CN109096142A - A kind of industrial process for separating of N-METHYLFORMAMIDE and diethylene glycol monomethyl ether - Google Patents
A kind of industrial process for separating of N-METHYLFORMAMIDE and diethylene glycol monomethyl ether Download PDFInfo
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- CN109096142A CN109096142A CN201810932024.9A CN201810932024A CN109096142A CN 109096142 A CN109096142 A CN 109096142A CN 201810932024 A CN201810932024 A CN 201810932024A CN 109096142 A CN109096142 A CN 109096142A
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- mdg
- nmf
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- rectifying
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to the industrial process for separating of main component N-METHYLFORMAMIDE (NMF) and diethylene glycol monomethyl ether (MDG) in electronic chemical product stripper.The method that the present invention uses low pressure molecular distillation can have many advantages, such as energy conservation, safety and environmental protection with the NMF and MDG in the useless stripper of high efficiente callback electronic chemical product.A kind of separation and purification technique of high purity N MF and MDG mainly comprises the steps that 1) decompression degassing: decompression degassing process is carried out to the mixture of NMF and MDG, after preventing material from entering molecule rectifying column, because pressure drop causes mist to splash；2) molecule rectifying: the material after degassing enters molecule rectifying column, different using the molecule mean free path of two kinds of ingredients, realizes separation.For the present invention compared with common process, the purity of finished product NMF and MDG reach 99% or more, and the NMF after rectifying and MDG reaches the purity requirement of electronic chemical product stripper, realize the separating-purifying of NMF and MDG.
Description
Technical field
The present invention relates to a kind of purification purifying techniques of the useless stripper of electronic chemical product, and main component is N-METHYLFORMAMIDE
(NMF) and diethylene glycol monomethyl ether (MDG).
Background technique
Stripper is used in liquid crystal display panel, removes on microcircuit exposure mask in the manufacture of the techniques such as semiconductor integrated circuit
Photoresist, stripper are mainly the mixture of organic amine and polar organic solvent.Present invention is generally directed to based on NMF and MDG
The stripper of ingredient is wanted, stripper becomes useless stripper because introducing other impurities after use, and the stripper that gives up is through separating-purifying
The mixture based on NMF and MDG is obtained afterwards, needs to obtain mixture further separating-purifying the NMF and MDG of high-purity,
The NMF and MDG of high-purity are deployed into stripper by a certain percentage can just regenerate use.NMF and the boiling point of MDG under normal pressure compared with
Height, energy consumption is high for conventional distil-lation, and requirement of the electron level stripper to purity is high, and conventional rectification is difficult to reach high-purity requirement.
The thermal stability of main component NMF and MDG in stripper are poor, and flash-point is low, point of the conventional rectification in NMF and MDG
There are certain security risks from, and conventional rectification realizes separation using the heat of vaporization difference of molecule, first by material high temperature
Gasification, then cryogenic condensation, needs to consume mass energy, less economical, not environmentally protective enough.Molecule rectifying is in high vacuum item
Under part, the spacing of evaporating surface and cryosurface is less than or equal to the steam molecule mean free path of separated object material, and steam molecule is flat
The equal big molecule of free path can fly and condense upon on cryosurface, realize the separation of raw material, and molecule rectifying has safety, section
It can environmental protection and the high feature of separative efficiency.
Summary of the invention
The present invention overcomes conventional rectification method separation NMF and the high disadvantages of MDG mixture energy consumption, make full use of molecule smart
The advantage evaporated realizes the efficient purification of NMF and MDG in useless stripper, NMF's and MDG is pure in product with new technological flow
Degree has reached 99.9% or more.The technique is outer in addition to the purity is high of recycling product, also simple, the environmentally protective and low energy with process
The advantages that consumption.
The technical solution adopted by the present invention is that:
A kind of separating technology of useless stripper NMF and MDG, the technique specifically includes the following steps:
1) be depressured degassing process: the degassed tower degassing of the mixture of NMF and MDG, feed flow rate is uniformly moderate, is depressured degassing tower
Pressure is 5000-10000 Pa.
2) molecule rectification working process: the material after decompression degassing scrapes membrane molecule rectifier unit with plate and carries out molecule rectifying, molecule
The temperature of rectifying is 70-100 DEG C, and pressure is 10-200 Pa, and the molecule mean free path of lighter component MDG is long, can be with after heated
Cryosurface enrichment is flown to, and the molecule mean free path of NMF is short, molecule flies less than cryosurface after being heated, can only be in heating surface richness
Collection, realizes the separation of NMF and MDG.
Detailed description of the invention
Fig. 1 is the separation rectification technique flow chart of NMF of the present invention and MDG.
Specific embodiment
This patent is further described with reference to embodiments, the present invention includes but is not limited to following embodiment.
Embodiment 1
The mixture of NMF and MDG is fed with the flow velocity room temperature of 360 kg/h, and the pressure for being depressured degassing tower is 5000-10000 Pa
According to Henry law, in the sealing container of certain temperature, gas partial pressure with the gas be dissolved in the molar concentration in solution at
Direct ratio.By decompression degassing tower processing, the gas content in material eliminates 90% or more.Reduce material and enters molecule rectifying
After tower because caused by pressure drop mist splash.It is continuous by heating decompression and liquid film after material enters molecule rectifying column
Update makes molecule continually quickly fly out from liquid level, the long MDG of molecule mean free path, can fly to cryosurface enrichment, and
The short NMF of molecule mean free path can only be enriched with sedimentation between heating surface and cryosurface, it is achieved that point of NMF and MDG
From, and the finished product purity of NMF and MDG is up to 99% or more.At 80 DEG C or so, pressure control exists for the temperature control of molecule rectifying column
10 Pa or so.
Claims (4)
1. the industrial process for separating of NMF and MDG a kind of, it is characterised in that the technique comprising the following specific steps
(a) be depressured degassing process: the mixture of NMF and MDG enters decompression degassing tower with certain flow rate, is de-gassed to material,
Large quantity of air is dissolved in liquid material, in the case where pressure drop, dissolved gas largely discharges, and mist is caused to splash, and influences
The separating effect of molecule rectifying；
(b) molecule rectification working process: the liquid material after degassing enters molecule rectifying column, average freely using the molecule of heterogeneity
Cheng Butong realizes the separation of heterogeneity, and the molecule mean free path of NMF is smaller, and the molecule mean free path of MDG is bigger, institute
Enrichment can be condensed on cryosurface with MDG, and NMF is enriched in heating surface.
2. the industrial process for separating of NMF and MDG according to claim 1 a kind of, which is characterized in that include but is not limited to pair
NMF separates rectifying with MDG, and heat-sensitive substance or the discrepant two mixtures matter of molecule mean free path can be sent out with this
Bright implementation separation.
3. the industrial process for separating of NMF and MDG according to claim 1 a kind of, which is characterized in that be depressured in step 1 de-
Pressure in gas tower is slightly larger than molecule Rectification column pressure, and the liquid being depressured in degassing tower can enter molecule essence under pressure
Evaporate tower.
4. the industrial process for separating of NMF and MDG according to claim 1 a kind of, which is characterized in that divide described in step 2
Sub- rectifying device scrapes membrane molecule rectifier unit using plate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810932024.9A CN109096142A (en) | 2018-08-17 | 2018-08-17 | A kind of industrial process for separating of N-METHYLFORMAMIDE and diethylene glycol monomethyl ether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810932024.9A CN109096142A (en) | 2018-08-17 | 2018-08-17 | A kind of industrial process for separating of N-METHYLFORMAMIDE and diethylene glycol monomethyl ether |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109096142A true CN109096142A (en) | 2018-12-28 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810932024.9A Pending CN109096142A (en) | 2018-08-17 | 2018-08-17 | A kind of industrial process for separating of N-METHYLFORMAMIDE and diethylene glycol monomethyl ether |
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| Country | Link |
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| CN (1) | CN109096142A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970591A (en) * | 2019-05-06 | 2019-07-05 | 新中天环保股份有限公司 | It is a kind of to recycle high-purity N-methylformamide technique from useless stripper |
| CN112851541A (en) * | 2021-02-24 | 2021-05-28 | 河北科技大学 | Method and device for recovering NMF and MDG from waste photoresist stripping solution |
-
2018
- 2018-08-17 CN CN201810932024.9A patent/CN109096142A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970591A (en) * | 2019-05-06 | 2019-07-05 | 新中天环保股份有限公司 | It is a kind of to recycle high-purity N-methylformamide technique from useless stripper |
| CN109970591B (en) * | 2019-05-06 | 2021-04-27 | 新中天环保股份有限公司 | Process for recovering high-purity N-methylformamide from waste stripping liquid |
| CN112851541A (en) * | 2021-02-24 | 2021-05-28 | 河北科技大学 | Method and device for recovering NMF and MDG from waste photoresist stripping solution |
| CN112851541B (en) * | 2021-02-24 | 2022-08-12 | 河北科技大学 | Method and device for recovering NMF and MDG from waste photoresist stripping solution |
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| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20181228 |
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| WD01 | Invention patent application deemed withdrawn after publication |