Embodiment 1
1) chloromethanes 50ml and liquid chlorine 45ml are taken, using shell and tube fluidized-bed reactor as consersion unit, takes calcium chloride 10g,
Water under high pressure is passed through in the tubulation of shell and tube fluid bed, technical grade dichloromethane 80ml is prepared；
2) it is 125 DEG C to set kiln temperatures, takes active fruit shell carbon DV11 to be dried in drying oven and uses centrifugation
After dehydrated cooled, it is fitted into glass column, wherein, the water content control of dichloromethane contains in mass percent after being dried in step 2)
Amount≤0.01%；
3) the technical grade dichloromethane being prepared by step 1) is from top to bottom done into Adsorption processing through glass column,
Produce chromatographic grade dichloromethane 70ml.
Embodiment 2
1) chloromethanes 100ml and liquid chlorine 90ml are taken, using shell and tube fluidized-bed reactor as consersion unit, takes calcium chloride 5g,
Water under high pressure is passed through in the tubulation of shell and tube fluid bed, technical grade dichloromethane 150ml is prepared；
2) it is 125 DEG C to set kiln temperatures, takes active fruit shell carbon DV11 to be dried in drying oven and uses centrifugation
After dehydrated cooled, it is fitted into glass column, wherein, the water content control of dichloromethane contains in mass percent after being dried in step 2)
Amount≤0.01%；
3) the technical grade dichloromethane being prepared by step 1) is from top to bottom done into Adsorption processing through glass column,
Produce chromatographic grade dichloromethane 120ml.
Embodiment 3
1) chloromethanes 75ml and liquid chlorine 65ml are taken, using shell and tube fluidized-bed reactor as consersion unit, takes calcium chloride 6g, is arranged
Water under high pressure is passed through in the tubulation of tubular type fluid bed, technical grade dichloromethane 120ml is prepared；
2) it is 125 DEG C to set kiln temperatures, takes active fruit shell carbon DV11 to be dried in drying oven and uses centrifugation
After dehydrated cooled, it is fitted into glass column, wherein, the water content control of dichloromethane contains in mass percent after being dried in step 2)
Amount≤0.01%；
3) the technical grade dichloromethane being prepared by step 1) is from top to bottom done into Adsorption processing through glass column,
Produce chromatographic grade dichloromethane 100ml.
Claims (6)
1. a kind of production technology of dichloromethane, it is characterised in that comprise the following steps：
1) using chloromethanes and liquid chlorine as raw material, using shell and tube fluidized-bed reactor as consersion unit, using calcium chloride as catalyst, instead
Answer formula as follows：
Main reaction：
CH3Cl+Cl2→CH2Cl2+HCl
Side reaction：
CH2Cl2+Cl2→CHCl3+HCl
CHCl3+Cl2→CCl4+HCl
Wherein, water under high pressure is passed through in the tubulation of shell and tube fluid bed, technical grade dichloromethane is prepared；
2) after taking active fruit shell carbon DV11 drying and dehydratings and cooling down, it is fitted into glass column；
3) the technical grade dichloromethane being prepared by step 1) is from top to bottom done into Adsorption processing through glass column, produced
Chromatographic grade dichloromethane.
2. the production technology of dichloromethane according to claim 1, it is characterised in that drying and dehydrating is adopted in the step 2)
It is dehydrated with centrifugation.
3. the production technology of dichloromethane according to claim 1, it is characterised in that drying is dry in the step 2)
Carried out in dry stove.
4. according to the production technology of the dichloromethane described in claim 1, it is characterised in that drying temperature in the step 2)
For 125 DEG C.
5. according to the production technology of the dichloromethane described in claim 1, it is characterised in that two after being dried in the step 2)
The water content control of chloromethanes is in mass percentage content≤0.01%.
A kind of 6. application of production technology of dichloromethane as claimed in claim 1 in terms of agricultural chemicals preparation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711093639.9A CN107814683A (en) | 2017-11-08 | 2017-11-08 | A kind of production technology of dichloromethane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711093639.9A CN107814683A (en) | 2017-11-08 | 2017-11-08 | A kind of production technology of dichloromethane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107814683A true CN107814683A (en) | 2018-03-20 |
Family
ID=61604761
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711093639.9A Withdrawn CN107814683A (en) | 2017-11-08 | 2017-11-08 | A kind of production technology of dichloromethane |
Country Status (1)
| Country | Link |
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| CN (1) | CN107814683A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115945302A (en) * | 2022-11-29 | 2023-04-11 | 池州飞昊达化工有限公司 | Centrifugal filtration system is used in production of diflufenican original medicine |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5513210A (en) * | 1978-07-14 | 1980-01-30 | Asahi Chem Ind Co Ltd | Preparation of chlorinated hydrocarbon |
| CN1137511A (en) * | 1995-03-30 | 1996-12-11 | 株式会社德山 | Method for preparation of methane polychloride |
| CN105693461A (en) * | 2014-11-26 | 2016-06-22 | 天津市科密欧化学试剂有限公司 | Preparation method of chromatographic grade dichloromethane |
| CN106478360A (en) * | 2016-10-08 | 2017-03-08 | 宁波巨化化工科技有限公司 | The catalytic chlorination system of dichloromethane yield ratio can be improved |
-
2017
- 2017-11-08 CN CN201711093639.9A patent/CN107814683A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5513210A (en) * | 1978-07-14 | 1980-01-30 | Asahi Chem Ind Co Ltd | Preparation of chlorinated hydrocarbon |
| CN1137511A (en) * | 1995-03-30 | 1996-12-11 | 株式会社德山 | Method for preparation of methane polychloride |
| CN105693461A (en) * | 2014-11-26 | 2016-06-22 | 天津市科密欧化学试剂有限公司 | Preparation method of chromatographic grade dichloromethane |
| CN106478360A (en) * | 2016-10-08 | 2017-03-08 | 宁波巨化化工科技有限公司 | The catalytic chlorination system of dichloromethane yield ratio can be improved |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115945302A (en) * | 2022-11-29 | 2023-04-11 | 池州飞昊达化工有限公司 | Centrifugal filtration system is used in production of diflufenican original medicine |
| CN115945302B (en) * | 2022-11-29 | 2023-06-30 | 池州飞昊达化工有限公司 | Centrifugal filtration system is used in production of metaflumizone former medicine |
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Application publication date: 20180320 |