CN110357766A - It is a kind of to prepare chloromethyl ether compound preparation process and its Preparation equipment - Google Patents
It is a kind of to prepare chloromethyl ether compound preparation process and its Preparation equipment Download PDFInfo
- Publication number
- CN110357766A CN110357766A CN201910484031.1A CN201910484031A CN110357766A CN 110357766 A CN110357766 A CN 110357766A CN 201910484031 A CN201910484031 A CN 201910484031A CN 110357766 A CN110357766 A CN 110357766A
- Authority
- CN
- China
- Prior art keywords
- ether compound
- fluid reservoir
- chloromethyl ether
- layer
- preparation process
- 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.)
- Pending
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Chloromethyl ether compound preparation process is prepared the invention discloses a kind of, alcohols is synthesized with paraformaldehyde, hcl reaction, obtains chloromethyl ether compound.Also disclose it is a kind of rectifying column used in chloromethyl ether compound is prepared using above-mentioned technique, including rectifying tower body, charging receiver, top discharge fluid reservoir, bottom discharge fluid reservoir, heater, condenser；Rectifying tower body is from top to bottom successively set as top discharge layer, upper packing layer, inlet tube, middle packing layer, air inlet pipe, lower packing layer, bottom discharge layer；The top of top discharge layer is equipped with upper condenser, and top discharge layer connects top discharge fluid reservoir, and the inlet tube connects feed liquor fluid reservoir, and bottom discharge layer is equipped with bottom heater, and bottom discharge layer connects bottom discharge fluid reservoir.The yield of synthesis technology of the invention, energy conservation and environmental protection, and product is high, and purity is good.Rectifying tower structure is novel, and easy to operate, gas-liquid mass transfer is high-efficient, so that rectifying speed is fast and rectification effect is good.
Description
Technical field
The present invention relates to compound synthesis preparation technical fields, specially a kind of to prepare chloromethyl ether compound preparation work
Skill and its Preparation equipment.
Background technique
Alkyl chloromethylether class compound may be used as the protecting group of pure and mild amide functional group, on the other hand be used as alkyl
Change reagent.Although the protection of alcoholic extract hydroxyl group can select to use there are many different types of protecting group, alkyl chloromethylether is
One of most important one protecting group.Its principal advantages are that upper protection is easy, and yield is preferable；It is special to deprotect, to many
Stable reaction.Such as Benzyl chloromethyl ether, methylchlormethyl ether are the good reagents for introducing benzyl protection and methoxyl group protection.
The reaction condition of alkyl chloromethylether and alcohol as mild as a dove, is generally required and is carried out in the presence of base, and common alkali includes n-
Pr2NEt, NaH, LDA etc..Under the same reaction conditions, allyl alcohol is also similarly protected, and phenolic hydroxyl group generally provides more
Good result.But if selecting reagent dosage appropriate, etherificate general alcohol hydroxyl can be selected in the presence of vinyl alcohol
Base.
Wherein, chloromethyl ether compound in the synthesis process, after reaction kettle has been completed, enters rectifying still (rectifying
Tower) interior rectifying, obtain sterling.Rectifying column in the prior art is in the rectifying for chloromethyl ether compound, existing master
Want problem to be: 1, the chloromethyl ethers type being prepared in the present invention is more, therefore, to the pressure requirements in distillation process
Higher, therefore, higher for the sealing requirements of equipment, the leakproofness of feedboard will affect the leakproofness of entire rectifying still.2,
The chloromethyl ethers type being prepared in the present invention is more therefore larger to the submission of the raw material storage tank of rectifying tap terminal, essence
The amount of evaporating is excessive, causes rectification effect poor, and rectifying amount is small, causes rectifying speed slow, therefore how to control the rectifying amount of raw material storage tank
It is the key that the mode of model budget can also be used certainly in current realization effectively quickly rectifying, calculates rectifying speed, control original
Expect the flow velocity of rear pump, Lai Shixian quickly and effectively rectifying, but the structure of rectifying storage tank itself is improved, and realizes control
The effective way of rectification efficiency.3, in rectifying still when gas-liquid mixed, when liquid flows down along packing layer, have and gradually concentrated to tower wall
Trend so that the flow quantity near tower wall is gradually increased, this phenomenon is known as wall stream, and wall stream effect causes gas-liquid two-phase filling out
The bed of material is unevenly distributed, so that mass-transfer efficiency be made to decline.Therefore, improve to the structure of packing layer is to need to improve at present
Direction.
Summary of the invention
To solve the above problems, the invention discloses it is a kind of prepare chloromethyl ether compound preparation process and its preparation set
It is standby, the effective solution above problem.
In order to reach the goals above, the invention provides the following technical scheme:
A kind of preparation process preparing chloromethyl ether compound, comprising the following steps: alcohols and paraformaldehyde, hydrogen chloride are anti-
It should synthesize, obtain chloromethyl ether compound.
Further, alcohols of the invention is the one of which of methanol, benzyl alcohol, ethylene chlorhydrin, propyl alcohol, isopropanol.
Further, reaction temperature of the invention is 5 DEG C ~ 15 DEG C.
Further, the reaction time is 3-8 hours.
Further, obtaining chloromethyl ether compound is methylchlormethyl ether, Benzyl chloromethyl ether, 2- chloroethyl chloromethane
Base ether, propyl chloromethylether, isopropyl chloride methyl ether, purity are greater than 98.5%(GC).
Specific preparation process is the following steps are included: be passed through alcohols and paraformaldehyde for hydrogen chloride gas under cryogenic
Aaerosol solution in, products therefrom obtains chloromethyl ether compound by carrying out rectification under vacuum in vacuum rectification tower.Product
Quality is stablized, gas phase purity > 98%, yield 78%.
The invention also discloses a kind of rectifying column for preparing chloromethyl ether compound, the rectifying column includes rectifying column
Body, charging receiver, top discharge fluid reservoir, bottom discharge fluid reservoir, heater, condenser；The rectifying tower body by up to
Under be successively set as top discharge layer, upper packing layer, inlet tube, middle packing layer, air inlet pipe, lower packing layer, bottom discharge layer；It is described
The top of top discharge layer is equipped with upper condenser, and the top discharge layer connects top discharge fluid reservoir, the inlet tube connection
Feed liquor fluid reservoir, the bottom discharge layer are equipped with bottom heater, and the bottom discharge layer connects bottom discharge fluid reservoir；It is described
Charging fluid reservoir and inlet tube are directly provided with feed liquor circuit, are additionally provided with side door circuit on the feed liquor circuit.
Further, the upper packing layer, middle packing layer, filler is filled in lower packing layer, the filler is to draw west
Ring filler, the Raschig ring filler include wire cylinder, inclined wire plate, and inclined wire plate is equipped in the wire cylinder, described oblique
Inclined meshed plate is arranged on wire cylinder.Filler of the invention uses coil of wire at tubular, and inclination is equipped in cylinder
Waffle slab, on the one hand strengthen stop, the incorporation time of fluid (liquids and gases), mass transfer effect is good, on the other hand, it is thermally conductive
Effect is good.And low in cost, preparation is conveniently.
Further, control valve is equipped on the bypass circulation and feed liquor circuit.It is controlled by valve, it is convenient to liquid
Flow control.
The invention has the following beneficial effects: 1, synthesis technology of the invention, the yield of energy conservation and environmental protection, and product is high, pure
It spends.2, Preparation equipment of the invention, rectifying tower structure is novel, and easy to operate, gas-liquid mass transfer is high-efficient, so that rectifying speed is fast
And rectification effect is good.
Detailed description of the invention
Fig. 1 is rectifying tower structure schematic diagram of the present invention；
Fig. 2 is Raschig ring filler structural schematic diagram.
In figure: rectifying tower body 1, charging receiver 2, top discharge fluid reservoir 3, bottom discharge fluid reservoir 4, heater 5, cold
Condenser 6, top discharge layer 8, upper packing layer 9, inlet tube 10, middle packing layer 11, air inlet pipe 12, lower packing layer 13, bottom discharge
Layer 14, feed liquor circuit 15, side door circuit 16, filler 17, wire cylinder 171, inclined wire plate 172, control valve 18.
Specific embodiment
With reference to the accompanying drawings and detailed description, the present invention is furture elucidated, it should be understood that following specific embodiments are only
For illustrating the present invention rather than limiting the scope of the invention.
Embodiment 1
A kind of preparation process preparing chloromethyl ether compound, comprising the following steps: alcohols and paraformaldehyde, hydrogen chloride are anti-
It should synthesize, obtain chloromethyl ether compound.
Further, alcohols of the invention is the one of which of methanol, benzyl alcohol, ethylene chlorhydrin, propyl alcohol, isopropanol.
Further, reaction temperature of the invention is 5 DEG C ~ 15 DEG C.
Further, the reaction time is 3-8 hours.
Further, obtaining chloromethyl ether compound is methylchlormethyl ether, Benzyl chloromethyl ether, 2- chloroethyl chloromethane
Base ether, propyl chloromethylether, isopropyl chloride methyl ether, purity are greater than 98.5%(GC).
Specific preparation process is the following steps are included: be passed through alcohols and paraformaldehyde for hydrogen chloride gas under cryogenic
Aaerosol solution in, products therefrom obtains chloromethyl ether compound by carrying out rectification under vacuum in vacuum rectification tower.Product
Quality is stablized, gas phase purity > 98%, yield 78%.
Embodiment 2
The invention also discloses a kind of rectifying columns for preparing chloromethyl ether compound, as shown in Figure 1, rectifying column includes rectifying column
Body 1, charging receiver 2, top discharge fluid reservoir 3, bottom discharge fluid reservoir 4, heater 5, condenser 6；Rectifying tower body is by upper
Top discharge layer 8, upper packing layer 9, inlet tube 10, middle packing layer 11, air inlet pipe 12, lower packing layer 13, bottom are successively set as under
Portion goes out the bed of material 14；The top of top discharge layer is equipped with upper condenser, and top discharge layer connects top discharge fluid reservoir, and inlet tube connects
Liquid fluid reservoir is tapped into, bottom discharge layer is equipped with bottom heater, and bottom discharge layer connects bottom discharge fluid reservoir.
Charging fluid reservoir and inlet tube are directly provided with feed liquor circuit 15, and side door circuit 16 is additionally provided on feed liquor circuit.
In the present embodiment, it as shown in Fig. 2, upper packing layer, middle packing layer, being filled with filler 17 in lower packing layer, fills out
Material is Raschig ring filler, and Raschig ring filler includes wire cylinder 171, inclined wire plate 172, is equipped with inclined wire plate in wire cylinder,
Inclined wire plate is inclined on wire cylinder.
In the present embodiment, control valve 18 is equipped on bypass circulation and feed liquor circuit.
The technical means disclosed in the embodiments of the present invention is not limited only to technological means disclosed in above embodiment, further includes
Technical solution consisting of any combination of the above technical features.It should be pointed out that for those skilled in the art
For, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also considered as
Protection scope of the present invention.
Claims (8)
1. a kind of prepare chloromethyl ether compound preparation process, it is characterised in that: the following steps are included: alcohols and poly first
Aldehyde, hcl reaction synthesis, obtain chloromethyl ether compound.
2. a kind of as described in claim 1 prepare chloromethyl ether compound preparation process, it is characterised in that: the alcohols
For the one of which of methanol, benzyl alcohol, ethylene chlorhydrin, propyl alcohol, isopropanol.
3. a kind of chloromethyl ether compound preparation process is prepared as described in claim 1, it is characterised in that: reaction temperature is
5℃~15℃。
4. a kind of chloromethyl ether compound preparation process is prepared as described in claim 1, it is characterised in that: the reaction time is
3-8 hours.
5. a kind of as described in claim 1 prepare chloromethyl ether compound preparation process, it is characterised in that: obtain chloromethyl
Ether compound is methylchlormethyl ether, Benzyl chloromethyl ether, 2- chloroethyl chloromethylether, propyl chloromethylether, isopropyl chloride
Methyl ether.
6. feature exists using rectifying column used in chloromethyl ether compound preparation process is prepared described in claim 1-5
In: the rectifying column include rectifying tower body, it is charging receiver, top discharge fluid reservoir, bottom discharge fluid reservoir, heater, cold
Condenser；The rectifying tower body be from top to bottom successively set as top discharge layer, upper packing layer, inlet tube, middle packing layer, air inlet pipe,
Lower packing layer, bottom discharge layer；The top of the top discharge layer is equipped with upper condenser, and top discharge layer connection top goes out
Expect that fluid reservoir, the inlet tube connect feed liquor fluid reservoir, the bottom discharge layer is equipped with bottom heater, the bottom discharge layer
Connect bottom discharge fluid reservoir；The charging fluid reservoir and inlet tube are directly provided with feed liquor circuit, also set on the feed liquor circuit
There is side door circuit.
7. rectifying column as claimed in claim 6, it is characterised in that: the upper packing layer, middle packing layer are filled out in lower packing layer
Filled with filler, the filler is Raschig ring filler, and the Raschig ring filler includes wire cylinder, inclined wire plate, the wire
Inclined wire plate is equipped in cylinder, the inclined wire plate is inclined on wire cylinder.
8. rectifying column as claimed in claim 6, it is characterised in that: be equipped with control on the bypass circulation and feed liquor circuit
Valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910484031.1A CN110357766A (en) | 2019-06-05 | 2019-06-05 | It is a kind of to prepare chloromethyl ether compound preparation process and its Preparation equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910484031.1A CN110357766A (en) | 2019-06-05 | 2019-06-05 | It is a kind of to prepare chloromethyl ether compound preparation process and its Preparation equipment |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110357766A true CN110357766A (en) | 2019-10-22 |
Family
ID=68215147
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910484031.1A Pending CN110357766A (en) | 2019-06-05 | 2019-06-05 | It is a kind of to prepare chloromethyl ether compound preparation process and its Preparation equipment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110357766A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516040A (en) * | 2011-10-31 | 2012-06-27 | 天津泰普药品科技发展有限公司 | Industrialized production method of phenylalkyl chloromethyl ether |
| CN104437295A (en) * | 2014-12-24 | 2015-03-25 | 赤峰盛森硅业科技发展有限公司 | Device and method for preparing tetramethoxysilane |
| CN104892423A (en) * | 2015-05-18 | 2015-09-09 | 太原理工大学 | A process of preparing dimethyl carbonate by oxidative carbonylation of methanol |
-
2019
- 2019-06-05 CN CN201910484031.1A patent/CN110357766A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516040A (en) * | 2011-10-31 | 2012-06-27 | 天津泰普药品科技发展有限公司 | Industrialized production method of phenylalkyl chloromethyl ether |
| CN104437295A (en) * | 2014-12-24 | 2015-03-25 | 赤峰盛森硅业科技发展有限公司 | Device and method for preparing tetramethoxysilane |
| CN104892423A (en) * | 2015-05-18 | 2015-09-09 | 太原理工大学 | A process of preparing dimethyl carbonate by oxidative carbonylation of methanol |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105037094A (en) | Energy coupling distillation method for preparing ethyl alcohol by means of acetic acid ester hydrogenation | |
| CN101928309B (en) | 3,2',6'-tri-N-acetyl gentamicin C1asynthesis method | |
| CN101092426A (en) | Reaction system and synthetic method for producing chloropropyl triethoxy silicane continuously | |
| CN102649698B (en) | The efficient production method of ethylene glycol | |
| CN110357766A (en) | It is a kind of to prepare chloromethyl ether compound preparation process and its Preparation equipment | |
| CN111635298A (en) | Method and device for preparing glycol ether | |
| CN110102072A (en) | Hypergravity rectifying couples the device and control method of decompression separation methanol-water with reacting | |
| CN106831360B (en) | Process method for continuously preparing β -naphthyl methyl ether | |
| CN102557849A (en) | Continuous reaction method | |
| CN210030505U (en) | Crotonaldehyde reaction rectification device | |
| CN104262177B (en) | A kind of separation purification method of thick diglycolamine | |
| CN207210295U (en) | A kind of ethanol purification system and chromatographically pure alcohol production system | |
| CN204779421U (en) | Utilize device of novel catalysis rectification regular packing production methylal | |
| CN211946867U (en) | Device for preparing high-purity methylal by synchronously operating extraction and rectification | |
| CN109851583A (en) | Epoxyalkane purification process | |
| CN103739423A (en) | Process for recovering C5 from etherified liquefied gas | |
| CN103755532B (en) | Chloromethyl ether continuous production system and production process utilizing same | |
| CN207307225U (en) | A kind of rectifier unit for phenyl ethylamine recycling | |
| CN208791523U (en) | A kind of purification alpha-pyrrolidone steams the device of slag | |
| CN103819304B (en) | The high mixture that boils of a kind of epoxy decolours and extracts the processing method of wherein trichloropropane | |
| CN212914588U (en) | A rectifier unit for production of unleaded gasoline antiknock agent | |
| CN213724895U (en) | Reaction recovery device of heptafluoro isobutyl alcohol | |
| CN204897786U (en) | Methyl tert butyl ether production facility | |
| CN102432434A (en) | Method for synthesizing 3-methyl-3-butene-1-ol | |
| CN207405107U (en) | A kind of process units of tert-butylcyclohexyl ethyl carbonate synthetic perfume |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191022 |