CN103073400A - Purification method of methylal - Google Patents
Purification method of methylal Download PDFInfo
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- CN103073400A CN103073400A CN201310055566XA CN201310055566A CN103073400A CN 103073400 A CN103073400 A CN 103073400A CN 201310055566X A CN201310055566X A CN 201310055566XA CN 201310055566 A CN201310055566 A CN 201310055566A CN 103073400 A CN103073400 A CN 103073400A
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Abstract
The invention relates to a purification method of methylal, and the purification method comprises the following steps of firstly placing methylal with the mass concentration being less than 95 percent and accounting for 0.25 to 0.75 percent of the capacity of a reboiler into a high-pressure rectifying system, then charging nitrogen gas into the rectifying system, heating and returning the methylal after the system pressure reaches 0.1 to 0.8MPa, collecting fractions when the tower top temperature reaches the range from 63.5 to 117.7 DEG C, supplementing the methylal with the mass concentration being less than 95 percent into the high-pressure rectifying system when collecting the fractions so as to enable the methylal in the system to account for 0.25 to 0.75 percent of the capacity of the reboiler, stopping the collection when the tower top temperature reaches 63.9 to 118.0 DEG C after the feeding is completed, condensing and cooling the collected fractions through a condenser, and obtaining the methylal with the mass concentration being more than 99.5 percent after the pressure is released. The obtained tower bottom liquid is mixture of methanol with the mass concentration of 99 percent and a little amount of methylal. The purification method has the advantages that a rectifying way of the high-pressure rectifying system is used for purifying the methylal, so that the requirement on the quality of raw materials is low, the purification yield is high, the energy demand is less, the industrialized continuous production can be favored, no harmful substance is discharged, and the environmental protection can be facilitated.
Description
Technical field
The invention still further relates to a kind of with the purify method of methylal〔Su〕 of high-pressure rectification system.
Background technology
The method of purification of methylal〔Su〕 adopts the mode of extraction agent high-pressure rectification and solution-air adverse current mostly at present.The extraction agent that the mode of extraction agent high-pressure rectification adopts mostly is greatly organic solvent and rectifying is complicated, be many glycol dimethyl ethers such as the used extraction agent of Chinese patent " 200710022224.2 ", this extraction agent not only cost is higher, and contaminative is stronger, is unsuitable for a large amount of life-time service.
The mode of solution-air adverse current adopts the polyalkylene or derivatives thereof to carry out the solution-air counter current contact with the purification methylal〔Su〕 such as Chinese patent " 95195524.1 ", and this mode required equipment is had relatively high expectations, and input cost is large, and complicated operation is unsuitable for generally using.
Therefore should provide a kind of new technical scheme to come methylal〔Su〕 is purified, to enlarge its use range.
Summary of the invention
The objective of the invention is: for addressing the above problem, provide the discharging of a kind of unharmful substance, purification efficiency is high, be beneficial to environmental protection, and the method for purification of methylal〔Su〕 simple to operate.
For achieving the above object, the technical solution used in the present invention is:
The method of purification of above-mentioned methylal〔Su〕 adds entry in the methylal〔Su〕 of mass concentration＜95%, adding water weight is 0.1～3 times that methylal〔Su〕 folding hundred is measured, the shared weight of pure methylal〔Su〕 in the methylal〔Su〕 that hundred amounts of wherein rolling over refer to mass concentration＜95%.
A kind of method of purification of methylal〔Su〕, comprise the steps: that first in high-pressure rectification system adding accounts for the methylal〔Su〕 of 0.25～0.75 mass concentration of this system's reboiler capacity＜95%, then be filled with nitrogen, after system pressure reaches 0.1～0.8Mpa, heat up, reflux, and the collection tower top temperature reaches the cut in 63.5～117.7 ℃ of scopes, the methylal〔Su〕 of additional mass concentration＜95% in the high-pressure rectification system again when collecting cut, to keep this intrasystem methylal〔Su〕 to account for 0.25～0.75 of this system's reboiler capacity, after charging is finished, when reaching 63.9～118.0 ℃, the cat head temperature stops to collect, the cut of collecting namely gets mass concentration through the condenser condenses cooling after the row pressure〉99.5% methylal〔Su〕, liquid is that mass concentration is the mixture of 99% methyl alcohol and a small amount of methylal〔Su〕 at the bottom of the tower of gained.
Further, described system pressure is 0.2～0.6Mpa, and tower top temperature is 63.7～104.7 ℃.
Advantage of the present invention is: utilize the mode of high-pressure rectification system rectifying that methylal〔Su〕 is purified, raw materials quality requires low, and purification efficiency is high, and energy requirement is few, is beneficial to industrial continuous large production, and the unharmful substance discharging is beneficial to environmental protection.Methylal〔Su〕 after the purification has very widely purposes, and it has important application in fields such as aerosol, paint remover, refrigeration agent, makeup, clean-out system, lustering agent, pesticide solvent, coating, fuel or fuel dopes.
Description of drawings
Fig. 1 is the schema of the another kind of methylal〔Su〕 method of purification of the present invention.
Embodiment
Wherein the method for purification of embodiment 1, embodiment 2 and the embodiment 3 usefulness methylal〔Su〕 shown in shown in Figure 1 is purified to it, below all embodiment further specify of the present invention, but do not limit protection scope of the present invention.
Embodiment 1
Be that 90% methylal〔Su〕 is purified to the 10000kg mass concentration, comprise the steps: to be first that 90% methylal〔Su〕 squeezes into that (the reboiler capacity of distillation system is 4m in the high-pressure rectification system with the 2000kg mass concentration
3, the volume of 2000kg methylal〔Su〕 is 2.35 m
3), inflated with nitrogen, keeping system pressure is 0.2Mpa, heat up, reflux, when tower top temperature reaches 63.5 temperature, collect cut, when collecting cut again in the high-pressure rectification system additional mass concentration be 90% methylal〔Su〕, account for 0.25～0.75 of this system's reboiler capacity to keep this intrasystem methylal〔Su〕, after having advanced material, when reaching 63.9 ℃, the cat head temperature stops to collect cooling, row pressure, the 8890kg mass concentration is 99.7% methylal〔Su〕, liquid is that the 990kg mass concentration is 99% methyl alcohol at the bottom of the tower.
Embodiment 2
Be that 85% methylal〔Su〕 is purified to the 20000kg mass concentration, comprise the steps: to be first that 85% methylal〔Su〕 squeezes into that (the reboiler capacity of distillation system is 4m in the high-pressure rectification system with the 2000kg mass concentration
3, the volume of 2000kg methylal〔Su〕 is 1.25 m
3), inflated with nitrogen, keeping system pressure is 0.3Mpa, heat up, reflux, when tower top temperature reaches 77.5 ℃, collect cut, when collecting cut again in the high-pressure rectification system additional mass concentration be 85% methylal〔Su〕, to keep this intrasystem methylal〔Su〕 to account for 0.25～0.75 of this system's reboiler capacity, after having advanced material, when reaching 77.9 ℃, the cat head temperature stops to collect cooling, row pressure, the 17500kg mass concentration is 99.9% methylal〔Su〕, liquid is that the 2370kg mass concentration is 99% methyl alcohol at the bottom of the tower, for the synthesis of methylal〔Su〕.
Embodiment 3
Be that 80% methylal〔Su〕 is purified to the certainweight mass concentration, comprise the steps: to be first that 80% methylal〔Su〕 squeezes into that (the reboiler capacity of distillation system is 5m in the high-pressure rectification system with the 2000kg mass concentration
3, the volume of 2000kg methylal〔Su〕 is 2.35 m
3)), inflated with nitrogen, keeping system pressure is 0.8Mpa, heat up, reflux, when tower top temperature reaches 117.7 ℃, collect cut, when collecting cut again in the high-pressure rectification system additional mass concentration be 80% methylal〔Su〕, account for 0.25～0.75 of this system's reboiler capacity to keep this intrasystem methylal〔Su〕, produce continuously by this way, the gained cut is through cooling, and row pressure gets mass concentration and be 99.9% methylal〔Su〕, liquid is that mass concentration is 99.9% methyl alcohol at the bottom of the gained tower, can be used for synthesizing dimethoxym ethane.
Claims (2)
1. the method for purification of a methylal〔Su〕, it is characterized in that comprising the steps: that first in high-pressure rectification system adding accounts for the methylal〔Su〕 of 0.25～0.75 mass concentration of this system's reboiler capacity＜95%, then be filled with nitrogen, after system pressure reaches 0.1～0.8Mpa, heat up, reflux, and the collection tower top temperature reaches the cut in 63.5～117.7 ℃ of scopes, the methylal〔Su〕 of additional mass concentration＜95% in the high-pressure rectification system again when collecting cut, to keep this intrasystem methylal〔Su〕 to account for 0.25～0.75 of this system's reboiler capacity, after charging is finished, when reaching 63.9～118.0 ℃, the cat head temperature stops to collect, the cut of collecting namely gets mass concentration through the condenser condenses cooling after the row pressure〉99.5% methylal〔Su〕, liquid is that mass concentration is the mixture of 99% methyl alcohol and a small amount of methylal〔Su〕 at the bottom of the tower of gained.
2. the method for purification of a kind of methylal〔Su〕 according to claim 3, it is characterized in that: described system pressure is 0.2～0.6Mpa, tower top temperature is 63.7～104.7 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310055566XA CN103073400A (en) | 2011-06-20 | 2011-06-20 | Purification method of methylal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310055566XA CN103073400A (en) | 2011-06-20 | 2011-06-20 | Purification method of methylal |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110164811A Division CN102320940A (en) | 2011-06-20 | 2011-06-20 | Method for purifying methylal |
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| CN103073400A true CN103073400A (en) | 2013-05-01 |
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| CN201310055566XA Pending CN103073400A (en) | 2011-06-20 | 2011-06-20 | Purification method of methylal |
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| CN (1) | CN103073400A (en) |
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2011
- 2011-06-20 CN CN201310055566XA patent/CN103073400A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 赵俊彤等: "变压精馏分离甲缩醛与甲醇混合物过程.pdf", 《化工进展》 * |
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Application publication date: 20130501 |