CN108727191A - A kind of preparation method of semiconductor grade propylene glycol methyl ether acetate - Google Patents
A kind of preparation method of semiconductor grade propylene glycol methyl ether acetate Download PDFInfo
- Publication number
- CN108727191A CN108727191A CN201710261566.3A CN201710261566A CN108727191A CN 108727191 A CN108727191 A CN 108727191A CN 201710261566 A CN201710261566 A CN 201710261566A CN 108727191 A CN108727191 A CN 108727191A
- Authority
- CN
- China
- Prior art keywords
- propylene glycol
- ether acetate
- methyl ether
- glycol methyl
- preparation
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C69/00—Esters of carboxylic acids; Esters of carbonic or haloformic acids
- C07C69/02—Esters of acyclic saturated monocarboxylic acids having the carboxyl group bound to an acyclic carbon atom or to hydrogen
- C07C69/12—Acetic acid esters
- C07C69/16—Acetic acid esters of dihydroxylic compounds
Abstract
The invention discloses a kind of preparation methods of semiconductor grade propylene glycol methyl ether acetate (abbreviation PMA), using technical grade propylene glycol methyl ether acetate as raw material, first pass through highly efficient distilling purification, molecular sieve dehydration, pass through resin deacidification again, cationic, anionic exchange resin removes metal ion and nonmetallic ion ion in propylene glycol methyl ether acetate, and semiconductor grade propylene glycol methyl ether acetate is obtained finally by ultrafiltration.Product weight content >=99.99% of the present invention, coloration APHA≤10, moisture≤50ppm, acidity≤20ppm, each individual event metal ion < 0.1ppb, each individual event nonmetallic ion < 100ppb, dust granules (0.5 μm of grain size >) < 5pcs/ml, meet the requirement of semiconductor device fabrication process.Present invention process is succinct, environmentally protective, easily realizes that serialization, safe operation, product quality are stablized, is suitble to industrialization, large-scale production.
Description
Technical field
The present invention relates to a kind of preparation methods of electron level organic chemicals, and in particular to a kind of semiconductor grade propylene glycol first
The preparation method of ether acetate.
Background technology
Semiconductor manufacturing is largely a kind of technical process related with chemistry, and up to 20% processing step is clear
The processing with crystal column surface is washed, involved purity of chemicals and cleanliness factor are to the yield rate of semiconductor devices, electric property and length
Phase reliability etc. has very important influence.As microelectric technique develops to ultra-large, great scale, chip integration
Higher and higher, crystal column surface photoetching lines are more and more finer, currently, high-end lithographic process technologies have reached 22nm, this is to electricity
Sub- chemicals proposes high requirement, the SEMI- that indices must reach semiconductor equipment and material structure is formulated
The requirement of C12 standards.
Semiconductor grade propylene glycol methyl ether acetate is one of process for fabrication of semiconductor device electronic chemical product, is a kind of peace
Entirely, environmentally friendly, function admirable Multifunctional organic solvent, is mainly used for the manufacturing process such as liquid crystal display, photoresist.The country also has
The related patents of propylene glycol methyl ether acetate electronic chemical product are reported, as mentioned propylene glycol methyl ether acetate in CN101993360A
By being detached from sub- this procedure of tower, 13 metal ion species can be reduced to 5ppb or less；CN102617345A and CN20251918U
It mentions by being detached from sub- tower process by the metal ion in propylene glycol methyl ether acetate such as：The weight such as sodium, potassium, calcium, magnesium, lead, zinc, iron
It measures content and is less than 10ppb.The above patent is identical technique and the method for using, and the sub- tower removal metal ion of the disengaging is real
It is exactly a kind of conventional rectificating method on border, belongs to primary purifying technique；Meanwhile not referring to electronic grade propylene glycol methyl ether acetate
The information such as all other quality index can not meet the technical specification and quality requirement of electronic grade chemicals.
In conclusion yet there are no the open report of the preparation method in relation to semiconductor grade propylene glycol methyl ether acetate.
Invention content
It is existing to solve the purpose of the present invention is to provide a kind of preparation method of semiconductor grade propylene glycol methyl ether acetate
The problems such as product weight content is low in technology, moisture is high, acidity is high, foreign ion weight content is high.
The technical solution adopted in the present invention is as follows：
A kind of preparation method of semiconductor grade propylene glycol methyl ether acetate is original with technical grade propylene glycol methyl ether acetate
Material, by rectification and purification, molecular sieve dehydration, then by resin deacidification, cationic, anionic exchange resin removes propylene glycol monomethyl ether acetic acid
Metal ion in ester and nonmetallic ion finally obtain semiconductor grade propylene glycol methyl ether acetate by ultrafiltration, specific to prepare
Method is as follows：
(1) rectification and purification：Technical grade weight content is first passed through efficiently in 99.0% or more propylene glycol methyl ether acetate
Light rectifying is taken off, then by efficiently taking off rectifying again, weight content >=99.99% of propylene glycol methyl ether acetate after rectification and purification；
(2) it is dehydrated：Propylene glycol methyl ether acetate after rectification and purification is passed through into molecular sieve dehydration, dewatered propylene glycol first
Moisture control is in 50ppm or less in ether acetate；
(3) depickling：Dewatered propylene glycol methyl ether acetate is removed into propylene glycol methyl ether acetate by resin adsorption bed
In acetic acid, remove acetic acid after propylene glycol methyl ether acetate in controlling pH in 20ppm or less；
(4) cation exchanges：Propylene glycol methyl ether acetate after depickling is exchanged into bed removal by cation exchange resin
Metal ion, cation exchange after propylene glycol methyl ether acetate in each individual event metal ion control in 0.1ppb or less；
(5) anion exchange：The propylene glycol methyl ether acetate for removing metal ion is exchanged by anion exchange resin
Bed removes nonmetallic ion, and each individual event nonmetallic ion control is in 100ppb in the propylene glycol methyl ether acetate after anion exchange
Below；
(6) ultrafiltration：Propylene glycol methyl ether acetate after removal nonmetallic ion is reduced into propylene glycol monomethyl ether by ultrafilter
Dust granules in acetate, the dust granules of 0.5 μm of grain size > are controlled in 5pcs/ in the propylene glycol methyl ether acetate after ultrafiltration
Ml or less.
In step (1) rectification and purification process, efficiently take off de- used in lightness-removing column and the efficiently de- rectifying again used in light rectifying
One kind in filler model BX500, CY700, CY700S, DY1000 that weight tower is selected efficiently takes off de- light used in light rectifying
The preferred CY700S of tower efficiently takes off the preferred CY700 of weight-removing column used in rectifying again.
In step (1) rectification and purification process, described efficiently takes off reflux ratio ranging from (1~50) in light distillation operation：1,
Preferred scope (2~45)：1；Reflux ratio range (0.5~3.0) in efficiently de- weight distillation operation：1, preferred scope (0.8~
2.5)：1.
In step (2) dehydration procedure, the molecular sieve is selectedOrAluminosilicate molecular sieves in
One kind, preferablyAluminosilicate molecular sieves.
In step (2) dehydration procedure, the aluminosilicate molecular sieves select particle diameter be 0.5~1.0,1.6~
One kind in 2.5mm, 3~5mm, preferably 1.6~2.5mm of particle diameter.
In step (3) deacidification process, resin used in the resin adsorption bed selects large aperture basicity styrene series anion
Any one of exchanger resin, preferably any one of large aperture weakly basic styrene type anion exchange resin.
In step (3) deacidification process, propylene glycol methyl ether acetate passes through propylene glycol methyl ether acetate when resin adsorption bed
Flow velocity is (1~50) BV/h, preferably (5~45) BV/h.
Step (4) cation exchange process in, the cation exchange resin be large aperture acidity polystyrene sun from
Any type of sub-exchange resin, preferably any one of storng-acid cation exchange resin.
Step (4) cation exchange process in, it is described by cation exchange resin exchange bed when propylene glycol monomethyl ether vinegar
The flow velocity of acid esters is (1~80) BV/h, preferably (5~70) BV/h.
In step (5) anion exchange procedures, the anion exchange resin be large aperture basicity styrene series the moon from
Any type of sub-exchange resin, preferably any one of strong-base anion-exchange resin.
In step (5) anion exchange procedures, it is described by anion exchange resin exchange bed when propylene glycol monomethyl ether vinegar
The flow velocity of acid esters is (1~50) BV/h, preferably BV=(5~45) BV/h.
In step (6) ultrafiltration process, the filter membrane used in the ultrafilter is hollow fiber ultrafiltration membrane, and material is poly-
One kind in amide, polyether sulfone, Kynoar, preferably Kynoar；The aperture < 0.5 of the hollow fiber ultrafiltration membrane
μm, preferably 0.05 μm.
Compared with prior art, the present invention has the advantages that following several respects：
(1) using technical grade propylene glycol methyl ether acetate as raw material, using a variety of purifying process being combined, product quality reaches
To the standard requirement of semiconductor grade electronic chemical product SEMI-C12.
(2) technical solution used by is scientific and reasonable, easy to operate, easily realizes that serialization, product quality are stablized, is suitable for work
Industry, large-scale production.
(3) taking off has the propylene glycol methyl ether acetate generation of a small amount of low weight content gently and during de- weight, can make through processing
Coating grade solvent is sold, and preparation process is environmentally protective；
De- light rectifying of the present invention refers to the light component impurity removed by rectifying in propylene glycol monomethyl ether product；De- weight
Rectifying refers to the heavy component impurity removed by rectifying in propylene glycol monomethyl ether product；Mixed bed refer to a certain proportion of positive and negative from
Sub-exchange resin is mixed loaded in same switch, is swapped, is removed to the ion in fluid.
Description of the drawings
Fig. 1 is the process flow diagram for preparing semiconductor grade propylene glycol methyl ether acetate.
Wherein：1 is efficient de-light rectification column, and 2 be efficiently de- heavy distillation column, and 3 be molecular sieve water separation tower, and 4 be resin deacidification
Tower, 5 be cation resin exchange tower, and 6 be resin anion (R.A.) exchange column, and 7 be ultrafilter.
Specific implementation mode
In order to make the objectives, technical solutions and advantages of the present invention clearer, With reference to embodiment, to this
Invention is further described.It should be understood that these descriptions are merely illustrative, and it is not intended to limit the scope of the present invention.
Embodiment 1
Combined process flow chart 1, by technical grade weight content 99.0% or more propylene glycol methyl ether acetate with 115L/
The flow of h is preheated rear de- light into 1：Lightness-removing column filler model CY700S, atmospheric operation, reflux ratio 10:1, bottom temperature
150.0±1.0℃；Tower bottoms enters 2 de- weights：Weight-removing column filler model CY700, operating pressure 30KPa, reflux ratio 1.2：1,
85.0 ± 0.5 DEG C of tower top temperature, 116.0 ± 1.0 DEG C of bottom temperature, overhead extraction high-purity propylene glycol methyl ether acetate, control
Flow 100L/h, weight content >=99.99%；Overhead extraction liquid enters 3 molecular sieve dehydrations：Molecular sieve modelAluminosilicate
Salt, 1.6~2.5mm of grain size, control moisture are less than 50ppm；Enter 4 resin deacidifications after dehydration：Resin model is D301R, adjustment
Flow velocity is 16BV/h, and Controlled acidity is less than 20ppm；Enter 5 cation exchange resins after depickling and removes metal ion：Resin model
For D001 × 1, adjustment flow velocity is 20BV/h, and control metal ion weight content is less than 0.1ppb；Enter 6 after removing metal ion
Anion exchange resin removes nonmetallic ion：Resin model is D201, and adjustment flow velocity is 12BV/h, controls each nonmetallic ion
Weight content is less than 100ppb；Finally enter 7 ultrafiltration removal dust granules：Filter membrane is hollow fiber ultrafiltration membrane, and material is poly-
Vinylidene, aperture 0.05, control dust granules (0.5 μm of grain size >) are in 5pcs/ml hereinafter, obtaining target product semiconductor grade
Propylene glycol methyl ether acetate, quality measurements are shown in Table 1.
Embodiment 2
Combined process flow chart 1, by technical grade weight content 99.0% or more propylene glycol methyl ether acetate with 165L/
The flow of h is preheated rear de- light into 1：Lightness-removing column filler model CY700, atmospheric operation, reflux ratio 15:1, bottom temperature
150.0±1.0℃；Tower bottoms enters 2 de- weights：Weight-removing column filler model CY700S, operating pressure 30KPa, reflux ratio 1.5：
1,85.0 ± 0.5 DEG C of tower top temperature, 116.0 ± 1.0 DEG C of bottom temperature, overhead extraction high-purity propylene glycol methyl ether acetate, control
Flow 150L/h processed, weight content >=99.99%；Overhead extraction liquid enters 3 molecular sieve dehydrations：Molecular sieve modelSial
Hydrochlorate, 3~5mm of grain size, control moisture are less than 50ppm；Enter 4 resin deacidifications after dehydration：Resin model is D301G, adjustment stream
Speed is 24BV/h, and Controlled acidity is less than 20ppm；Enter 5 cation exchange resins after depickling and removes metal ion：Resin model is
D001 × 2, adjustment flow velocity are 30BV/h, and control metal ion weight content is less than 0.1ppb；Enter 6 the moon after removing metal ion
Ion exchange resin removes nonmetallic ion：Resin model is D201 × 4, adjustment flow velocity is 18BV/h, control it is each it is nonmetallic from
Sub- weight content is less than 100ppb；Finally enter 7 ultrafiltration removal dust granules：Filter membrane is hollow fiber ultrafiltration membrane, and material is
Kynoar, aperture 0.2, control dust granules (0.5 μm of grain size >) are in 5pcs/ml hereinafter, obtaining target product semiconductor
Grade propylene glycol monomethyl ether acetate, quality measurements are shown in Table 1.
Embodiment 3
Combined process flow chart 1, by technical grade weight content 99.0% or more propylene glycol methyl ether acetate with 215L/
The flow of h is preheated rear de- light into 1：Lightness-removing column filler model DY1000, atmospheric operation, reflux ratio 25:1, bottom temperature
150.0±1.0℃；Tower bottoms enters 2 de- weights：Weight-removing column filler model BX500, operating pressure 30KPa, reflux ratio 2.0：1,
85.0 ± 0.5 DEG C of tower top temperature, 116.0 ± 1.0 DEG C of bottom temperature, overhead extraction high-purity propylene glycol methyl ether acetate, control
Flow 200L/h, weight content >=99.99%；Overhead extraction liquid enters 3 molecular sieve dehydrations：Molecular sieve modelAluminosilicate
Salt, 0.5~1.0mm of grain size, control moisture are less than 50ppm；Enter 4 resin deacidifications after dehydration：Resin model is D301T, adjustment
Flow velocity is 32BV/h, and Controlled acidity is less than 20ppm；Enter 5 cation exchange resins after depickling and removes metal ion：Resin model
For D001 × 3, adjustment flow velocity is 40BV/h, and control metal ion weight content is less than 0.1ppb；Enter 6 after removing metal ion
Anion exchange resin removes nonmetallic ion：Resin model is D201 × 7, and adjustment flow velocity is 24BV/h, and control is each nonmetallic
Ion weight content is less than 100ppb；Finally enter 7 ultrafiltration removal dust granules：Filter membrane is hollow fiber ultrafiltration membrane, material
For Kynoar, aperture 0.02, control dust granules (0.5 μm of grain size >) are partly led in 5pcs/ml hereinafter, obtaining target product
Body grade propylene glycol monomethyl ether acetate, quality measurements are shown in Table 1.
1 Examples 1 to 3 semiconductor grade propylene glycol methyl ether acetate quality measurements of table
As it can be seen from table 1 the preparation method of the semiconductor grade propylene glycol methyl ether acetate of the present invention, can produce weight
It is content >=99.99%, coloration APHA≤10, moisture≤50ppm, acidity≤20ppm, each individual event metal ion < 0.1ppb, each
The semiconductor grade propylene glycol monomethyl ether acetic acid of individual event nonmetallic ion < 100ppb, dust granules (0.5 μm of grain size >) < 5pcs/ml
Ester product.
Wherein primary analysis method：Product weight content uses gas chromatographic analysis, moisture weight content to take using karr
Not moisture teller is analyzed, and anion is analyzed using ionic liquid phase chromatography (IC), and metal ion weight content uses inductive coupling
Plasma mass spectrometry (ICP-MS) is analyzed.
Although embodiments of the present invention are described in detail, it should be understood that, without departing from the present invention's
In the case of spirit and scope, can embodiments of the present invention be made with various changes, replacement and change.
Claims (10)
1. a kind of preparation method of semiconductor grade propylene glycol methyl ether acetate, it is characterised in that：With industrial grade propylene glycol monomethyl ether vinegar
Acid esters is raw material, first passes through rectification and purification, molecular sieve dehydration, then by resin deacidification, cationic, anionic exchange resin removal the third two
Metal ion in alcohol methyl ether acetate and nonmetallic ion obtain semiconductor grade propylene glycol monomethyl ether acetic acid finally by ultrafiltration
Ester.
2. preparation method according to claim 1, it is characterised in that：Specific preparation method includes the following steps：
(1) rectification and purification：Technical grade weight content is first passed through into efficient take off gently in 99.0% or more propylene glycol methyl ether acetate
Rectifying, then by efficiently taking off rectifying again, propylene glycol methyl ether acetate weight content >=99.99% after rectification and purification；
(2) it is dehydrated：Propylene glycol methyl ether acetate after rectification and purification is passed through into molecular sieve dehydration, dewatered propylene glycol monomethyl ether vinegar
Moisture control is in 50ppm or less in acid esters；
(3) depickling：Dewatered propylene glycol methyl ether acetate is removed by resin adsorption bed in propylene glycol methyl ether acetate
Acetic acid, remove acetic acid after propylene glycol methyl ether acetate in controlling pH in 20ppm or less；
(4) cation exchanges：Propylene glycol methyl ether acetate after depickling is exchanged into bed by cation exchange resin and removes metal
Ion, cation exchange after propylene glycol methyl ether acetate in individual event metal ion control in 0.1ppb or less；
(5) anion exchange：The propylene glycol methyl ether acetate for removing metal ion is exchanged into bed by anion exchange resin
Except nonmetallic ion, individual event nonmetallic ion is in 100ppb or less in the propylene glycol methyl ether acetate after anion exchange；
(6) ultrafiltration：Propylene glycol methyl ether acetate after removal nonmetallic ion, which is passed through ultrafilter, reduces propylene glycol monomethyl ether acetic acid
Dust granules in ester, in the propylene glycol methyl ether acetate after ultrafiltration the dust granules control of 0.5 μm of grain size > 5pcs/ml with
Under.
3. preparation method according to claim 2, it is characterised in that：In step (1) rectification and purification process, efficiently de- light essence
Evaporate filler model BX500, CY700, CY700S that the weight-removing column used in lightness-removing column used and efficiently de- rectifying again is selected and
One kind in DY1000.
4. preparation method according to claim 2, it is characterised in that：In step (1) rectification and purification process, described is efficient
It is 1~50 to take off reflux ratio in light distillation operation：1；Reflux ratio is 0.5~3.0 in efficiently de- weight distillation operation：1.
5. preparation method according to claim 2, it is characterised in that：In step (2) dehydration procedure, molecule screening
WithOrAluminosilicate molecular sieves in one kind；The aluminosilicate molecular sieves select the particle diameter to be
0.5~1.0,1.6~2.5mm or 3~5mm.
6. preparation method according to claim 2, it is characterised in that：In step (3) deacidification process, the resin adsorption bed
Resin used selects large aperture basicity styrene series anion exchange resin.
7. preparation method according to claim 2, it is characterised in that：In step (3) deacidification process, propylene glycol monomethyl ether acetic acid
The flow velocity that ester passes through propylene glycol methyl ether acetate when resin adsorption bed is 1~50BV/h.
8. preparation method according to claim 2, it is characterised in that：Step (4) cation exchanges in process, the sun
Ion exchange resin is large aperture acidity styrene type cation exchange resin；Described exchanges bed by cation exchange resin
When propylene glycol methyl ether acetate flow velocity be 1~80BV/h.
9. preparation method according to claim 2, it is characterised in that：In step (5) anion exchange procedures, described the moon
Ion exchange resin is large aperture basicity styrene series anion exchange resin；Described exchanges bed by anion exchange resin
When propylene glycol methyl ether acetate flow velocity be 1~50BV/h.
10. preparation method according to claim 2, it is characterised in that：In step (6) ultrafiltration process, used in ultrafilter
Filter membrane is hollow fiber ultrafiltration membrane, and material is one kind in polyamide, polyether sulfone and Kynoar, the hollow fibre
Tie up 0.5 μm of the aperture < of ultrafiltration membrane.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710261566.3A CN108727191A (en) | 2017-04-20 | 2017-04-20 | A kind of preparation method of semiconductor grade propylene glycol methyl ether acetate |
| PCT/CN2017/105710 WO2018192195A1 (en) | 2017-04-20 | 2017-10-11 | Method for preparing semiconductor-grade propylene glycol methyl ether acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710261566.3A CN108727191A (en) | 2017-04-20 | 2017-04-20 | A kind of preparation method of semiconductor grade propylene glycol methyl ether acetate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108727191A true CN108727191A (en) | 2018-11-02 |
Family
ID=63855479
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710261566.3A Pending CN108727191A (en) | 2017-04-20 | 2017-04-20 | A kind of preparation method of semiconductor grade propylene glycol methyl ether acetate |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN108727191A (en) |
| WO (1) | WO2018192195A1 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110204442A (en) * | 2019-05-23 | 2019-09-06 | 安徽京控环境技术服务有限公司 | A method of purification propylene glycol methyl ether acetate is recycled from spent organic solvent |
| CN110305012A (en) * | 2019-08-16 | 2019-10-08 | 南通百川新材料有限公司 | A kind of synthesis technology of semiconductor grade propylene glycol methyl ether acetate |
| CN114262269A (en) * | 2021-12-30 | 2022-04-01 | 宁波南大光电材料有限公司 | Preparation method of propylene glycol methyl ether acetate |
| CN114656339A (en) * | 2022-04-25 | 2022-06-24 | 北京袭明科技有限公司 | Production method and device of high-purity electronic-grade propylene glycol monomethyl ether |
| CN115806472A (en) * | 2021-09-13 | 2023-03-17 | 中国石油化工股份有限公司 | Preparation method of electronic-grade isopropanol and system for preparing electronic-grade isopropanol |
| CN115872868A (en) * | 2021-09-27 | 2023-03-31 | 载元产业株式会社 | Method for purifying high-purity alkylene glycol monoalkyl ether carboxylate for photoresist process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924242A (en) * | 2012-08-17 | 2013-02-13 | 上海泰坦科技有限公司 | Method for purifying propylene glycol ether compounds |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59176232A (en) * | 1983-03-17 | 1984-10-05 | アトランテイツク・リツチフイ−ルド・カンパニ− | Manufacture of monocarboxylic acid ester of alkyleneglycolmonoalkyl ether |
| US4544453A (en) * | 1983-03-17 | 1985-10-01 | Atlantic Richfield Company | Stripping of unreacted glycol ethers and acids from an esterification reaction mixture |
| CN1304359C (en) * | 2005-04-22 | 2007-03-14 | 江苏华伦化工有限公司 | Process for synthesizing propylene glycol monomethyl ether acetate (PMA) |
| CN101993360B (en) * | 2009-08-21 | 2014-04-09 | 江苏瑞佳化学有限公司 | Preparation method of electronic grade propylene glycol methyl ether acetate |
| CN202519181U (en) * | 2012-03-17 | 2012-11-07 | 江苏怡达化工有限公司 | Device for continuously producing electronic grade propylene glycol methyl ether acetate |
| CN104370742B (en) * | 2014-10-16 | 2016-01-06 | 惠州Tcl环境科技有限公司 | A kind of method of PGMEA that purifies from PGMEA waste liquid |
| CN104498640B (en) * | 2014-12-19 | 2018-02-06 | 成都连接流体分离科技有限公司 | A kind of technique using plant refuse as raw material coproduction xylose, microcrystalline cellulose and sodium lignin sulfonate |
-
2017
- 2017-04-20 CN CN201710261566.3A patent/CN108727191A/en active Pending
- 2017-10-11 WO PCT/CN2017/105710 patent/WO2018192195A1/en active Application Filing
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924242A (en) * | 2012-08-17 | 2013-02-13 | 上海泰坦科技有限公司 | Method for purifying propylene glycol ether compounds |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110204442A (en) * | 2019-05-23 | 2019-09-06 | 安徽京控环境技术服务有限公司 | A method of purification propylene glycol methyl ether acetate is recycled from spent organic solvent |
| CN110305012A (en) * | 2019-08-16 | 2019-10-08 | 南通百川新材料有限公司 | A kind of synthesis technology of semiconductor grade propylene glycol methyl ether acetate |
| CN115806472A (en) * | 2021-09-13 | 2023-03-17 | 中国石油化工股份有限公司 | Preparation method of electronic-grade isopropanol and system for preparing electronic-grade isopropanol |
| CN115872868A (en) * | 2021-09-27 | 2023-03-31 | 载元产业株式会社 | Method for purifying high-purity alkylene glycol monoalkyl ether carboxylate for photoresist process |
| CN114262269A (en) * | 2021-12-30 | 2022-04-01 | 宁波南大光电材料有限公司 | Preparation method of propylene glycol methyl ether acetate |
| CN114262269B (en) * | 2021-12-30 | 2023-09-26 | 宁波南大光电材料有限公司 | Preparation method of propylene glycol methyl ether acetate |
| CN114656339A (en) * | 2022-04-25 | 2022-06-24 | 北京袭明科技有限公司 | Production method and device of high-purity electronic-grade propylene glycol monomethyl ether |
| CN114656339B (en) * | 2022-04-25 | 2023-12-29 | 北京袭明科技有限公司 | Method and device for producing high-purity electronic grade propylene glycol monomethyl ether |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2018192195A1 (en) | 2018-10-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108727191A (en) | A kind of preparation method of semiconductor grade propylene glycol methyl ether acetate | |
| CN108727164A (en) | A kind of preparation method of semiconductor grade propylene glycol monomethyl ether | |
| CN108794371B (en) | A kind of refining methd of N-Methyl pyrrolidone product | |
| JP2003535836A5 (en) | ||
| CN104557529B (en) | A kind of process for purification for n-propyl acetate lactate synthesis and device | |
| CN103613486A (en) | Preparation method of ultrapure isopropanol | |
| CN108658785B (en) | The separation method of difficult separation system containing triethylamine | |
| CN114344932A (en) | Method and device for producing high-purity electronic grade acetone | |
| CN107903148A (en) | Top grade alcohol, alcohol fuel, electronic grade anhydrous alcohol production device and its production technology | |
| CN105502295A (en) | Electronic grade hydrogen chloride purification method | |
| CN113429329A (en) | Purification method of semiconductor grade N-methyl pyrrolidone | |
| CN110713432A (en) | Preparation method of anhydrous electronic grade ethanol | |
| CN102093160B (en) | Method for preparing chromatographically-pure trichloromethane | |
| CN103601624A (en) | Preparation method for ultra pure acetone | |
| CN104926690B (en) | The recovery process for purification and device of acetonitrile in a kind of synthesis for Ceftriaxone Sodium | |
| CN104130105B (en) | The method that in D-4-methylsulfonylphserine serine ethyl ester production, ethanol is recycled | |
| CN111574326A (en) | Purification method of semiconductor grade isopropanol | |
| CN107459472A (en) | The process for purification of dimethyl sulfoxide solvent in carbon fibre precursor production process | |
| CN103467252B (en) | Method for increasing purity of di-trimethylolpropane | |
| CN114702385B (en) | Production method and device of high-purity electronic grade propylene glycol methyl ether acetate | |
| CN108689812A (en) | A kind of method of ion liquid abstraction rectifying methanol removal and water simultaneously | |
| CN109134197B (en) | Method for separating dichloropropanol from dichloropropanol hydrochloric acid solution by using alkane entrainer | |
| CN113527214B (en) | Method for preparing 4, 6-dihydroxypyrimidine | |
| CN107137949B (en) | Extraction and rectification partition plate tower device and method for dehydrating low-concentration isopropanol solution | |
| CN102659574B (en) | Crystal separation method and equipment in production of Kunlun purified terephthalic acid (KPTA) through advanced oxidization process |
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 |
Application publication date: 20181102 |
|
| RJ01 | Rejection of invention patent application after publication |